Process for the preparation of alkaline polyphosphides having long phosphorus atoms chains as well as of pure phosphorus and of semiconductors fillers and films containing them and apparatus for its realization

The present invention relates to phosphor lace materials with long phosphorus chains, their preparation and use e.g. to semiconductors or other devices that employ them. Such materials include high phosphorus polyphosphors (i.e. phosphorus (III) that the polymeric nature is lying), alkaline material polyosychotics, xionoolfenic phosphorus, and novel forms of phosphorus. 0 Steam transport is employed in the manufacture of crystalline phosphorus, polycrystalline and amorphous and bulk polyphosphide-based materials in thick and thin films. Instant evaporation and chemical vapor deposition are used to make thin films. A condensed phase technique is used in the production of crystalline and polycrystalline polyphosphides. The addition of impurities to the diffusion semiconductor is employed to increase the conductivity of these materials. Grinding joints are formed in the materials by means of appropriated metal contacts · Film materials can be used with epic coatings. Powdered crystals and amorphous materials can be used as fire retardant charges. Crystalline materials, especially fibrous forms, can be used as raw materials.

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Over the past decades, the use of semiconductors has become increasingly widespread and important. Silicon-based semiconductors, for example, have generally been successful in providing a wide variety of useful devices such as pn function rectifiers (diodes /, transistors, silicon control rectifiers (DOS), photovoltaic cells, lus sensitive diodes and the like. However, due to the high cost of producing crude silicon and the ever-increasing demand for semiconductors in a growing range of applications, there has been a need to correspondingly broaden the range of useful semiconductor materials available.

Useful semiconductors of the present invention have an energy band range of between 3 and V (more specifically 1.4 and 2.2 and V /, a photoconductor ratio greater than 3, more specifically erroneous). and lu.OOOy; a conductivity between 10 and 10 o '

-cm units specifically within the range of 10 ~ ^ ..

—9 ohn-em / je good chemical and physical stability under ambient operating conditions'. Accordingly, while many materials may be semi-conductive in the sense that they are neither pure metals nor pure insulators, only those sen- ductive materials that meet these criteria can be considered to be semi-conductive in the context of the present invention.

Given the need r. While developing alternative energy sources other than petroleum-based, the potential commercial utility of a semiconductor increases dramatically when the semiconductor also has an effective photovoltaic characteristic, that is, the ability to convert economically. It is energy efficient to keep energy in electrical potential '; From an economical point of view, amorphous semiconductors, particularly in the form of films, are more desirable than normal crystals:

»

Γί '.

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Potentially lower production yield *. Semi-conductors also have better electrical qualities than polycrystalline furnaces of the same material used cr. mnitoc di semi-conductive devices n «

The semiconductor industry has continued to lusca new useful semiconductor materials, 'Ιδη of crystalline cylinders and the like,

In the domain of non-silicon crystals, monocrystals of semi-conductive compounds, including GaAs, Gol and Inf, are being used commercially,

Other semi-conductive materials have been used for special purposes *. For example, OdS and selenium are used as photoconductors in many xerographic machines.

In the present application, the semiconductor thermodevice means a device that includes a semiconductor material whether the device employs electrical contacts, that is, a clectronic device or both. non-electronical device, such as photoconductors employed in xerography, phosphorescent materials, phosphorus in a cathode ray tube or so, some of the known forms of phosphorus have been reported to have properties if: clogging, many are unstable, highly Roaotivae oxidizers and no known form of phosphorus have been successfully used as a useful semiconductor.

The materials derived from the 5-5 group elements such as gallium phosphoxide and indium phosphide are tetracritically linked and thus, as will be highlighted below, are clearly distinct from the compounds set forth herein. Furthermore, their conduction properties are not dominated by the phosphorus-phosphorus bond, that is, the primary conduction pathways are not phosphorus-phosphorus bonds.

Others have reported that the hydrogenated phosphorus is similar in structure to black phosphorus and has semi-conductive properties *.

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Research work on high phosphorous polyphosphors has been carried out by a group led by II, G. Von

Schnering Several reports in this group indicate that the compound of the phosphorus containing the highest phosphorus content they produced is the crystalline Mih (U = group of metals /. These polyphosphides are produced by heating a mixture of metal and phosphorus in a closed ampoule. . Von Schnering states g., C, based on their structure, polyphosphors are classified as valence compounds in a classical sense and that this means that these compounds are, or should be, insulators or semiconductors, that is, nonmetals.

Monoclinic phosphorus, also called Hittorf phosphorus, is prepared according to the prior art from stride and lead phosphorus as follows: 1 g white phosphorus and 50 g lead are acu. slowly at 650Â ° C until melted in a sealed tube and kept for a short time at that temperature. The solution is then cooled at 1 ° C per day for 11 days to 520% ​​and subsequently quenched to room temperature. It is then electrolyzed in a 2 kg solution of lead acetate in 8 liters of 6% acetic acid and phosphorus is collected in an hourglass placed under the anode. Almost square tabular crystals, about 0.2xC, 2x :: 0.05 mm, are obtained in this manner.

The structure of this prior art monoclinic phosphorus was determined by Thum and Krebs. The crystals comprise two layers of phosphorus pentagonal tubes with all tubes parallel and then another pair of phosphorus layers all distributed in pentagonal tubes, the tubes of the second pair of cornets all parallel but perpendicular to the tubes of the first pair of meat. A special group of crystals was determined, as well as the binding angles and the binding distances. See the summary of prior art knowledge in the section! Book Match The Structure of the Elements by Jerry

Donahue, published in 1974.

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The electronical properties of the phosphor crystals of I-Iittorf are not mentioned *, owing to their small size and their electrical properties cannot be easily determined.

The preparation of high grade phosphorus for electronical purposes according to the prior art processes is very complex and time consuming, therefore the electronic grade phosphorus is very expensive.

The prior art also shows a need for stable phosphorus compounds for use as fire retardants. Crystalline forms have additional utility as additives for plastics, glass and other materials.

The Applicant has discovered a family of alkaline metal polyphosphate ms having semiconductor, optic, and semi-finished pros.

Useful semiconductor pronouns

By "polyphosphide" is meant a material dominated by multiple phosphorus-phosphorus bonds. By useful myconductor it is meant not only that the conductivity of the material is intermediate between that of insulators or metals, but also the demonstration of a group of useful properties:

- Stability

- Resilient material structure

- Range of energy bands within a useful range typically 1 to 25 eT)

- inherent high resistivity, m. s capable of adding impurities.

- photoconductivity.de

- efficient luminescence

- Ability to form a grinding joint.

- Ability to be formed at relative temperatures.

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(for semiconductors) by easy-to-extrapolate processes.

- Ability to be formed under the furnace of large amorphous thin films.

Ability to be formed into ductile polymer fibers.

Polifpsforofcos are a unique family of materials that have all these characteristics.

Iressrvagão of utility in multiple forms

It is equally significant that the useful properties remain essentially constant over a wide range of crystalline and amorphous chemical and physical compositions).

As far as the Applicant is aware, polyphosphites are the only useful semiconductors in which desirable properties of the single crystal type are preserved in amorphous form. This is of major technological importance because the amorphous shape is at least easier to modify and often essential for large-scale applications such as photovoltaic cells, large display targets and electrostatic copiers »

But so far, the problem with amorphous semiconductors is that they do not easily form as a stable single-phase material. And even when they are forced to. Thus, the amorphous form loses some very desirable characteristics of its crystalline counterpart.

The known dominant semiconductor (silicon)¹:) has a tetrahedral coordination in its crystali form. Any attempt to make him amorphous (to be Si amorphous) is known to be accompanied by one. breakage of tetrahedral bonds, leaving pending bonds that destroy useful semiconductor properties.

If pure amorphous is useless, unstable and brittle. Attempts to satisfy pending hydrogen bonds

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or fluorine are partially successful.

central structure rapsl

The Applicant assumes that a. Preservation of useful properties between the multiple forms of polyphosphates is the direct result of the structure of the materials which, by their voice, is made possible by the unique properties of phosphorus, particularly its ability to line polymers dominated by covalent bonds. phosphorus in the majori. of the phosphorus locations,

In a crystalline form, polyphosphides of the type (with M - li, Ra, K, Rb, Os) are a structure formed by a phosphorus skeleton consisting of parallel tubes with a pentagonal cross section.

In these ligados-Ι2-pontes bridged phosphor tubes shown in Figures 4, 5 β 6. The building block for this atomic structure can be seen as Ιθ formed by two rigid units 3? ^} and Ι-Β? γ (form;

I by the association of rigid units dc and 3? ^ '' Using the building blocks or assemblies described above, Kosyakov in a journal article j (Russian Chemical Journal ”, 48 (2), 1979) theoretically showed that these Polyphosphorus compounds could be treated as polymeric materials using their basic building blocks as genera # Hence, in principle, it is possible to construct a large number of 'atavistic' structures that have the same phosphorous frameworks.

The work carried out by the Applicant has been synthesized by various techniques described further below. te, crystals of and also compositions of type (¢ £ ^.) jj ε · with b much larger than a. These new phosphorus-rich compounds originally noted as 'fibers',⁴“Thin fics” or strips ”are called in this investigation; Where x is much larger than 15 '₀ These low-lethal materials are prepared by x-ray, or x-ray. thick films (larger than; 10 niche) of polycrystalline fibers and large synonymous rubies.

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than 1 cnr) of amorphous character. Polycrystalline fibers have the same morphology as Zx-,_ç.

first skeletal structural skeleton ΜΑ .. (x much larger than 15) than Applicant • ii. * ““ Discovered is shaped by a phosphorus skeleton similar to the structure of the compounds

The Applicant has found that the useful eloctrical and optical properties of these crystalline materials and (x much greater than 15) are similar, but the properties of these materials are therefore dominated by the multiple covalent bonds RA of the match skeletons with a slightly lower coordination number than the others. that 3. Surprisingly, the Applicant also found that the useful electro-optical properties of these materials were essentially preserved in the case of crystalline materials YL (> 15) and their corresponding amorphous,

Unlike previously known materials, this is a rigid one-dimensional structure and resilient in the following sense. 'η. (Symmetry of polyphosphide crystal is too low vtriclinic) Applicant sipce that, in the transition from crystal to amorphous form, low symmetry material is accommodating covers. gradually the increased structural disorder that characterizes the amorphous state *. There is no breaking of the strong tetrahedral bonds with the same coordination number ε. 4), as in silicon, because phosphorus, with a much smaller coordinating number than silicon, can cause a much larger structural disorder without the creation of ponderous bonds. Polyphosphors are polymers by nature. 0 The result is a polymeric amorphous structure with no apparent X-ray diffraction peaks, a wider local order than is possible with conventional amorphous semiconductors. The Applicant assumes that this gradual onset of anorficity is the reason for this. the preservation of the desired crystal properties in the amorphous Toretos poliff.

Distinction in relation to

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Useful known seaconductors

The composition and structure of the polyphore family clearly distinguishes them from all known useful semiconductors;

G-group 40.

α-5u (II-V)

2b-6a (II-Vl) 1b-3a-6a

Oalcogenctos (ASgSe ^) (Crystalline Si- Si; H Amorphous etc.) (GaAs, Gar, In.;, Etc.) (Gas, OdTe, HgGâTe, etc.) (OulnSea)

Distinction from known forms of phosphorus Alkaline niphosphides ii, R

K, Rb, Os; at rue xa 15 is much larger than 15) phosphorus-rich. 3The shards of material blush '.'x high' they almost complete phosphorus dog '. However, their structure (parallel pentagonal tubes) and their properties (stability, energy band range, conductivity, photoconductivity) clearly distinguish them from all black, white / yellow, red and violet phosphorus-based materials. / IHttorf), The structural relationships between these various re are discussed:

Ct. '' XZmQ · ύ work done by. Applicant contributed to clarify this aspect of the phosphorus itself. '

The nomenclature in this area was a little confusing. ' 'The following summarizes the commonly used designations'.

1- 1 amorphous or red X

Amorphous phosphorus is a generic term for: · all non-crystalline forms of red phosphorus generally prepared by heat treatment of white phosphorus.

2- 1 violet

This microcrystalline form of phosphorus

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Red is prepared from DCs of pure T, or white or amorphous red, by prolonged heat treatment.

-P from Hittorf

However, it is crystalline, red in color and structurally identical to violet P. Hittorf's powder is prepared in the presence of large excess of lead *. Despite this, the terms Hittorf P and violet P '' have been used interchangeably. The crystal structure consists of double layers of parallel pentagonal tubes, with adjacent double layers perpendicular to the former forming a monoclinic cell. Hittor's P crystals are slightly larger (about 100 microns) than those of violet P crystals.

Big Crystal Monlinlco Match

Even the largest crystals (some mm), essentially iso-natural with the two above, are described herein. These new crystals are prepared by steam transport (YS) treatments of alkaline phosphorous charges. Inclusion of alkali metal is apparently essential for the formation of large crystals. The analysis confirms the presence of alkali metal (500 to 2000 ppm) in these large phosphorus crystals.

«Twisted Fiber Phosphorus

A christian form. described phosphorous salt prepared by tra. YT sum of amorphous P 'charges. It is assumed to be almost isolated.

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i “structural with strips” polycrystalline_χ.

RA3'EL OF LEA; WHY REASON Phosphorus is and the many allotropic forms and elemental R are the province of the variety and complexity of the bonds and structures that can be obtained with phosphorus. There is no readily available, detailed model of the exact manner in which alkali metal works. The Applicant develops a vast body of data showing how the metal stabilizes phosphorus in a single way. Rupture can be selected from the set of potentially available structures.

Without the presence of at least one alkali metal, the following undesirable phenomena occur:

A.) Phosphorus is unstable (eg 1 white;

B; To the extent that a single known phase is accessible to P, it may be a phase only at high temperatures and a size limited to nicrooristals (eg, violet), or

C) at high pressures (eg r black} 5

Without an alkali metal in the charge, the type of structure is not formed by vapor transport. Preferably, it obtains the form of the phosphorus twisted fiber which the Applicant has discovered. This crystalline phase is metastable and the structure has not thus been defined as shown by Ramsm, Ramsm and photoluminescence data.

The presence of alkali metal in the vapor transport favors the completely parallel untwisted face, λ also favors, as the Applicant has discovered, the

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dog dc gr · jades nonoclinical x crystals at a different temperature.

u dominant role of. structure, rather than composition, as a determinant of properties, is clear to note that (x much greater than 1) properties (range of energy band, photoluminescence).

cic., electron

Rc

U which are essentially those of

IKn, x5⁷ co '.

they are slightly different from those of the monoclinic, it is evident that (in a small amount of meth). Alkaline can serve to select a stable phase. But will non-alkaline vetals also act? Hrcbs refers to non-alkaline polysulfides, with tubular structures consisting of the element 2b-4a-x-.

(2.L - Zn, Cd, Hg and 4a. Sn, PbJ. For which are these compounds formed?

A speculative hypothesis is that these materials form a tubular structure because the element of group 4a is amphoteric and may occupy a bond of P instead of r.

An effective electron affinity of the structure can be calculated based on the ionization energies of the alkali metals, all of them smaller or equal. a 5.1 and L We can in turn calculate the effective ionization potentials for other possible compositions, such as the 2b-4a-P2 element compounds. All of the above-mentioned Erebs materials have lower effective ionization. or equal to 4.8 and V.

USEFUL PROPERTIES

The important initial finding was that the thin strands of stable monochromatic semiconductor KP ^^, with a range of the energy band corresponding to the velfel light (1.8 and Vy, which have efficient photoconductivity and photoluninescence. Main characteristics of a semiconductor with potential uses in electronics and optics, Fine EIOs of other alkaline materials also have these properties (M = Li, Ti, SL, Os),

To see what potential value I am, the materials have; be prepared in a size and size suitable for manufacturing test devices. However, the crystalline habit was not found to be confusing to the growth of large moncrystals that are free of^!! crystallographic twinning. The large, twin-free monos are the basis of all semiconductor device technologies today. Polycrystalline materials are less desirable because even if the individual grains are large, the presence of grain boundaries serves to destroy some desirable properties due to the physical and chemical discontinuities that are associated with such boundaries. As a result, the Applicant's attention turned to the crfs they had discovered.

Love semiconductors are useful, whether used as a junction device such as a photovoltaic cell or as a coating as a copier. electrostatic, have generally been made with the film tool for extrinsic reasons (cost, ease of manufacture) and need for application) and intrinsic reasons (material problems in the amorphous bulk state).

The Applicant has found that it can be - ftc under the furnace dc - a stable thin amorphous film (e.g., a vapor transport). (This cannot be done with silicon; the amorphous Si is not stable, whereas the monocrictal Si is /.

Stable, bulky and thin films of amorphous KR much larger than 15% may also be made by steam transport.

There is also clear evidence that these polyphosphors are still different in another way. The useful properties of these materials Lf- .. e (x much higher)

-Λ

than 15) are similar both in crystalline form and in their amorphous counterparts, as shown in Tables Σ7Ι and ΣΥΊΙ below.

Applications that use amorphous a. The thin film form that does not require joints can be easily imagined (eg electrotactic). In fact, the inherent high resistivity (approx. 10 a to 10-ohm-cm) is an advantage for such unstitched applications.

Electronic and optical-electronic devices all need to form some junction in the material or with the material. This requires a reduction in material resistivity by adding impurities to the semiconductor.

The Applicant has found that the diffused Hi in KP ^ serves the purpose of reducing the strength of the material by various orders of magnitude. Surface analysis demonstrated that solid state diffusion of Hi (ΚΡτ_5 depositing on a Hi layer) follows a normal diffusion pattern during the film growth process.

Hi depositive configurations in the form of a posterior contact is diffuser; and other materials such as Cu, · Α1, Mg, Mi, Au, Ag, β Si as top contacts, lead to Junction formation. Current-Voltage (IV) characteristics of the junction were measured with. those top contacts. Capacitàacia-Voltage junction capacitors were average; with top contacts from Al and Au. Data indicate that the double junction formation with a high strength layer is close to the top contact.

The high strength layer is an undoped portion of the KP-1 film which results from the present impurity addition procedure.

A small photovoltaic defect (micro arap current under a short circuit condition) was observed.

SUMMARY OF P0LIFO5EORBT.CS

The following describes the processes that

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And. Wanna? - did you find out that you can prepare pclifoofeι-υ'ό? t's variable composition and methodology. '', already dg ffaoe, J ', thickened (01)

71, the process consists of thermal heating, absorption (heating of an adjusted temperature) and cooling of the initial charge carried out in a container of minimal volume.^rBy vapor transport, crystalline and polycrystalline crystals are obtained in bulk.

An initial reaction charge is located in an area of ​​an evacuated tube that is heated to a temperature, Tc, which is May; than Td means Td at the temperature (s) of other area (s) where they deposit material from the vapor. Crystalline EP-SP2 is obtained. crystalline, polystalline (in bulk, and in the form ''. · '' thin films) and amorphous in bulk with '.. high Value of xj phosphorus monocluminous color strands · star shape $ and twisted phosphor fibers.

Two-source Yapcr .. (3 rt T) transport to the reagent positions which are the source are loaded into a physically separated evacuated chamber, at a distance between a deposition of debris between them. . Both sources are heated to higher temperatures than the deposition chamber (to achieve amorphous material at least; see below). Deposition sounds need not be the coldest in the system, but a colder area should not be able to condense more than one component.

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23-W was the first process using amorphous LR-irj with the thin-film furnace. Thin amorphous polycrystalline thin films are obtained and polycrystalline thin amorphous Thin films in bulk with a high value of x.

D. Rapid Cooling of Fusion II

Warms up un-charged nu®. vacuum tube seals (isothermally if possible) to temperatures higher than the melting point as determined by the observed endotropic character in D2A experiments and stored at that temperature for a certain period of time. The tube is so removed from the air supply:

focused. Obtained '7' ~ ç Instant

A garga in powder form is carried in small quantities under a slight argon flow rate._t in a R1 'heated susceptor, which is lying at temperatures below 800 ° C. Within the susceptor, the serial is placed through a tortuous path in which it is theoretically forced to contact hot surfaces. This is intended to rapidly and completely vaporize the charge so that the composition of the vapor stream is the same as that of the powder being injected. The steam stream is directed into a vacuum chamber where it collides with colder surfaces, resulting in condensed product materials. By this process, amorphous films were obtained.

I r-

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F .... 'Steam Chiropractic (CVS / ± hr), this process consists of the production of material by mixing two (or more) vaporized components that have to undergo some chemical reaction to provide the products. As practiced by the Applicant, K and P. are introduced separately into furnaces after measurement, in which they are rapidly vaporized or transported downstream by an argon stream to a cooling reaction chamber. that to the incubated streams produce materials of the condensed product.

It is the importance of the CED that, among all these processes, it is easy to extrapolate to sl.^JP? tions and for the addition of impurities r tu, that is, ite dopagen synthesis of material. Thus amorphous thin films of

Molecular Current Derorloon (IS2)

This process consists of a technique of conveying steam from multiple cu. It is based only on 2S-YT and Eolecular Feirite Epithelia (KBE), independently heated sources and allowed to vaporize the rd.caccn substrate at a controlled rate not attainable. 2S-Vx '. Deposition occurs in a vacuum controlled chamber^nogo. deposition situV (which also occurs with 2S-W). The chamber may be continuously fused to control pressure.

the EP EP.

there

A wide variety of polyester materials

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Forotos with different physical formations and compositions are initially prepared during investigations carried out by the Applicant. In the wandering, for potential semiconductor potentials the emphasis of the work has shifted from the preparation of non-crystalline materials of amorphous materials or under the bulk furnace or large area thin films.

Of all the formulation materials, M3? - ^, KRjfj is the single highest crystalline polyphosphorus compound (x equal to or greater than? ') That exists for the Er system. (By contrast, the other alkali metals may form compounds such as x 7 or i 13, such as CsT ..

ϋ.Ί-ι -j, and Co / o and Hy do not .r force as ec. For many reasons, the KB system is easier to control than other P-alloal metal systems where multiple compounds can be formed.

Furthermore, it is concluded from the results of the applicant's experimental work that, whenever K-s> 3? are vaporized in whatever manner and brought under a certain ratio ((P) / \ E} equal to or greater than 15) to a. zone whose temperature lies within the eorsect range if amorphous EL / ij fossa. By that interval is meant that the temperature must be sufficiently low to prevent the crystallization of Er »_ç and high enough ~ 15 so that no EB is deposited, where x is much larger than 15.

Based on this principle, all synthesis processes can be considered to work on the same general principle. Each simple process. I used different means to achieve source vaporization control or deposition control. Two-source systems (2S-VS, OVB and MED) are particularly useful as important variables can be independently controlled *.

Based on the above considerations, the EB-. _ςamorphous thin film form was chosen by the Applicant as the main composition for the development of the

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ii! development of useful semiconductor materials.

í ί

SB&amp;SO t

In a general survey of the nature of the polyphosphides, thin strands of single-ion crown-long potassium polyphosphoride were produced by single source vapor transport. When the nature of this material was investigated, it was found by the fraction of a ray so-critical that the crystals were^; However, these crystals were also found to be nomiconducting. When measuring emission at 4 ° K under argon laser illumination, photoluminescence was observed. ccn I nm. 1.8 s Y, thus indicating that the sateriel possibly has a bandwidth within this energy gum. Subsequently, to determine the conductivity of these wires, silver-dyed conductive wires were attached. To observe if the wires conduit! were actually fixed to a very small crystal; it was placed under a sioroscope while measuring; the debt is &amp; is. Surprisingly the conductivity did not go drastically when the crystal was occluded in the microscope field changing the illumination, Kedin ume. photo-conductivity ratio fie 100 being the conductivity «·^Γ'- * T dc.de unlighted wire wire equal to about 20 ^u (oha-cn). {rare, settling if the wires had a fie range! energy edge, seditions were then made to study

O. dependence on conductivity in relation to length_Λ wavelength, the dependence of optical absorption on the wavelength and the dependence on the conductivity of the fine strands on the temperature, these measurements together with the photolumetric measurements (c at 4^fiK, allow to establish that the fine yarns ti '· ώα have a bandwidth of approximately 1.8 s Y. j It has thus been established that the thin KP-- yarns^! were potentially useful semiconductors, amorphous film was used inside a quartz tube during the vapor transport production of the fine wires. This amorphous film was found to have also a bonda range in the order of about 10 ° C._O As the fine threads, ε, film

Λ _no 4- ί

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1,3 and V c a ration of araesser photocondutivids.de. v.

Λ^-- ,^The Ί ^s ** l '^_ (olUl-CBl / o ί · φ iac »4 · o: in_s It has been established that it is also a potentially useful semiconductor.

The problem with the invention then was whether EP2 could be produced as giveaways of crystals, such as silicon used in semiconductor production; only the amorphous or polyetheric films could be reprofiucably made and used for semiconductor production; and the complete characterization of the material yarns produced by them are vapor transport experiments and any analogous materials which might have the same useful properties.

After many experiments of steam transfer, the inventors have surprisingly found that polystalline and amorphous materials that have been transported by steam transport by heating a single source of a mixture of potassium and phosphorus and material are condensed at the other end of a closed tube. It consisted of 13? ^aaE when tested by wet analysis were X3? where x may range from about 100 to about 10,000.

The inventors then discovered that the affinity of phosphorus for potassium, or any suitable alkaline metal for this subject, in single source vapor transport, causes the initial deposition of KEjtj as the most stable polyphosphide. If there is an excess of phosphorus, then a new phosphorus form (ΙΌ? ,, where x is much larger than 15%.) This new form of phosphorus has the same useful elector qualities.

During the course of their investigations, the inventors, in an attempt to form thin films of anorphic and polycrystalline and other HD-alkalitron metals._ç and is a semicon 15 in analogs which could not be formed by single-source vapor transport, have designed a two-boil steam (separate source) process whereby the alkali metal and phosphorus are separated and heated separately. By controlling the temperature of a separate intermediate deposition, thin films were prepared.^tte alkali metal, polycrystalline and amorphous furnaces. This technique has also led to the production of thin films of polycrystalline phosphorus material and thick films of amorphous phosphorus material of the new form and other polymer type materials having z. Ke formula_w believing that K is an alkali metal ex is much worth 15.

Instant Evaporation and Chemical Vapor Deposition were also used and the Molecular Current Deposition method was used to synthesize these materials.

Did you use SI? such as. formula of all no2 *.

lifcofo ?? etoc. Top will be highlighted / 0 below, x can range from 7 to infinite pure useful semicriductors, Cs known alkaline phosphides have the formulas ΜΕγ, ** 21 0 It has been found that there are presumably forms of the polymer having the formula EQ: and where x is much bigger than 15,

Also during these investigations, the single source vapor transport method was improved over the prior art by controlling the deposition temperature so that it was constant over a large area. thick films of large area and 13 'synthetic rubies. amorphous and pcl · ..crystalline where x is much higher than 15.

Large amounts of srictaliro and polyetheristalene were obtained, wherein Ι-Σ is an alkali metal, by isochromic heating together of stoichiometric proportions of an alkali and phosphorus. This condensed phase process yields an excellent Er ,,, where x ranges from 7 to 13. For use in a single source vapor transport, the phase process itself

<img file="PT76047B_D0018.tif" />

The prior art is facilitated by mixing and milling the above together an alkali metal and phosphorus in a ball mill which is preferably heated to an iguol temperature of about 100 ° C. This grinding surprisingly gives rise to relatively stable powders.

All of the parallel pipe polyphosphs have an energy band range of approximately 1.8 and V, photoconductivity ratios of greater than 5. (ratios measured within a range of 100 to 10,000 / and a small conductivity of the order of IO ”⁸ at 10 “⁹ (ohm-cm

As the Applicant has found that the amorphous forces of material, that is, KF of ileal polyphosphides. in which x is greater than 6, formed in pre. Substantially the presence of an alkali metal has semiconductivity properties, it has been found that the local order of the amorphous materials is substantially esna and in all cases consist of parallel pentagonal tubes substantially along their length.

There are all polyphosphides, the 5 covalent phosphorus-phosphorus (homoatomic) bonds in most faith sites.-torus dominate any other bonds: ^;present to provide the driving paths and all of them have semiconductor properties.

The covalent bonds of phosphorus atoms which are all used in chaining providing the dominant conduction beams and the local parallel order in these materials provide the good semiconductor properties. Phosphorus atoms are trivalenorrhoidal spirals or tubes having such. The atoms of the metes and the threads straight sections with the form of the '. such alkaline when present,

Igarn chaining them;

each other. Different atomic species of phosphorus, particularly trivalent species, capable of forming 3 covalent hoxic bonds, should also form semiconductors.

Thus, the Applicant invented new ways

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i

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· 3 solids?_ν Polymorphine and Polymorphine and Processes and Blinds for the Preparation, Processes and Apparatus for the Preparation of Metal Polymorphs by Multiple Single Source Techniques, Processes and Apparatus for the Preparation of High Phosphorus Polymers multiple separate source techniques processes and apparatus for the manufacture of condensed phase techniques in polycrystalline forms, semiconductor devices comprising a group of polyphosphate having seven or more phosphorus atoms bonded together forming penta tubes. goncir having a bandwidth greater than 1 and V and photoconcentration ratios of 100 to 10,000, semiconductor devices comprising ΙΦ, where I 1 is an alkali metal ox is greater than 6, and materials having a ; bandwidth greater than 1 and V and ra || Action on photoconductivity of 10 to 10,000 devices! ' semiconductors formed by a high proportion of covalently bonded trivalent bonded phosphors, preferably phosphorus, wherein the linked atoms are joined by multiple covalent bonds whose local order comprises layers of linked atoms that are parallel in each layer. and the layers are parallel to each other, strands being preferably pentagonal tubes, semiconductor devices which comprise fuels; a motel, alkaline and said structures in c! Where the number of consecutive covalent chained bonds is preferably greater than the number of non-chained bonds required for such material to make semiconductor, compound semiconductor devices comprising at least two chained units having each unit a skeleton with at least 7th cationically linked, preferably phosphorus-linked, atoms having alkali metal atoms concomitantly bonding the backbone of one unit to another, junction devices, processes for forming such semiconductor devices, electrical current conduction and generation of polymers.

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electrical potential using such devices »

The Applicant has therefore covered all the classes of materials that serve as useful Writers having some of the class first produced and previously characterized by the Applicant and will have others already known in the prior art to discover their useful semiconductor properties until discovered. and inventions ca Applicant.

pots and ecsec materials have in the range of the energy band within the range of 1 to 5 and Y, preferably within the range of 1.4 to 2._s2 εΥ and preferably equal to about 1_sE © Y »Your photoconductivity rates are greater than 5 and actually range from 100 ε 10,000. Their capacities are within the range of 10 ”, - 10 (dirz-cn), with ο« · »3_» being about 10 (ctr-cm).

Those of ordinary skill in the art will readily understand that the alkali metal component of the polyphide ferret or any ^weto^R Trivalent cells capable of forming homoatotic covalent bonds ε having the formula KP can comprise any number of allyl metals (or the combination of rectals having the same bonding behavior as an alkali metal) are proportional to changing the basic pentagonal structure. tubular and without significantly affecting the electrical semiconductor properties of the material.

The Applicant has further developed and invented processes for adding impurities to the inventive materials by adding iron, chromium and nickel to increase conductivity. Joints are prepared using Al, Au, Cu, lg, 8 ±, Ag, li, wet ink, silver and ε point pressure contacts.

The incorporation of ami-ni n '. in polyphosphorides (all parallel tubes) also allowed to increase inductivity.

The same reason for the addition of dusts is also part of the scope of the present invention and the discovery of the Applicant.

The semiconductor materials and devices of the present invention have a wide variety of uses. These include photoconductors used in photocopy equipment; moon emitting diodes; transistors, diodes and integrated circuits; photovoltaic applications; metal oxide semiconductors; moon detection applications; phosphorus subjected to photon or electron excitation and any other use of suitable semiconductors.

During the Applicant's research work it was also possible to obtain for the first time large crystals of clinical phosphorus. These crystals are obtained by the vapor transport technique using a charge of or a mixture of Hep ( M / P) in other proportions. Surprisingly, these large single phosphorus crystals contain a significant amount of alkali metals (500 to 2000 ppm have been observed). Under the same conditions, these crystals cannot be grown without the presence of alkaline metals.

Two different crystalline habits were observed in these large phosphorus crystals,

A crystalline habit has been identified as being formed by pyramid-shaped crystals, as shown in Figure 39. These crystals are difficult to break. The other form is a platelet-like crystal that is cleavable as shown in Figure 40.

The largest crystals with the crystalline habit represented in Figure 3S that were obtained by the Applicant are 4mmx3mmx2mm high. The largest crystals with the crystalline habit depicted in Figure 40 are 4 mm long and 2 mm thick.

Crystals have a metallic appearance when observed by reflections and blood red when observed by transmission. The chemical analysis they: r has between about 500 and 2000 parts per million mt Ιοί caline. The Aspect of X-Drain Diffraction Figures

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in foot, Raman spectrum and differentiated thermal analysis are all consistent with Hittorf's match of technique

C? 1 ύ vi J_ Π-ΟΧ * o

The photolurinescence of crystals that develop in the presence of cesium in Figure 41 is that of crystals that have developed on p. The fluid presence of Figure 42 shows peaks at 4-019 3981 cm which indicates an interval of the energy band equal to the crown of the

2.1 cV at room temperature for this monocyclic phosphorus',

Crystals may be used as a source of phosphorus; As optical totatives in the red and infrared region of the spectrum (they are birefringants) as substrates for the development of materials such as indium phosphide and gallium phosphide, they may be used in luminescent dials or as lasers.

From the same charge, the Applicant was able to develop the deposition at a slightly lower temperature of the star-shaped fibrous crystals depicted in Figures 44 and 45Ϊ by vapor transport, the Applicant was also able to develop an allotropic crystal of phosphorus. twisted phosphor fiber repre. ntacla in Figure 46 „

Polyphosphors may be used as fire retardants and as reinforcing agents for plastics, glass and other materials. Twisted tube-shaped fibers and star-shaped fibers should be of particular importance in reinforcing composite materials because of their ability to mechanically interconnect with the surrounding material. Platelets should be of particular interest in sheet metal materials where glass flakes are currently employed.

Film materials according to the present invention may be used as coatings because of their chemical stability, fire retardancy and optical properties.

It is therefore an object of the present invention to provide a new class of materials useful as semiconductors.

Other objects of the present invention include providing new processes and apparatus for the manufacture of polyphosphs.

Still other objects of the present invention are to provide stable forms of high phosphorous materials and processes and apparatus for their manufacture.

Another object of the invention is to provide new phosphorus furnaces and processes and apparatus for preparing them.

also aim of. present invention to provide wetting agents for such materials and processes thereof.

Still another object of the present invention is to provide semicenductor devices employing the abovementioned natorials.

Another object of the invention is to provide large monoclinic phosphorus crystals.

Still another object of the present invention is to provide high purity phosphorus.

Still another object of the invention is to provide new semiconductors vs. materials.

Another objective there. that of the invention is to provide a bi-refringent material for use in the red and infrared region. of the spectrum '.

Still another object of the invention is to provide pure manufacturing of materials of the above type.

Another object of the invention is to provide processes that are more convenient and less expensive than those of the prior art.

Another object of the invention is to provide coating materials, fillers,

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reinforcement and fire retardants.

Other obvious objects of the invention will appear in country. , subsequently in the present specification.

The invention accordingly comprises one or more inventive phases and the relationship of such phases with respect to each other will be exemplified in the following methods, hereinafter described, compositions of matter having the characteristics, the properties of the invention. and the frog ''? constituents or components which will be exemplified in the following compositions described in art. Manufactured materials having the characteristics, properties and ratio of elements that will be exemplified by the subsequent described products and the apparatus comprising the construction and arrangement aspects of the parts which will be exemplified in the following described apparatuses. The scope of the invention is indicated in the claims.

BRIEF DESCRIPTION OF THE DRAWINGS

For a more complete understanding of the nature and objects of the invention, the following description is given in connection with the accompanying drawings in which it is described.

Figure 1 is a diagrammatic but also straight-through view of the single source vaper conveying apparatus in accordance with the present invention;

Figure 2 is a diagrammatic view of a part of the steam conveying apparatus of Figure j. Figure 3 is a diagrammatic view of another single source steam conveying apparatus according to the present invention;

Figure 4 is a computer-supplied diagram of the X-ray diffraction data of 5 'phosphorus atoms. ^en ^^{eu c} ^^0E0 setal alkali> e;

Figure 5 is a diagram provided by the user of the X-ray diffraction data of a cross section of EK ... showing how the eovalent bond of the phosphorus atoms of Figure 4 forms a tubular structure. Pentagon?.;

Fig. 6 is a computer-provided diagram of longitudinal section X-ray diffraction data of Figs. 7 and 8 are photomicrographs of fine crystallized strands;

Figure 9 is an impression of the crystalline powder X-ray diffraction figure; Figure 10 is. .a print of the X-radios diffraction figure X? crystalline, where x is greater than 15, in powder form;

Figure 11 is a diagrammatic view of an experimental vapor delivery reaction tube from two sources in accordance with the present invention;

Figure 12 is a temperature graph or: length function for the reaction tube of Figure 11;

Figure 13 is a diagram of the ratio xsK of the reaction products existing.: In the reaction tube of Figure 13.ja. Figure 14 is a schematic diagram of the vapor transport uporellio from two sources of οονΑο: the present invention. ;

Figure 15 is a diagram of one of the elements of the apparatus shown in Figure 14; Figure 15 is a diagrammatic view of another reaction heading for conveying steam from two sources according to the invention;

Figure 17 is a diagrammatic view of a ball mill according to the present invention;

Figures 18, 19, 20 are tix-uao cc micrographs. (S33?) Of a film of one. formaε „new form of phosphorus, where x is much larger than aue 15;

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Figure 21 is a photomicrograph of a surface after attacking said W? high x-ray, synthesized by single source vapor transport, according to the present invention;

Figure 22 is a photomicrograph of an amorphous, after etched, surface of said high x-ray, synthesized by vapor transport from sources according to the present invention. Figure 23 is a photomicrograph of the ελυna surface depicted in FIG. Figure 22;

Figure 24 is a photomicrograph of an attacked surface perpendicular to the surface shown in Figures 22 and 23; Figure 25 is a photomicrograph taken with 3BI (scanning electron microscope) of the upper surface of an amorphous thin film synthesized by transportation of floor from two sources in accordance with the present invention;

Figure 26 is a partial cross-sectional view in diagrammatic view illustrating the formation of a joint in accordance with the present invention;

Figure 27 is a representation of the figure obtained on the oscilloscope display 'in the experiment illustrated in Figure 26; and Figure 28 is a partial cross-sectional diagrammatic view illustrating the furnace; of a junction c and according to the present invention;

Figure 29 is a representation of the figure obtained on the scope display in the experiment illustrated in Figure 28;

Figure 30 is a diagram of a photosensitive resistor according to the present invention;

Figures 31, 32, 33 are representations of the figures obtained on the oscilloscope display showing the joining activity and accretion devices of the present invention;

Figures 34, 35 and 36 are graphs of junction capacity versus electrical potential.

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applied to junction devices according to the invention;

Figure 37 is tv: graph of capacitance and resistance as a function of the potential sequence applied to accordion devices to the present invention;

Figure 36 is a preferred embodiment of the sealed ampoule used to form nonoclinic phosphorus according to the present invention;

the figure. 39 is a photomicrograph of a nonoclinic phosphorus cryothal according to the presence of Fig. 40 is a photomicrograph of nonoclinic phosphorus crystal according to the invention. Figure 41 is a diagram of the photoluninescence response. â € ƒâ € ƒâ € ƒa monoclinic phosphorus crystal according to the present invention;

Fig. 42 is a diagram similar to Fig. 6 of the non-cleavage photon response of a vonocyclic phosphorus crystal of the present invention; and Fig. 43 is a spectrum of nonoclinic phosphorem in accordance with the present invention;

Figures 44 and 45 are SEM photomicrographs of other phosphorus furnaces according to FIG. the present invention;

Figure 46 is a photomicrograph of a SE ray of another novel phosphorus form according to the present invention;

Figure 47 is a diagrammatic view e.g. side elevation of the instantaneous evaporation apparatus according to the present invention;

Figure 48 is a cross-sectional view taken along line 48-48 of Figure 47;

Figure 49 is a cross-sectional view taken along line 49-49 of Figure 48;

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α Figure 50 is a diagram of the anarchic deposition qiuQiicc. steam vapor: agreement with the urgent need.

0 ..uaics reference numbers, refers ^rwe look at elements throughout &lt;.the various views s draw s „

Materials of eight phosphorus content, for example, exemplified by the high phosphorus polyphosphorides KR4, wherein 15.5 µm. alkalethanol, and the new phosphorus furnaces, for example, all have apparently local sweat either crystalline, polycrystalline or amorphous. The Applicant admits that in the crystalline form as amorphous, this place tc:. the furnace of elongated phosphorus tubes with straight pentagonal sections as shown in Figures 4, b and b. All generally parallel pentagonal tubes on the local scale and in the double layers of R &amp; d of the pentagonal phosphorus tubes are linked together by atoms. motal alkaline interstitial. The new forms of phosphorus according to the present invention, much, if not most, of the alkali metal atoms are missing. However, it appears that a form of phosphorus formed in the fill of quantities; The small amounts of alkali metal atoms develop from vapor deposition in the same form as the experiment to be discussed below indicates that at least one further of this is by growth of the phosphorus cloud. in a layer of θ P ° d^and act as a mold by having the match arrange with the same structure. All materials having these all parallel pentagonal phosphor tubes have, as the Applicant discovered, the range of the energy band between 1.4 and 2.2 eV and o. mostly in the order of 1.8 eV, photo conductivity ratios range from 100 to 10,000 ”, so it is indicated that all alkali metal niphosphides are

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Phosphorus content, from 1-Ti ^ to Kb-j and the forms you will find on the polyphenols of ΪΦ ^ 5 ^{what about il0V?}· Ion: ·. of phosphorus discovered by Requires. te (EQ?_V in q &amp; e χ ό larger than 3.5), which all have parallel tube structure, if stable, if stable, will be useful semiconductor materials, barring s. inclusion of elements that act as traps, causing the formation of grain boundaries or the like.

ii .; All these materials that get you:? the parallel parallel pentagonal tubular structure, the investigations made by the Applicant indicate that a; multiple continuous covalent phosphorus-phosphorus bonds in the tubes which are substantially larger in size, whereas the number of other bonds will provide primary electrically conductive pathways for the electrons and gaps and thus provide good semiconductor properties. It is also the Applicant's opinion that the presence of alkaline alkaloids in the charge, even when combined, results in minimal traces in the new phosphorus furnaces that the Applicant has discovered promotes the erccinento of materials in which they maintain same structural and electronic properties as monocyclic phosphorus, depending on the conditions of deposition.

The family of semiconductor members to which the invention is directed comprises high phosphorus polyphosphors having the formula wherein the alkoxide of an alkali metal of the group i and i is the atomic ratio of phosphor metal atoms. , x being monos skin equal to? Suitable metal group members are Xi, Ra, K, Rb, Os, Eabora. Assuming that the francium is suitable, it is very rare, not involved in any known synthesis of radioactive PII. The inventors have prepared and tested high phosphorus polyphorphs wherein Ϊ1 includes Xi, fu, E, Rb or Os'.

The polyphosphide compounds according to the present invention are such. . · Are currently defined they must contain an alkali metal .. Some of the new forms of phosphorus will have to be formed in the presence

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of minimum quantities if not even non-measurable quuctuities of alceliuo metal₀ However, other rates may also be present and in high quantities such as, for example, ₆ riopantes or impurities.

and coconut was found late in the afternoon. new form of phosphorus_s was synthesized primarily as follows below and then_O

As shown in Figure 1, a furnace with a temperature of 10 ° C, having a terry 12 preferably constructed of iron; 1 outer jacket 12 is enclosed by clothing. The thermal insulation of an asbestos fabric 14 which may comprise an asbestos fabric has been constructed in the inventors' laboratory.

An atomic ratio P / E equal to about one dose (12) was obtained with reagents 56 in iemo 10_çChorus an illustrative example_The 5g5% of the true phosphorus, and C6.6 potassium were transferred under nitrogen to the quartz tube 52. The transfer was washed repeatedly after acetone and air dried. . However, such washing is considered to be specific as well as the solvent chosen.

After being loaded with ca 1'agents

36 »tube 52 was subjected to a vacuum equal to or equal to

-4 .

Trcr_s sealed and placed in the end 1C-> G tube 52 was mixed with a li. .tilt into hunger. The electric power supplied to the conductors 24 and 26 was adjusted to set the temperature gradient of, for example, 65G^ÇFrom 30 ° C to 30 ° C from the hot seine 28 to the hot zone 36. With the above described slope within the oven 10, the reagents 56 were certainly located in the warmest temperature range 28 '. After keeping the furnace 10 in these conditions for a long time, for example approximately 4-2 hours, the power supply to the eeutheree 24 and 6 was interrupted and the tube 32 allowed to cool. ce atln

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_w52? At room temperature, tube 32 was cut open cr. uv.r. cf teocfcra fie asoto and the contents of the tu'O? 2 were removed. The contents of the tube were then washed with

O--.ro. of pyrophoric materials, obtaining^w “* Approx. 2'g of stable product. That means an increase of approximately 33 percent.

Using this method of curing, several phases of the resulting resultant product appeared at well defined positions within the tube 32 as shown in the Figure. 2". A dark gray residue

4-C adjacent to a yellowish brown film 42 is typically produced at the end of the hot zone 30, which the reactants 36 are initially positioned, along the direction of decreasing temperatures along the tube 32, are at: there are deposits of the film. black to purple 42 which are a polycrystalline material. Following deposits on film 42 is an abrupt ring of a crystallite mass 44, and adjacent to the crystallites 44 is one. light area where thin strands develop 46.

A highly reflective coating or film deposit 48 is found in the lower portion of the tube 32 at the beginning of cold ninth 28. Above the film deposit 48 there appears to be a thin red film deposit. 50, depending on the temperature maintained in that zone. Deposits 48 and 50 may be polyether, amorphous or a mixture of polycrystalline and amorphous material depending on reagents and temperature. The end of the cold zone 28 is in a pocket or a deposit of film 52 which is airfoil material.

As there is a continuous temperature range from the hot zone to the cold sound of the reaction tube shown in Figures 2, the nature of the deposited materials varies continuously from very fine high quality crystalline yarns to polystalline and amorphous. To control the reaction and attempt to deposit large areas of uniform layers of material, a three zone furnace was constructed as represented by

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According to this embodiment shown the three zone oven 54 is essentially identical to the oven 10 shown in Figure 1, wherein the oven 54 comprises an outer iron jacket 56, a pipe 60 or a pipe of reaction ·. 58 '. Oom the end. For simplicity, the ammonia windings around the outer jacket 56 and tube 58 have been omitted in Figure 3. Iron 546 is different from oven 10 in that tube 58 is much longer compared to tube 32 and preferably is of the order of 48 cm in length. In addition, oven 54 is associated with three of these. distinct heated zones 62, 64 and b6 which are individually controllable to create a definite teratural gradient along tube 60. Tube 60 may be supported by blocks of. 08 and 70 so as to ensure a bias of the tube 60 and the reaction tube towards the heated zone 62 to maintain the reagents 36 in the appropriate position.

The preparation of very fine PE yarns was made,_r Very good quality using fixed temperature, 55 °, 475 and F ° O degrees Liver G! Λ CuS erucvidac zones 62, 64 and 66, r. .. ^ ectively. Yeri sc also qu-c the volumous deposits generated in the ceiling

10, when loaded into the inner core 60 of oven 54 or so heated to the temperature gradient identified above, would purify to form film deposits, such as films 4 &amp; 52 shown in Figure 2, but only when employed a zone which was heated to a high temperature of at least 40-4.55 b.

f? Information on the structural cell unit and crystals produced according to the process described above were obtained by X-ray diffraction assays with a single monocrystall and performed with an automated diffractometer. A 100 micron diameter fibrous monocrotal was chosen and mounted on a fiberglass. The structure was detained by direct processes using a total of 2,544 independent reflections. All atoms were iccalised by an electron map and Fonrier differential synthesis.

Typical needle-like crystals were: ni examined χ: οι · high magnification and electron scanning (S3i). Photographs 335 ·? * Resultent-s th. Cross-section of the needles show that the needles appear to be made up of dense fibrils rather than echo tubes. A sharp, twin-stranded twinning of crystals also discernible in:^Γ*15 ^:^^s Figures 7 and 8, the primary fibril diameter of the firo-wire crystals is estimated to be approximately 0.1-0.2 microns. The naive fibrils appear to have an optimal structure consisting of blades of approximately 500 μm thick.

From the study of the initial crystal refining data, the stoichiometry of the potassium phosphorus stew compound appears to be Ee.

The atomic structure of the phosphorus of the oponest is lined by identical unitary tubes with a pentagonal straight section. The tubes are one-dimensional;

,: x long direction of needle axis. The phosphor tubes are parallel to each other. ' In the simplest description, two separate double phosphor tubes are connected by a layer of potassium atoms. As calculated by the interathnic distances, the atoms of E are at least partially ionically linked with atoms f and j. A section view of a thin wire is shown in Figure 5.

More specifically, each potassium looanalysis is associated with a rigid unit of 15 phosphorus atoms having a structure as shown. In this rigid unit all phosphorus atoms except one are joined to three other phosphorus atoms. The other phosphorus atoms are in the chain, and the missing bonds attached to a potassium atom are not represented. Figure 5 Thus, the potassium atom appears to connect tubular phosphorus units by air from an E-3? absent. In the structure investigated, the

There '·

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potío-ic has atoms of fofofcr οοη, ο mie neighbors near distances 3.6 A, 2_;Δ9 A and 2.76 A, respectively. The distances ϊ-i range from 2.13 A to 2, bò A *. Binding angles in phosphorus chains range from 87 to 113^The is at. average is 102s, arsenic gives a layered structure which It has a mean bonding angle of 98 if it is not known to be a useful semiconductor. Black phosphorus has a similar width to a bond angle equal to. 96a ', triple-atom atoms which can form their three bonds at the interval 87^The 113- with an average value greater than op5 may form our chained structure of

If the covalent bonds are present, the material can be expected to have the same electronic properties of IA ...

Table X indicates the values ​​of the crystalline reticulum parameters - the atomic positions., And are determined for c - ---, crystalline.

TA Ε Ε Ε A: 1 xerânctrcc do.crystalline lattice for KF ^

Tricyclic system unit cell parameters a - y, u7 A ° 0.13)^Q b = 11.912 A *³ 0.10) A ° c »7.172 A ° C + -0.15) A °

CX = 101.4 (± 0.1) ° / 9 = 107.9 (± 0.2) °% = 89.3 (± 0.1; °

The initiation cell is primitive with one molecule per unit cell and a volume of 723.3 cubic angstroms *.

ί &amp; α-ρο from space x'j

At the highest symmetry that can only be achieved with the above structural configuration is a group of space_no center-symmetric with the cstequiometría given by

The raios-ray diffraction values ​​by _PCorresponding δ3 for c polioristaliuc material IX, color. copper lighting are shown in Figure 9 „

I show the spacing d with: .the corresponding intensities of dc reiea-Σ.

Similar X-ray powder direction values ​​were observed for fine yarn and colicrystalline materials. how

I. = li, Na, K Kb and Cs,

Tf all of these isostructural elements, the stamural skeleton can be considered to be lined by parallel pentagonal phosphor tubes,

These pipes are connected by a 1-EM ™ bridge.

For rigid units for this type of solid structure, the building block can be considered as cu txp.

Therefore:

<i> huh?₇) ·£» 20?₄) —— which represents the basic structure.

Similarly, water from the building blocks in such compounds may be present in much greater amounts than the other. In the case of EQ? , for example, 2> there may be building blocks of (E & p and (ΐ ^ ,, ί which are present in a ratio of & to b, respectively. Ob CL LC.

and that mathematically x »(7a ❖ 8b) / ^ a).

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It is also possible to have a behavior, b tc-r a much larger value than a and have the same basic structural arrangement '.

This type of polymer-like tubular structure will result in "K-type" thin fibers or yarns with x much larger than 15 "polycrystal" fiber and fiber "yarns". with a value of x much higher than • UI

1COO (K = Xi, Ra, Kj Rb, Ce) it was found that crystallization at low temperature (about 400 ° C) using the vapor transport technique. The 3-X ray diffraction data in material powders are substantially the same. . Data for K3? „Cm where x is much larger than 15 under copper illumination is shown in Figure 10.»

Fuck yourself compares? the structure described above is that of other structures based on pentagonal straight section phosphor tubes. The compound KP3. is iso esna trutural with liP,_r.-j Ma

Lt r- &lt;

go

Rb Cs The other alkali metals seem to play the same role3. from K »

From the structural data, it is concluded that numerous ctopocytes can be formed which will be based on pentagor straight section tubular building blocks. We have found that in phosphorus materials, partially, phosphorus atoms can be replaced by atoms of other elements of the phosphorus family, such as As, Bi, Sb. Substitution of up to 50 percent atoms is possible without adversely affecting the basic structure of high phosphorus t-β polyphosphs'.

Table II lists the various synthesized compounds Ki ... in which the same structure was determined.

Crystalline KCl5 as r-oyster a X-ray powder diffraction »typical analysis

BELA 11

Hard Drives

EFj ©

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Building blocks

Lyrical Structure

Ks (B₄-I3>₅) or 6 · ϊ₇) and>₆) (P1 -lly-Pp or (¹¾)

Li, La, and, Kb, Cs

IsostructiD Compounds with Lt-, ς Crystalline

Vl-x hs-y cen: C x ith 1 7Ã 7.5

It's the La group

3rd group 5a (ds, Li, 5b)

Initially, the inventors have discovered as mentioned earlier, that the crystalline fines produced in the apparatus are shown in FIGS. now that the thin strands K? .4, had varying ectequionetric proportions of ΧΙ '^ θ cqq » ^and surprisingly no control of temperatures in the three famine zones represented in Haura. 3 would produce amorphous ovens from Eâ? ^. It was therefore necessary to refine the processes of production of these materials and to attempt a new vapor transport apparatus from two sources to produce succinctly amorphous polycrystalline EB3 materials, which are thought to be very new. phosphorus gallows, They were also prepared by this process which consists of depositing initially 25 and subsequently cutting off the source of alkaline ketal where only phosphorus vapor is pre-disposed for phosphorus deposition. Furthermore, the condensed phase process has been investigated side by side. 'u -sa nd 0 molar loads of E? .. materials and where x varies between · 7 and 15 were investigated, East ... oroccse, as x;

rsoteraxcami i? · '4 *.

closed. The Requc IlE materials. norpium crystal;

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These are heated and the reaction is safe.

It follows that processes which were high-grade inter alia measuring the characteristics produced a wide variety of these: so that they are constituted in the crystalline crystals.

detailed description nailed to synthesize nasphorus and the way it is electro-optic and has been shown to be useful conductors.

Irrigation of Applicable Techniques of. Transport from one, the Source \ Tfc.'J ca c Fcsíore Content Ifede Steam Prevenir.j \ e «t * ι - ew Ta! -'ΛΓ'ολ'υ energy to a sirtena to create vapor species that give rise to products by condensation or deposition at appropriate temperatures is called vapor transport. For the following discussion, in which the materials of the force are kept in close contact and heated. at dc at approximately the same temperature, the following description applies as a single source technique.

The methodology described by Von Schnering was essentially a single-source vapor transport technique, although the load sometimes consisted of separate meth) and phosphorus packages heated to approximately the same temperatures. However, the flow of vapor species to the deposition zones was indeed the same when metal and phosphorus are primarily mixed together, more specifically in the single source vapor transport species. together at a high temperature and then deposit at a low temperature.

steam are first brought

Hey sefuida, it describes the developed:? ·

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Applicant as applied for the preparation of alkali metal polyphosphors and the departure from the Von Schnering process, which results in an improved, more selective preparation of crystalline metal polyphosphides of the type. KD-5, and low alkali metal polyphosphorides, polycrystalline material, type io_χ where x is much larger than 15, and is a new form of phosphorus phosphor, wherein the alum metal tsor can be less than 50 ppm (parts per million).

The studies carried out by the Applicant are divided into several categories: type of load, proportion of load constituents, tube length and geometry, and temperature gradient profile. The following examples illustrate the deposition ratios of the temperature dependent products that the Applicant has discovered and the temperature control processes in the selective preparation of desired prices.

General Information

An alkali metal and red phosphorus are introduced into. four-sealed tubes, under reduced pressures (about 10-4 Torr), The atomic proportions between the two elements vary between 5/1 and 30/1, with 15 for the proportion of the charge. more with; · ...

The elements are generally placed in a mill. as a whole, before loading the quartz tubes, the grinding is carried out on the stainless steel balls with the ball mills and lasts for at least 40 hours. The mills are usually heated to durante ^ δ during grinding to help disperse the metal in the red phosphorus powder,

The grinding allows to achieve an intimate contact of the two elements in a way as homogeneous as possible. Milling products are usually fine powders that are easily handled in a dry box and can be stored without any further detail.

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vieivei_ώ The wells have a remarkable stability when exposed to air and moisture, when compared with the ectubilations of their constituents, especially the alkaline rectal stability. For example, the precise addition of water and paddles will result in combustion of randomized materials and in a small comparison of the crystalline and amorphous polycrystal materials.

A mixture of the elements (alkali metal and red phosphorus) is introduced into the reduced pressure [ca. from cccprirentc by 2_Ç5th cc diameter. The tube 58 is supported within the heating range of a 3-hour row. lindberg 24357-3 uca of the two scenarios indicated as' guiòa 'A process employs a second tube of cuaría 60 coconut support piece, which is, in its voice, centered on the chamber,' far from the heating elements, by asbestos blocks 68 and 70, whereby coupled tubes rest tilted, will ensure that the reagents remain in the drop and warm zone. Another process (figuralX4) is the use of woven tape constructed supports 137; 139 is wound around the reaction tube in an expanding spiral, 2.54 ca (one inch) wide and filling the recirculated section of the heating curve. This woven tape asks for sar made from a variety of materials: Asbestos, Mberirax (ãa^noCarb &amp; rundum Corpany®) or '' glass grit. Are the implications of using both processes described below?

• · Reagents are transformed into products by applying energy to the shell through the strength and strength of the force. »Reagents are applied at a sufficiently high temperature while · 0 VV

<img file="PT76047B_D0037.tif" />

Other parts of the tube are stripped to the appropriate lower temperature, the products will deposit or condense from the vapor species. The crater torch differential which causes this so-called steam synthesis is achieved in a 3-zone furnace by choosing different temperature values ​​for the individually controlled heating elements.

Ϋ.ΟΰΕΰαϋ 1 - 7 is shown in Figure 3. The 50 cn tube which has tt. The ragents is maintained by the second quartz tube! Wow gold. heating of 61 in. application of a thermal gradient by controlling the 3 set temperature values ​​gives a decreasing gradient now. That is, the slope of the gzafiiI into, Δδ / d, where T is the temperature effected along the chamber, is approximately constant and | between the centers of the two elsncn^- and external heating i This linear gradient, applied over the long! The dimensions of the tube work to separate the wood from the materials lined in the reaction. Products appear © distributed according to

P ; cmv characteristic fear at decreasing deposition temperature: dark purple films; r. black polyioricteilines; a ring of Christian tiles on our walls; single crystals or fine wires; 'j nomelbas pots' film: Pecans of morphology of pecan grains at colder temperatures, dark gray amorphous material.

A number of experiments have shown that morphological activity will not form in these sealed tubes and only when the coldest temperature is higher than the 575 ° C crown. In the same way, the occurrence of the red crystalline material could be greatly reduced by maintaining the temperatures. - lower than 450-0 or greater than this tc.nperaturai

The Applicant also found that ο - · ”Ρ_ΊCrystalline poly does not form in a single source apparatus. The polycrystalline and amorphous materials for!

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where x is much larger than 15; woven serve not to orient the reaction tube .as also as Home:

These are the focal points for heat transfer between the three heating zones. These barriers originated diicrencas

Tira .- 'steeper strip between zones on a sloping nunes gradient within the center zone. A result is a stepped-type temperature profile which can be controlled to produce products constantly by adopting appropriate ranges. deposition temperatures.

A. Determination of Fre Deposition Temperatures:

There is von Schnering's description of the preparation of nonocristcls (fios?_Ί^), he referred to the preparation from the elements by imposing the heating of the elements potassium and red phosphorus - con ur _Otemperature ratio of S00 / 20020, in a quartz tube approximately 20 ~ 20 »He further states that the crystals form between ^,!> C and 32020 «, the ovens used pray the famine of single-element or; that the gradient is caused by the heat loss of some. end tubosο pipes that are placed in the oven,

As the first improvement introduced in this procedure, a three zone furnace was used, each of which is shown in Figure 3 with independently controlled heating elements and a heating chamber of 61 cm. in length (Model Iiindberg 543^rY, oven and zones will reach and control the gradi after the diode. By supporting the reaction tube, which has now been extended to approximately 52 ca in length by a second open quartz tube, which was in turn supported by asbestos tubes, a generally linear temperature gradient, ZXf, was obtained. / d, near constant change between the centers of the two extremes of extreme heating. The energy for this '-ά' V &lt;_

<img file="PT76047B_D0039.tif" />

chlorinates was controlled by a Hcdelo liindbcrg 53'744-À Control Console, which uses, three proportional indefinite dv controller SCfí to maintain! to tsmoGr «.uu shrunk by? middle of aoci wheels. nr.erto co 'ruorclton manually adjusted »

The decreasing linear gradient, | applied and long of the relatively large pipe dimensions^{, Ί}The rooting served to cleanly separate the variety of materials from different primed products ”to the reaction. The products line up according to ume. caructoritic distribution at deposition temperature in addition to purplish films. dark to crystalline black; honey of crystalline single-crystal or thin-chewed cheeses₀polycrystalline, small grain, not cold temperatures, amorphous materials, colored cinaonta xscurá,

* íi ij In this example, a 5 || xZodclo lindberg 54357 as shown in section 2, figure 3, comprising heating elements embedded in refractory material in separate cylindrical sections of lengths equal to 15.3 cm, 50.6 cm and 15, 3 cm, so as to obtain a total length of the chamber with a length of 61 cm. The chamber diameter is equal to 8 in. Sermon control pairs (not shown) · are located about the i

i 7.0, 30.5, 55.5 cm over the length of 61 cm. i 'the firsts' .a camera ds aquecinen !. were tarnished with glass wool to minimize the heat of the oven. A quartz tube with a disfoometer equal to 4.5 cm and 60 cm long was maintained with a minimum inclination swallow by means of blocks; ds riiauto in the heating chamber.

} The quartz reaction tube had a rounded bottom, 49 cm long and 2.5 cm long.

<img file="PT76047B_D0040.tif" />

diameter reduced to a tube I narrow edition 10 cm in length by 1.0 ca in width. Under a dry atmosphere, 6.51% of red phosphorus and 0.62 g of potassium were transferred to the tube. The ratio atom: phosphorus atom to the metal was equal

1. Phosphorus was reagent grade (.T, T_Ç labor).

Tc-rr θ is sealed by means of some cn of the widest part of the pipe ie adi •? ibo was evacuated at r-edo and the total length equal to 51 tube was placed in the 3 ninth oven as described above and the temperature values ​​of the three dolly were set to 650 ^ 0, 450-0 and 3CO2S over a period of 5 hours and stored for another 164 hours. The power was turned off and the oven was allowed to cool to room temperature with the inherent cooling rate of the oven. The tube was tinted under an atmosphere le αζοτο punch chrrrné ccn

Lysiim with crystalline forms.

Table 3 shows the different processing parameters used also for. other tests together with the types of products obtained en. In each test, before opening the aperture, the tubes of the first three tests were inspected for the positions along the tubes of the various products: the dark crystal ring in the pot and the start of red polycrystalline films *. Thin strands were always observed between these two points. These positions were subsequently correlated with the gradients created by the annotated defined temperature values. These data are summarized in Table IV.

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<td></td><td></td><td>MO</td><td>O</td><td>•P</td><td>m</td><td></td>

<td></td><td></td><td>ro</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>p4</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>m</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>here</td><td> •</td><td></td><td></td><td>Z “\</td>

<td></td><td></td><td>frog</td><td> &amp;</td><td></td><td></td><td>O</td>

<td>ί</td><td></td><td>g</td><td>The</td><td></td><td></td><td>rd</td>

<td></td><td></td><td> +⁵</td><td>ro</td><td></td><td></td><td>Ky</td>

<td> 1</td><td></td><td>there</td><td>EH</td><td></td><td></td><td></td>

<td></td><td></td><td>Pi</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>ro</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td> &amp;</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>The</td><td>laugh</td><td></td><td></td><td></td>

<td></td><td></td><td>ro</td><td>O</td><td></td><td></td><td></td>

<td></td><td></td><td>EH</td><td>M</td><td></td><td></td><td>z- \</td>

<td>V</td><td></td><td rowspan="2">frog</td><td>H</td><td>frog</td><td></td><td>cn</td>

<td>t</td><td></td><td>ro</td><td>frog</td><td></td><td>&lt;_z</td>

<td>ΐί</td><td></td><td>there</td><td rowspan="2">PM</td><td>H</td><td></td><td></td>

<td>I</td><td></td><td>ad</td><td></td><td></td><td></td>

<td> 4</td><td></td><td></td><td> •</td><td></td><td></td><td></td>

<td> (</td><td></td><td>O</td><td>PM</td><td></td><td></td><td></td>

<td></td><td></td><td>will</td><td>s</td><td></td><td></td><td></td>

<td></td><td> &gt;</td><td>O,</td><td>ro</td><td></td><td></td><td> 00</td>

<td></td><td>H</td><td>s frog</td><td>EH</td><td></td><td></td><td>Vz »</td>

<td> 1</td><td> &lt;4</td><td>oh The</td><td></td><td></td><td></td><td></td>

<td> 1</td><td>THE</td><td>ro</td><td>rH</td><td></td><td></td><td></td>

<td></td><td rowspan="2"></td><td rowspan="2">M1</td><td>ro</td><td></td><td></td><td>Z ~ S</td>

<td> 1;</td><td>frog</td><td></td><td></td><td>O</td>

<td></td><td></td><td></td><td> &lt;4</td><td></td><td> »</td><td></td>

<td></td><td> «</td><td>ro</td><td></td><td></td><td></td><td></td>

<td>ij</td><td></td><td>ad</td><td></td><td></td><td></td><td></td>

<td>ί</td><td> «4</td><td>frog</td><td></td><td></td><td></td><td></td>

<td>ll</td><td>EH</td><td>ro</td><td></td><td></td><td></td><td></td>

<td> '}</td><td></td><td>OH</td><td>O</td><td></td><td></td><td></td>

<td></td><td></td><td>O</td><td> &amp;</td><td></td><td></td><td>Z ~ M</td>

<td></td><td></td><td>lj</td><td>The</td><td></td><td></td><td>GRANDFATHER</td>

<td></td><td></td><td>frog</td><td>ro</td><td></td><td></td><td>v_z</td>

<td>J</td><td></td><td>f »</td><td>EH</td><td></td><td></td><td></td>

<td></td><td></td><td>m</td><td></td><td></td><td></td><td></td>

<td>j,</td><td></td><td>O</td><td></td><td></td><td></td><td></td>

<td>ll</td><td></td><td>iti</td><td></td><td></td><td></td><td></td>

<td>l ·</td><td></td><td>there</td><td></td><td></td><td></td><td></td>

<td> ;·</td><td></td><td>ϊ&gt;</td><td>m</td><td></td><td></td><td>m</td>

<td>ij</td><td></td><td>ro</td><td rowspan="2">EH</td><td></td><td></td><td></td>

<td></td><td></td><td>H</td><td></td><td></td><td></td>

<td>Ί 11</td><td></td><td>ro</td><td></td><td></td><td></td><td></td>

<td>i;</td><td></td><td>The</td><td></td><td></td><td></td><td>z— * »</td>

<td></td><td></td><td>O</td><td>CM</td><td></td><td></td><td>'st</td>

<td></td><td></td><td>O</td><td>EH</td><td></td><td></td><td></td>

<td></td><td></td><td>frog</td><td></td><td></td><td></td><td></td>

<td> •_r.</td><td></td><td>O</td><td></td><td></td><td></td><td>«Zs</td>

<td></td><td></td><td>-P</td><td>. rH</td><td></td><td></td><td>ΓΠ</td>

<td> 5'</td><td></td><td>frog</td><td>EH</td><td></td><td></td><td>S-/</td>

<td>jí</td><td></td><td>d</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>O</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>JH</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>PM</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td rowspan="2">M</td><td>THE</td><td></td><td></td><td></td>

<td></td><td></td><td>• laughs</td><td></td><td></td><td>z— \</td>

<td></td><td></td><td>O</td><td></td><td></td><td></td><td>Ç \ 1</td>

<td></td><td></td><td>• d</td><td>frog</td><td></td><td></td><td>VuZ</td>

<td></td><td></td><td></td><td>ro</td><td></td><td></td><td></td>

<td></td><td></td><td>O will</td><td>THE</td><td></td><td></td><td></td>

<td></td><td></td><td>Hi</td><td></td><td></td><td></td><td></td>

<td>_t.</td><td></td><td>• rl</td><td> •</td><td></td><td></td><td></td>

<td></td><td></td><td>frog</td><td></td><td></td><td></td><td></td>

<td>lj</td><td></td><td>O</td><td>ro</td><td>Hi</td><td></td><td>rd</td>

<td>u</td><td></td><td>PM</td><td> (4</td><td>S3</td><td></td><td>SwZ *</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>Hello</td><td>Hello</td><td>Hello</td><td>Hello</td><td>Hello</td>

<td>O</td><td>The</td><td>THE</td><td>THE</td><td>THE</td>

<td>M-</td><td>rO</td><td>M ·</td><td>THE</td><td>M-</td>

<td>s</td><td>s</td><td>The</td><td>The</td><td>The</td>

<td>O</td><td>O</td><td> □</td><td>O</td><td>O</td>

<td>M *</td><td>The</td><td>O</td><td>THE</td><td>THE</td>

<td></td><td> *</td><td>• k</td><td> ·»</td><td>• k</td>

<td></td><td>CO</td><td>m H</td><td>CO H</td><td>ro H</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>Hello</td><td>Hello</td><td>Hello</td><td>Hello</td><td>hello</td>

<td>THE</td><td>O</td><td>O</td><td>THE</td><td>O</td>

<td>m</td><td>THE</td><td>CO</td><td>THE</td><td>THE</td>

<td>M-</td><td>M-</td><td>M-</td><td>M-</td><td>M ·</td>

<td>The</td><td>The</td><td>The</td><td>The</td><td>The</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>O</td><td>O</td><td>THE</td><td>THE</td><td>O</td>

<td>«K</td><td> *</td><td> *</td><td>• k</td><td>• k</td>

<td>O</td><td>co</td><td>CO</td><td>M-</td><td>CM</td>

<td>co</td><td>rn</td><td>rO</td><td>rn</td><td>M-</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>Hello</td><td>Hello</td><td>Hello</td><td>ot</td><td>Hello</td>

<td>THE</td><td>tn</td><td>THE</td><td>O</td><td>THE</td>

<td>t&gt;</td><td>co</td><td>O</td><td>H</td><td>CO</td>

<td>M-</td><td>M-</td><td>THE</td><td>THE</td><td>M-</td>

<td>The</td><td>The</td><td>The</td><td>The</td><td>The</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>O</td><td>IA</td><td>THE</td><td>O</td><td>THE</td>

<td>• t</td><td> «.</td><td> ·&gt;</td><td>• k</td><td>K</td>

<td>Md</td><td>co</td><td>m</td><td>CO</td><td> 00</td>

<td>CM</td><td>CM</td><td>CM</td><td>CM</td><td>CM</td>

<td>frog</td><td>frog</td><td>frog</td><td>frog</td><td>frog</td>

<td>frog</td><td>frog</td><td>frog</td><td>there</td><td>frog</td>

<td>• rl</td><td>• rl</td><td>• rl</td><td>• rl</td><td>• rl</td>

<td>na</td><td>d</td><td>d</td><td>d</td><td>• d</td>

<td>Γ</td><td>THERE</td><td>O H</td><td>co</td><td>CO</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>O</td><td>THE</td><td>O</td><td>O</td><td rowspan="2"> $</td>

<td>CO</td><td>CO</td><td>Μ-</td><td>Μ-</td>

<td>O</td><td>THE</td><td>Α</td><td>Α</td><td>THE</td>

<td>The</td><td>CO</td><td>t&gt;</td><td> 00</td><td>CO</td>

<td>• «</td><td>M</td><td>M-</td><td>M-</td><td>Μ-</td>

<td>ο</td><td>O</td><td>O</td><td>O</td><td>Α</td>

<td>The</td><td>O</td><td>THE</td><td>H</td><td>rH</td>

<td>co</td><td>CO</td><td>THE</td><td>co</td><td>CO</td>

<td>&lt;-N</td><td>O</td><td>x - '*</td><td>x ^&gt;</td><td>z ~ \</td>

<td>H</td><td>CM</td><td>CO</td><td>M-</td><td>THE</td>

<td>rH</td><td>CM</td><td>CO</td><td>co</td><td>CO</td>

<img file="PT76047B_D0045.tif" />

<td colspan="9">ro</td>

<td></td><td> 02</td><td></td><td></td><td></td><td>frog</td><td></td><td></td><td></td>

<td></td><td>Ctf</td><td></td><td> *</td><td></td><td>ctf</td><td></td><td></td><td></td>

<td></td><td>YOU</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>ctf</td><td></td><td> 02</td><td></td><td> ©</td><td></td><td></td><td></td>

<td></td><td>Fi</td><td></td><td>Ph</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>ctf</td><td></td><td></td><td></td><td>r4</td><td></td><td></td><td></td>

<td></td><td></td><td></td><td>O</td><td></td><td> ©</td><td></td><td></td><td></td>

<td></td><td> ©</td><td></td><td>JCtf</td><td></td><td>laugh</td><td></td><td></td><td></td>

<td></td><td> 02</td><td></td><td>O)</td><td></td><td>ctf</td><td></td><td></td><td></td>

<td></td><td></td><td></td><td>O</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td> 02</td><td></td><td>ctf</td><td></td><td>O</td><td></td><td></td><td></td>

<td></td><td>d</td><td></td><td>Φ</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>fc</td><td></td><td>Fi</td><td></td><td> ©</td><td></td><td></td><td></td>

<td></td><td>•P</td><td></td><td></td><td></td><td>Fi</td><td></td><td></td><td></td>

<td></td><td> 02</td><td></td><td> ©</td><td></td><td>-P</td><td></td><td></td><td></td>

<td></td><td>O</td><td></td><td>YOU</td><td></td><td>laugh</td><td></td><td></td><td></td>

<td></td><td>s</td><td></td><td></td><td></td><td> ©</td><td></td><td></td><td></td>

<td></td><td>s</td><td></td><td>O</td><td></td><td></td><td></td><td> «</td><td></td>

<td></td><td></td><td></td><td>•H</td><td></td><td>O</td><td></td><td>O</td><td></td>

<td></td><td>s</td><td></td><td>ctf</td><td></td><td>o&gt;</td><td></td><td> 01</td><td></td>

<td></td><td>O</td><td></td><td> 02</td><td></td><td>d</td><td></td><td>LT \</td><td></td>

<td></td><td>O</td><td></td><td>laugh</td><td></td><td>laugh</td><td></td><td></td><td>and</td>

<td></td><td></td><td></td><td> ©</td><td></td><td> 02</td><td></td><td></td><td>The</td>

<td></td><td> ©</td><td></td><td></td><td></td><td> ©</td><td></td><td>Ή</td><td>O</td>

<td></td><td>-P</td><td></td><td>O</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>laugh</td><td></td><td>laugh</td><td></td><td>O</td><td></td><td> ©</td><td>IT \</td>

<td></td><td>Φ</td><td></td><td></td><td></td><td>laugh</td><td></td><td>OK</td><td>Λ</td>

<td></td><td>The</td><td></td><td> 02</td><td></td><td></td><td></td><td></td><td>O</td>

<td></td><td> ©</td><td></td><td>O</td><td></td><td>frog</td><td></td><td>fc</td><td></td>

<td></td><td> +3</td><td></td><td>YOU</td><td></td><td>d</td><td></td><td> 0</td><td> +1</td>

<td> •</td><td>fl</td><td></td><td>ctf</td><td></td><td>fc</td><td></td><td></td><td></td>

<td></td><td> 02</td><td></td><td> 02</td><td></td><td> 445</td><td></td><td>• rl</td><td>ω</td>

<td>s</td><td>YOU</td><td></td><td>laugh</td><td></td><td>frog</td><td></td><td>fc</td><td>&lt;d</td>

<td>O</td><td>laugh</td><td></td><td></td><td></td><td> 0</td><td></td><td></td><td></td>

<td>O</td><td> 02</td><td></td><td>O</td><td></td><td>£</td><td></td><td>O</td><td>you</td>

<td></td><td>laughs »</td><td></td><td>•P</td><td></td><td> 3</td><td></td><td></td><td> 0</td>

<td> 1</td><td> 02</td><td></td><td>laugh</td><td></td><td></td><td></td><td>s</td><td>Μ</td>

<td></td><td>you</td><td></td><td>φ</td><td></td><td>frog</td><td></td><td> 0</td><td>• laughs</td>

<td></td><td>laugh</td><td></td><td>The</td><td></td><td>ctf</td><td></td><td>O</td><td>fc</td>

<td></td><td>•H</td><td></td><td>•H</td><td></td><td></td><td></td><td></td><td></td>

<td>H</td><td></td><td></td><td>O</td><td></td><td> 02</td><td></td><td> 02</td><td> 0</td>

<td></td><td> 02</td><td></td><td> ©</td><td></td><td>ctf</td><td></td><td>d</td><td> 0</td>

<td></td><td>O</td><td></td><td>laugh</td><td></td><td>OK</td><td></td><td>-P</td><td>O</td>

<td> «4</td><td>YOU</td><td></td><td>σ¹</td><td></td><td> 0</td><td></td><td>•H</td><td></td>

<td></td><td>Ctf</td><td></td><td>ctf</td><td></td><td>P</td><td></td><td> ©</td><td>frog</td>

<td>THE</td><td> 02</td><td></td><td> ©</td><td></td><td></td><td></td><td></td><td>ctf</td>

<td></td><td>laugh</td><td></td><td>Fi</td><td></td><td>The</td><td></td><td></td><td>-P</td>

<td>Pi</td><td></td><td></td><td></td><td></td><td> ©</td><td></td><td>O</td><td>•H</td>

<td></td><td> 02</td><td></td><td>φ</td><td></td><td></td><td></td><td>id</td><td>φ</td>

<td></td><td>O</td><td></td><td>OK</td><td></td><td> 0</td><td></td><td>frog</td><td>Ή</td>

<td></td><td>YOU</td><td></td><td></td><td></td><td>You</td><td></td><td></td><td></td>

<td>&lt;í</td><td>O</td><td></td><td>frog</td><td></td><td>laugh</td><td></td><td>d</td><td>O</td>

<td></td><td>•P</td><td></td><td>•H</td><td></td><td> ©</td><td></td><td>fc</td><td>id</td>

<td>E4</td><td></td><td></td><td>Qi</td><td></td><td>O</td><td></td><td>laugh</td><td>frog</td>

<td></td><td>j3</td><td></td><td>Fi</td><td></td><td>frog</td><td></td><td>•P</td><td></td>

<td></td><td>ctf</td><td></td><td> ©</td><td></td><td> 02</td><td></td><td>d</td><td> 0</td>

<td></td><td>Fi</td><td></td><td>laugh</td><td></td><td>fc</td><td></td><td>fc</td><td>2d</td>

<td></td><td>O</td><td></td><td></td><td></td><td> 0</td><td></td><td>φ</td><td> 0</td>

<td></td><td>"P</td><td></td><td>O</td><td></td><td></td><td></td><td>laugh</td><td>• laughs</td>

<td></td><td></td><td></td><td>iCtf</td><td></td><td>frog</td><td></td><td> 0</td><td>frog</td>

<td></td><td>CO</td><td></td><td>frog</td><td> «</td><td> 0</td><td></td><td> ©</td><td> 0</td>

<td></td><td></td><td></td><td></td><td>ro</td><td>• laughs</td><td></td><td>•P</td><td>Pi</td>

<td></td><td> ©</td><td> •</td><td>tr »</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>m</td><td></td><td>H</td><td></td><td></td><td> ©</td><td> ©</td>

<td></td><td>OJ</td><td>O</td><td> ©</td><td>Ή</td><td>frog</td><td></td><td>YOU</td><td>YOU</td>

<td></td><td> ·*</td><td>-P</td><td></td><td>THE</td><td> 0</td><td></td><td></td><td></td>

<td></td><td>THE</td><td>d</td><td></td><td>P</td><td>rd</td><td></td><td>frog</td><td>frog</td>

<td></td><td></td><td>d</td><td></td><td>φ</td><td>ctf</td><td></td><td>d</td><td>d</td>

<td></td><td>frog</td><td>O</td><td>frog</td><td>THE</td><td>laugh</td><td></td><td>fc</td><td>fc</td>

<td></td><td>• r)</td><td></td><td>M</td><td></td><td>O</td><td></td><td>laugh</td><td>laugh</td>

<td></td><td>THE</td><td>THE</td><td>"H</td><td>O</td><td>d</td><td> •</td><td>-P</td><td>-P</td>

<td></td><td></td><td></td><td>Fi</td><td></td><td></td><td>frog</td><td>• laughs</td><td>• rl</td>

<td></td><td> &lt;0</td><td></td><td>Φ</td><td>a&gt;</td><td> 0</td><td>d</td><td>Φ</td><td>Φ</td>

<td></td><td>Pi</td><td>d</td><td>laugh</td><td> +³</td><td> 3</td><td>OK</td><td>i ~ i</td><td>H</td>

<td></td><td></td><td></td><td></td><td>P</td><td>fc</td><td>d</td><td></td><td></td>

<td></td><td>frog</td><td>O</td><td>frog</td><td>d</td><td> 0</td><td>•P</td><td>frog</td><td>frog</td>

<td></td><td>O</td><td>Ico</td><td>O</td><td>The</td><td>laugh</td><td>• &lt;“i</td><td></td><td> &lt;3</td>

<td></td><td></td><td>O&gt;</td><td></td><td>H</td><td></td><td>frog</td><td></td><td></td>

<td></td><td></td><td>here</td><td></td><td>d</td><td></td><td> 0</td><td></td><td></td>

<td></td><td></td><td>B</td><td></td><td>you</td><td></td><td>laugh</td><td></td><td></td>

<td></td><td></td><td>csi</td><td></td><td>• laughs</td><td></td><td> ©</td><td></td><td></td>

<td></td><td></td><td>THE</td><td></td><td></td><td></td><td>you</td><td></td><td></td>

<td></td><td></td><td>φ</td><td></td><td>•H</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>f4</td><td></td><td>you</td><td></td><td>frog</td><td></td><td></td>

<td></td><td></td><td>THE</td><td></td><td>O</td><td></td><td>d</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td></td><td></td><td>H</td><td></td><td></td>

<td></td><td></td><td>tS</td><td></td><td>O</td><td></td><td>laugh</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>nrf</td><td></td><td> 0</td><td></td><td></td>

<td></td><td></td><td>tó</td><td></td><td>d</td><td></td><td>M</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>Qj</td><td></td><td>H</td><td></td><td></td>

<td></td><td></td><td>gJ</td><td></td><td>frog</td><td></td><td> ©</td><td></td><td></td>

<td></td><td></td><td>THE</td><td></td><td>you</td><td></td><td>P4</td><td></td><td></td>

The information provided by these tcmporatua ·.?. © the profint type; ΧΡ.ς seems to form along the peruro le?

Nonocrystals have a range of between which varies from 465-475^sFor example, the onset of deposition of cyclic crystalline red materials is equal to about 450%. In fact, the amorphous material deposited even when the lower temperature was about> 509 ° C. Cçuondo cs:> temperature was increased to 4CC not observed? formation of no amorphous material,

The test where this temperature was used, so often ended in a breakdown of the reaction tube so that the products could actually be used, and that the temperature-product ratio of amber material was confirmed in later tests using more advanced techniques). Assuming an average value of a, .., gv: u, the upper limit of the formation of amorphous material was considered to be about 375-0.

The pressures res the heated pipes. have not been measured.

3 2-Temperature radients that will favor the growth ds. nonocrystals,. (fine strands), ______________ „

Using knowledge of the relationships between c, product morphology and deposition temperature in Tables III and 17, we sought to improve the synthesis technique to allow greater grape type selectivity. temperature profiles, res femoo that would result in larger areas of the. surface of the tube within the appropriate temperature ranges for spun products. Several materials available with low thermal conductivity and easily manipulated shapes have been added for use as heat transfer barriers.

<img file="PT76047B_D0046.tif" />

We went. Delay asbestos fabric tapes * are a suitable product to support reaction tubes and create complex gradients, consisting of reasonably constant, or isothermal, temperature areas separated by areas (across barriers) with color decreases or temperature gradients. accented. f.The profiles called "v-type" were applied c *. all subsequent periods in which specific products with maximum yields were sought '

Another improvement that helped to obtain more reproducible temperature profiles of the essay for testing was to use ur. It is a type of solid material from the ceramic to fill the free space between the heating chamber and the wall. And in earlier rehearsals, this: • spaces were full of glass that helped to stop the loss of heat, but not very well. The large cylindrical clearances are n;_: es ns;> π._ώ post-redirect from the chamber as the dog ovens are not damaged so as to support a^noabout its length, may for applications col; flow passage, than closed systems, are being employed in these allologies.

The following examples have all aimed at trying y. The growth of larger macronutrients, such as better yields, both with respect to a percentage of the product sheets and an absolute yield. These results have really been achieved. ”

ESBfPIO II In this example, a forge of 3 schas of the identical Eido Lindberg 54 357 en des? and er. dimensions of that of Example I. Elements were also controlled in the same manner with. The. 59744-A Control Console manually regulated₀ The ends of the heating chamber were covered with a heat resistant ceramic type material to minimize heat

<img file="PT76047B_D0047.tif" />

The loss of heat in the oven. The reaction tube was supported if heated by two ring dc fit ·? i> anion fabric. One of them was situated at 16-19 ση the other between 42 and 45 ca along the chamber. This places both rings completely inside the central heating housing, adjacent to the joints of the central elements and the two outer sections. The rings were constructed so that the tube was inclined at a minimum angle '. C urol served ρ.ην to insulate the heating sonas a 't. another acting as a heat transfer barrier, the fourth reaction tube (Figure 3) had a rounded bottom, 48 inches in length by 2.5 cm in diameter, and redusifed to a narrow addition tube 162, with 10 cm long by 1,0 cm wide '; icb a atmosphere of asoto punch iatroused 5_f47 g! of vorv-cH10 phosphorus and 0.50 g of potassium within the tube. The atom atom: the phosphorus atom for metal was 15: 1. The phosphorus was 39.3999 b-pure. The potassium was 99.3% pure, the tube was evacuated at 10Â ° C Torr and sealed by melting. add tube to any. Entering meters: 1 from the widest part of the pipe so that the length 1 is equal to the crown of 52 cm. A sealed tube was placed in the 3-probe oven as described above and the three-probe temperature values ​​were pure pure, 475.^TheO is 450-0 for an interval [from 4 hours and stored for an additional 79 viruses. The power was immediately turned off in all three sounds and the oven was allowed to cool to room temperature at the inherent cooling rate of the oven. The tube was aborted by cutting under an atmosphere of dry soil in a glovebox. The | products consisted of crystalline and polycrystalline forms; lire.

Table V summarizes the processing parameter values ​​for a similar test range._; (given for the above example, those from the reference 10 test).

<img file="PT76047B_D0048.tif" />

Sound pressure

Ref. Proportion Grams Grams Torr. Τ_η . T_? T ^ VT / Total Length with <y> Η- Hro ro • d> of

μ £

od sS

<td></td><td>O JH</td><td>O μ</td><td>THE</td><td>O</td><td>O •s</td>

<td>O</td><td>ω</td><td>ro</td><td>CJ</td><td>CM</td><td>fH</td>

<td>tr \</td><td>O</td><td>O</td><td>THE</td><td>tn</td><td>tn</td>

cn

<td></td><td>kO</td><td colspan="4">kO</td>

<td>co</td><td>O</td><td>O</td><td></td><td></td><td>co</td>

<td>CM</td><td>H</td><td>H</td><td></td><td></td><td>O-</td>

<td></td><td></td><td></td><td>n-</td><td></td><td></td>

<td>H-</td><td>kO</td><td>kO</td><td>n-</td><td>* 3t</td><td>CM</td>

<td>CM</td><td>cn</td><td>ΟΊ</td><td>H</td><td>rH</td><td>r-</td>

co

The co

The knockout

O '&lt;0 • tf

Μ (Xj

ΟΙ

CJ rH

Χ «χ

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>THE</td><td>THE</td><td>THE</td><td>tn</td><td>in</td><td>tn</td>

<td>nj-</td><td></td><td></td><td>Π-</td><td>H-</td><td>H-</td>

<td>tn</td><td>tn</td><td>tn</td><td>tn</td><td>tn</td><td>O</td>

<td>co</td><td>CO</td><td>-Π-</td><td>Ο-</td><td>Ο-</td><td>Ο-</td>

<td>H-</td><td>H-</td><td>Π-</td><td>Π-</td><td>Π-</td><td>Π-</td>

<td>O</td><td>O</td><td>Ο</td><td>Ο</td><td>Ο</td><td>Ο</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>O</td><td>O</td>

<td>kO</td><td>kO</td><td>kO</td><td>kO</td><td>kO</td><td>kO</td>

<td>• Φ 1</td><td>m δ.</td><td>i</td><td>O</td><td rowspan="2">I O</td><td></td>

<td>1 O</td><td>B O</td><td>B O</td><td>s O</td><td>O</td>

<td>rH</td><td>rH</td><td>rH</td><td>rH</td><td>rH</td><td>H</td>

<td>H</td><td>H</td><td>M</td><td>«K</td><td>ffk</td><td>M</td>

<td>ç*</td><td>rH</td><td>O-</td><td>rH</td><td>rH</td><td>tn</td>

μ μ

<td>O</td><td>rH</td><td>ro</td><td> 00</td><td> 0—</td><td>O</td>

<td> 00</td><td>O</td><td>O</td><td>ΟΊ</td><td>CT&gt;</td><td>O</td>

<td>• k</td><td>• i</td><td>η</td><td>• k</td><td> *</td><td> «4</td>

<td>kO</td><td>kO</td><td>k0</td><td>tn</td><td>tn</td><td>kO</td>

rd Ο

<td>co</td><td> *4*</td><td>m</td><td>O</td><td>O</td><td>tn</td>

<td>tn</td><td>THE</td><td>THE</td><td>tn</td><td>tn</td><td>CM</td>

<td>• k</td><td>«K</td><td>• k</td><td>Here</td><td>«K</td><td>&lt;k</td>

<td>O</td><td>rH</td><td>rH</td><td>O</td><td>O</td><td>O</td>

<td>rH</td><td>cr,</td><td>CO Ck</td><td>rH</td><td>rH</td><td>rO</td>

<td></td><td>«K</td><td>Pk</td><td> ·»</td><td>• k</td><td>* k</td>

<td>THE</td><td></td><td>H-</td><td>THE</td><td>THE</td><td>O</td>

<td>H</td><td></td><td></td><td>rH</td><td>H</td><td>m</td>

ko r- co c o H rH

H

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X> v * vfc +³ laughs

O

I!>

tf

THE

W m

tf

A (Ti

VO tn

CM

<td></td><td></td><td>O m</td><td>O m</td>

<td></td><td></td><td>(D</td><td>(D</td>

<td></td><td></td><td>ro</td><td>ro</td>

<td></td><td></td><td>tf</td><td>tf</td>

<td>O</td><td>O</td><td>O</td><td>O</td>

<td> ·»</td><td>at</td><td>laugh</td><td>laugh</td>

<td>THE</td><td>O</td><td>ω</td><td>frog</td>

<td>m</td><td>tn</td><td>O</td><td>O</td>

<td></td><td></td><td></td><td></td>

<td></td><td>M ·</td><td></td><td></td>

<td></td><td></td><td></td><td></td>

<td></td><td>H</td><td></td><td></td>

<td></td><td>Φ</td><td></td><td></td>

<td></td><td>rd</td><td></td><td></td>

<td></td><td></td><td></td><td>tf ·</td>

<td>co</td><td>rô</td><td></td><td>CO</td>

<td>ç-</td><td> □</td><td></td><td>THE</td>

<td> \</td><td>rô</td><td></td><td> \</td>

<td>CM</td><td>φ</td><td>CM</td><td>CM</td>

<td>Ç-</td><td>O</td><td>Ç-</td><td>Ç-</td>

oomo tn co in tf- 'mr tfra tf laughs

laugh

<td></td><td></td><td></td><td></td><td></td><td> 0</td>

<td>O</td><td>in</td><td>O</td><td>O</td><td></td><td>Φ</td>

<td>ç-</td><td>and-</td><td>m</td><td>m</td><td>ΟΛ</td><td></td>

<td>tf ·</td><td>tf-</td><td>tf ·</td><td>tf-</td><td>cn</td><td>•The</td>

<td></td><td></td><td></td><td></td><td>cn</td><td>rô</td>

<td></td><td></td><td></td><td></td><td>cn</td><td>• laughs</td>

<td></td><td></td><td></td><td></td><td>tr »</td><td>O</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>ΟΊ</td><td></td>

<td>O</td><td>m</td><td>O</td><td>O</td><td>cn</td><td>«D</td>

<td>GRANDFATHER</td><td>m</td><td>grandfather</td><td>GRANDFATHER</td><td></td><td>. rô</td>

<td></td><td></td><td> •</td><td></td><td> «»</td><td>rô</td>

<td></td><td></td><td></td><td></td><td>THE</td><td></td>

<td>m</td><td>m</td><td>m</td><td>m</td><td> ··»</td><td>φ</td>

<td> 1</td><td> 1</td><td> 1</td><td>I</td><td></td><td>Pi</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td>m</td><td></td>

<td>THE</td><td>THE</td><td>THE</td><td>THE</td><td>cn</td><td>φ</td>

<td>K</td><td>M</td><td>M</td><td>M</td><td> ·»</td><td>na</td>

<td>THE</td><td>THE</td><td>r-</td><td>ç-</td><td>cn</td><td></td>

<td></td><td></td><td></td><td></td><td>cn</td><td>K</td>

<td></td><td></td><td></td><td></td><td>"The</td><td>• g</td>

<td></td><td></td><td></td><td></td><td>M</td><td>O</td>

<td>VQ</td><td>O</td><td>CM</td><td>ç-</td><td></td><td>tf</td><td>laugh</td>

<td>m</td><td>c ~ -</td><td>THE</td><td>co</td><td></td><td>SI</td><td>O</td>

<td> ·&gt;</td><td>•The</td><td>Λ</td><td>•The</td><td></td><td> ®</td><td>THE</td>

<td>grandfather</td><td>tn</td><td>grandfather</td><td>tn</td><td></td><td>laugh</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>laugh</td><td>The</td>

<td></td><td></td><td></td><td></td><td></td><td></td><td>ffl</td>

<td></td><td> &gt;—»</td><td>X ~ * a</td><td>x — s</td><td></td><td></td><td></td>

<td></td><td>THE</td><td>rô</td><td>• rj</td><td></td><td>tf</td><td>"The</td>

<td></td><td></td><td></td><td>THE</td><td>O</td><td>•P</td><td>rô</td>

<td></td><td></td><td> &lt;—*</td><td>* sZ ·</td><td>The</td><td>THE</td><td>rô</td>

<td>O-</td><td>co</td><td>O</td><td>σ \</td><td>O</td><td>tf</td><td>«D</td>

<td>OJ</td><td>THE</td><td>ΓΟ</td><td>H</td><td>•P</td><td></td><td>φ</td>

<td>•The</td><td> ·»</td><td>•The</td><td>"The</td><td>&gt; tf</td><td>Φ</td><td>í&gt;</td>

<td>O</td><td>O</td><td>O</td><td>O</td><td></td><td>ro</td><td></td>

<td></td><td></td><td></td><td></td><td>tf</td><td></td><td>O</td>

<td></td><td></td><td></td><td></td><td>laugh</td><td>frog</td><td>rô</td>

<td></td><td></td><td></td><td></td><td> 3</td><td>• laughs</td><td></td>

<td></td><td></td><td></td><td></td><td>THE</td><td>tf</td><td>O</td>

<td>r-</td><td>m</td><td></td><td></td><td></td><td>THE</td><td>big brother</td>

<td>"The</td><td>"The</td><td></td><td></td><td>O</td><td>laugh</td><td>co</td>

<td>σ \</td><td></td><td>tn</td><td></td><td>The</td><td>frog</td><td>CO</td>

<td>CVl</td><td>you</td><td>H</td><td> £&gt;</td><td>O</td><td>-P</td><td>CD</td>

<td></td><td></td><td></td><td></td><td>-P</td><td>d</td><td>rô</td>

<td></td><td></td><td></td><td></td><td>rô</td><td>The</td><td>Pi</td>

<td>OJ</td><td>ΓΠ</td><td>'Φ</td><td>tn</td><td></td><td> *</td><td>O</td>

<td>H</td><td>H</td><td>H</td><td>H</td><td>tf</td><td>, Q</td><td>O</td>

oa * ω

• P o

£ • laughs

¡5b a

for the

The¹ ©

• P ro

All these tests δ, ΰτεαζ origincn to forms

<img file="PT76047B_D0050.tif" />

such fcrax always larger than in Example Γ. The polycrystalline materials were always in the form of film or deposited on the cooler ends of the tube and were usually limited to approx.^mThe last 10 cm of the tube, although there was usually some overlap with the monocrystals. structure of._r>, as determined by data from the diffrences of the¹ Lightning Ao, Chemical analysis by hamicristair. They may be difficult to obtain with great concern because of their stability and digestion of materials to VIII to XI color. the data

Polycrystalline novelties were characterized by 7 ° ray diffraction and wet analytical procedures. The pelivia. c; na; .ococs extreme p.

In some cases, the cells showed various crystallinities that were in many respects different from those of deΪΏ ^, but they were distinctly different from others. In addition, the hybrid analysis, coupled with specimens of flame absorption, consistently showed: an alkalectal rectum as the condominium of the bulk order of the parts per fraction (i.e. less than 1000 pp · And often less than 500 ppm) and with F / X ratios ranging from about 200 to about 5000 rare

tic rts that favor the development of rolicristrlín materials;

rush

Following the successful improvements achieved in the ihonooristsic preparation, references were made to control the materials consisting of a know-how 5-well expeforno series and to choose

XI!

I l | i;

-τ ·, -

<img file="PT76047B_D0051.tif" />

are dc a dento in order to find the appropriate stepped gradients vices to produce seloetr «r» r · '' * · »ι iu; vt. L · υ I <. ».0 T> olicrâ £ i bcc3 -iû l »ninth oosc caraoc proceaenres.

These assays suggested the necessary fractures to obtain the desired products. What remained to be demonstrated was how to optimize these products. Table VI shows the type of profiles used for the observed products.

«Tf rd ra t>

The tf tf!>

tf ra ra μ

oo

μ tf

To

tf

To

• «d • To ra &amp;

<img file="PT76047B_D0052.tif" />

<td>Α</td><td>Μ</td><td>Μ</td><td>Η</td><td>Μ</td><td>Μ</td><td>Μ</td>

<td></td><td></td><td>Μ</td><td>Μ</td><td>Μ</td><td>Μ</td><td>Μ</td>

Ratio Pressure Time length o

ΙΛ

O 'tf μ

ra tf xx tf ra o · itf η o EH o

CM O EH O

AO EH the tf tf

O

Eh tf

Ou tf tf

The tf

Ntf m

tf tf

M tf tf

Μ

M

En

<td>ο</td><td>ιη</td><td>frog</td><td>ο</td><td>ο</td><td>ο</td>

<td> **</td><td>Ç"</td><td></td><td>ο »</td><td>β »</td><td>β *</td>

<td>Α</td><td>ο</td><td></td><td></td><td></td><td>ο</td>

<td>ιη</td><td>THERE</td><td>frog</td><td></td><td>Γ * Ί</td><td></td>

The tf

THE

<td>νο</td><td colspan="2">&lt;ο</td><td colspan="2">Ç-</td><td>CM</td>

<td></td><td></td><td></td><td>ιη</td><td>Ε—</td><td>Α</td>

<td></td><td></td><td></td><td>ct</td><td> \</td><td></td>

<td>C \ J</td><td>C \ J</td><td>CM</td><td>σ \</td><td>ο</td><td>OJ</td>

<td> !&gt;·</td><td>Ç-</td><td>Ç-</td><td>σι</td><td>ιη</td><td>Ε—</td>

<td>Ο</td><td>ο</td><td>Ο</td><td>Ο</td><td>μ</td><td>ιη</td>

<td>m</td><td>ο</td><td>ιη</td><td>m</td><td>CM</td><td>CM</td>

<td>m</td><td>Α^-</td><td>ΓΟ</td><td>m</td><td>CM</td><td>ΠΊ</td>

<td>ιη</td><td>ιη</td><td>ιη</td><td>ο</td><td>ιη</td><td>ο</td>

<td>ΜΟ</td><td>ηι</td><td>Ε-</td><td>ιη</td><td>ηι</td><td>Α</td>

<td>α</td><td>Α</td><td>ΠΊ</td><td>m</td><td>CM</td><td>Α ·</td>

<td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>Ο</td>

<td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>ο</td>

<td>νο</td><td>RV</td><td>ιο</td><td>ιο</td><td>ιο</td><td>νο</td>

<td>• d- «</td><td>• d · Β</td><td>Α ·</td><td>ιη I</td><td>Α · Β</td><td>* d “ Β</td>

<td>s ο</td><td>1 ο</td><td>Ο</td><td>D Ο</td><td>1 ο</td><td>I Ο</td>

<td>rd</td><td>rd</td><td>Α</td><td>rd</td><td>Α</td><td>rd</td>

<td>Μ</td><td>Μ</td><td>Η</td><td>Η</td><td>Η</td><td>Μ</td>

<td>m</td><td>ιη</td><td>Ε-</td><td>rd</td><td>ιη</td><td>ιη</td>

<td colspan="5">μ</td>

<td>m</td><td>νο</td><td>ο</td><td>ο</td><td>ιη</td>

<td>νο</td><td>νο</td><td>• d</td><td>ο</td><td>CTi</td>

<td> ·»</td><td> *&lt;&gt;</td><td> ·»</td><td>Ç"</td><td>«Λ</td>

<td>ιη</td><td>ιη</td><td>ιη</td><td>ο</td><td>* d *</td>

<td>Ο</td><td>πΊ</td><td>σλ</td><td>&lt;Ν</td><td>ιη</td>

<td>ιη</td><td>Α</td><td>• d *</td><td>ιη</td><td>CM</td>

<td> ·,</td><td>χ.</td><td>Λ</td><td></td><td>Λ</td>

<td>ο</td><td>Α</td><td>rd</td><td>rd</td><td>rd</td>

μ ζ— \ sa r-) 10 μ μ

ΙΓ \ ιη

<td>Α</td><td>ιη</td><td>ιη</td><td>ιη</td><td>ιη</td><td>THE</td>

<td>Α</td><td>Α</td><td>Α</td><td>Α</td><td>Α</td><td>Α</td>

<td> \</td><td></td><td></td><td> ·\</td><td></td><td></td>

<td>Μ</td><td>Μ</td><td>Μ</td><td>Μ</td><td>Μ</td><td>Μ</td>

— C— ΑγΗ γΗ οϋ σ \ ο

Η γΗ CM fi

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(I

P t &lt;5

THE

THE

A &lt;í

A • I ij

I i:

í

1:

ι i í i i

<td colspan="9">O you you O "you</td>

<td></td><td></td><td></td><td></td><td>O</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>•you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>d</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>"s</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>you</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>d</td><td></td><td rowspan="2">frog THE</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>laugh</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>O</td><td></td><td>frog</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>THE</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>frog</td><td></td><td>THE</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>tJ</td><td></td><td>you</td><td>z — i</td><td>frog</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td> 4³</td><td>frog</td><td>you</td><td></td><td></td>

<td></td><td></td><td>frog</td><td></td><td>O</td><td>• rl</td><td>you</td><td></td><td></td>

<td></td><td></td><td>O</td><td></td><td> 4³</td><td>you</td><td>•you</td><td></td><td></td>

<td></td><td></td><td> 3</td><td></td><td></td><td> 4³</td><td>THE</td><td></td><td></td>

<td></td><td>frog</td><td>you</td><td></td><td>O</td><td>frog</td><td>you</td><td></td><td></td>

<td></td><td>O</td><td>•H</td><td></td><td>THE</td><td>•you</td><td> 4³</td><td></td><td></td>

<td></td><td>you</td><td>O</td><td></td><td>The</td><td>you</td><td>frog</td><td></td><td></td>

<td></td><td>d</td><td>The</td><td></td><td>frog</td><td>O</td><td>•you</td><td></td><td>O</td>

<td></td><td>THE</td><td rowspan="2">The</td><td rowspan="2">you</td><td> 4³</td><td>O</td><td>you</td><td></td><td>THE</td>

<td></td><td rowspan="2">m</td><td></td><td>you</td><td>O</td><td>O</td><td>you</td>

<td></td><td>frog</td><td>you</td><td>frog</td><td>O</td><td>• laughs</td><td>THE</td><td></td>

<td>O</td><td>♦ laughs</td><td rowspan="2">you</td><td>d</td><td> 4³</td><td>The</td><td>jH</td><td>you</td><td>you</td>

<td>The</td><td>d</td><td>-P</td><td>you</td><td></td><td>O</td><td>O</td><td>frog</td>

<td>O</td><td>• laughs</td><td>d</td><td>you</td><td>frog</td><td></td><td rowspan="2">THE</td><td></td><td>frog</td>

<td> 4³</td><td>ϋ</td><td>M</td><td>frog</td><td>•you</td><td>frog</td><td>c |</td><td>, Q</td>

<td>*you</td><td>* laughs</td><td>O</td><td>THE</td><td>THE</td><td> 2</td><td>frog</td><td></td><td rowspan="2">O</td>

<td> 1</td><td>s</td><td>The</td><td>you</td><td>you</td><td>you</td><td>you</td><td>THE</td>

<td>O</td><td>•H</td><td rowspan="2">you</td><td></td><td>you</td><td>•you</td><td>THE</td><td>you</td><td>O</td>

<td>The</td><td></td><td>Si</td><td>ω</td><td>Ή</td><td>d</td><td>•you</td><td> 4³</td>

<td>O</td><td>frog</td><td>you</td><td>you</td><td></td><td></td><td>O</td><td>you</td><td>d</td>

<td> 4³</td><td>O</td><td>d</td><td></td><td>O</td><td>frog</td><td>'you</td><td>frog</td><td>THE</td>

<td>Ό5</td><td>•P</td><td> 4³</td><td>O</td><td rowspan="2">d</td><td>O</td><td>THE</td><td> 4³</td><td>O</td>

<td></td><td>laugh</td><td>frog</td><td>Italy</td><td>•you</td><td>frog</td><td>you</td><td>you</td>

<td>O</td><td>frog</td><td>•you</td><td>frog</td><td>O</td><td>"you</td><td rowspan="2">THE</td><td rowspan="2">The</td><td rowspan="2">THE</td>

<td>Italy</td><td> 0</td><td>s</td><td>frog</td><td> &amp;</td><td></td>

<td>N</td><td>frog</td><td> 1</td><td>frog</td><td>The</td><td rowspan="2"> 1</td><td> |</td><td rowspan="2"> 1</td><td rowspan="2"> 1</td>

<td>you</td><td>H</td><td>The</td><td>you</td><td>frog</td><td></td>

<td>you</td><td>frog</td><td>THE.</td><td>THE</td><td> 4³</td><td>is</td><td>THE</td><td>you</td><td> *</td>

<td></td><td></td><td> &lt;-&gt;,</td><td>Z— '</td><td>zs</td><td>z- \</td><td></td><td></td><td></td>

<td>you</td><td>rQ</td><td>O-</td><td>—Rd</td><td>frog</td><td>Ά</td><td></td><td></td><td></td>

<img file="PT76047B_D0054.tif" />

In the first run, which is the subject of Example III, the temperatures of the range of values ​​used in Example I were precisely doubled by the linear cooling gradients modified to a gradient gradient. Not surprisingly, all product types were found with some variations in quantities compared to those in Section A. When the lowest temperature was raised to 400 ° C, as in the second Labela test, no amorphous material was found as expected. . With a core section temperature of 425²However, almost two thirds of the interior of the tube was covered with polycrystalline films and only a small number of thin filaments were found meaning that almost 3 films could be produced almost exclusively.

In the third and fourth trials, however, in which the coldest temperatures were kept equal to 350 ° C (sufficiently cold to form amorphous material in the first test) and the central zone temperatures were lowered to 375 and 35 ° C, amorphous matexials were not formed in large quantities. On the contrary, large amounts of both monocrystalline and polycrystalline material were found in a relatively short space of the tube and, at best, only thin films of amorphous materials may have formed in the rest of the tubes. The same phenomenon was observed in the two subsequent trials, although there were clearly thin amorphous films in one trial. Apparently, . Most vapor-shaped species condense into polycrystalline and monocrystal forms and no significant amount of vapor travels to the region that is sufficiently cold to form amorphous forms.

<img file="PT76047B_D0055.tif" />

A 3-zone furnace of the Lindbrrg 54357 model identical in design to work with the first example was also useful in this regard. On elementor. Aqaca '£: - ·. die paper rolls rolled by the Mesa standard. · · be.víralo Medeio iindberg 5S744-A, continually ajurt- a. The chatroom of the dog ?, of warming were '' o · dar ca: · '- n ^ teri ·! Heat resistant stop. ninirisar c through the oven. The reaction tube was apoip_Oy. Ο.οί- woven asbestos tape rings, One of the rráic a.et -.- a. replaced between 14-19 cr, and the other between &lt;2-45 cr. a: lango from the face. I. ro place, anhos the rings complete? '- · .tc inside' central heating sound, good to Z^r. of the central elements with the two main sections. They were constructed in such a way that the tube was kept at a slight angle. The rings are also: to immolate to the heating zones one of the other; .Ctu-ndc · as barriers to. transfer of '' item. C .. ύ! The quartz rod tube had. The bottom is 4 cm in length by 2.5 cm in length and reduced to a narrow addition tube 10 µm in length by 10 cm in diameter. Under an atmosphere of fresh azeto, 5.93 g of red phosphorus, 50 g of potassium were transferred to the tube.

The atomic ratio of the phosphorus to the metal was 15, the phosphorus was 02.2299%, potassium was 93.25% pure.

L u \ .Uuu avacuafo 5 x 10 'Sorr and sealed by the fucac i dc addition tube with a few cm of the widest part [' '.ο tube, -^?the way the total length was equal to j - 51 cm. The sealed tube was placed in the oven at 5 ° C above, the temperature gradient was controlled for 0 ° C, &lt;-65 ° C.²0 and 550 for a period; ivy and kept for 72 hours. The energy by the oven was then simultaneously connected and the oven cooled to ambient temperature._s with. the cooling rate of the pipe is cut to open under a dc.azoto rccc atmosphere in a chariné oGm dc • '-rublet gloves. The pj? Odutcs

<img file="PT76047B_D0056.tif" />

ira ·, · η nonocrasf-: ia, poleul &amp; s pelicristnlinro o il: ..... cryo.

D .. Reduction of, EcllX Cylindrical Synthetic Rubies^çtb5- (21.2 £ £ ° -^{: 0} Seer laughed at doreri · tr-r i 'recce ~jjjj nue, parr cd - n grondos either: amorphous drift, if he had ra-troducir better. to be used. fia— no-ui-o · ra-re çn^r If the volume of the muteri els is to be obtained, the option for firm headings, the conditions apxproperly p-rr. tinban growth to be confined? an ep-np ncor than what was previously employed The i-7u chooses to allow only the end of the pipe to be 375^sThe uira te: ora tura infringer. This could in principle be achieved by removing thermal barriers. Ko ents it was also recognized that if one. large area of ​​the tube reigns and conditions for the formation of other materials, is + o 6, monocrystalline or K3 ?,_r polycrystallinc (x is nui^J; c greater than 15) these materials would act ”^r'.c three¹¹ rare rare species. Steam It was pmt - it was nessary to describe the formation of bending. n-tari-ic, ^ sro was achieved by increasing the tararxes. central water for the irises that would be useful for training q .; polycrisau materials •• crystalline. -u. only. then area in which to heal ϊ, -. tariain err, f-voracidos was. by. thermal barrier area, where rapid falls of tcr.c er atura occur.

As shown in the following example and in the other experiments in Table VII, lower the improvements in the procedure. At first it was the use of the Ecxe; vell “I hate LCl7CuO Digital Control Programmers” to actuate the.-Ra -nuocJr.cato elements. This made it possible to pre-program the squeegee treadmill so that it was possible to treat reproducibly from trial to trial, to rarely run the treatment of the glass; ra. * · the cratnelade · -₅ elininra: 'the pain breaker: the tube

<img file="PT76047B_D0057.tif" />

c n. prfnç-c '.c “ó ^ forum. This means that he does not believe it. - with steam with phosphor

-—; · cabbage. cono 3? ^. Bait was often the reason why they made reactive products. This reaot.⁴vidadc eonenguia-ro frenuentenente eliminate iiapregn enfie &lt;·. &lt;-. '•' Affects solvents that dissolved phosphorus. '• rn &lt;v ·. Follow-up improvement consisted of applying UV¹¹ -fionion i / v-rti ^ c wire? 0G ~ &lt;iS'0-5CC2G along tube wire c from c. strong r.ctal / phosphor until the fie zones! opposition -before transporting vrpor wire, puo pcrrlti | [c] - Accepted by two other methods, such as the factor or processes of the invention.

4; treaianth. o important raises uelbo3. ·· ic.-nte cc-nsi.-tin cr altcr ~ r a. geometry in tulle. r> 'y ur wire: long tube diameter diameter, _

J '-a fi,> an, c body wire pipe has been shortened ^notó! ccrca wire en co fic tube addition 160 fie 1C κι. fie ('tether (tigw 2) elongated and sealed in such a way as to create it.'. '· fi-7 cr. drsso tubB^f-isponíii - 1 no irior do *. «Τ · ο, Quan.1. In this last section of the R-Or.uc, if the vapor gradient was applied, that section was filled with 'li' cylinders. Bulky wire growth has been improved.

! ' Xhs fc - ο do 3 wire zones Eodelo lindbcr ...

; 50 ?, the size of the furnace size employed at the end of module I was also used in this 3b: elongated cells, however, were controlled by ur. Liu-Cyclo Digital Control Controller ”SOB-7700 which has persuaded that the process was progressed through the process of reproducible play.

The ends of the heating pipe are covered with heat-resistant material *

; shrug the loss. The heat of the furnace, the reaction wire tube, was supported by two strands of the child wire tape: The moles were constructed so that the tube was bent at a slight angle »Cc - ' Trisloxic Levels to Isolate Our Acuecing Acts

fie reception tube where the funnel was rounded, 35 cm long by 2.5 cm in diameter and receding into a narrow welded tube (162), color 20 cm long by cm> cm wide. -a freeze-dried atmosphere, 7Â ° 92Â ° C with a load on a cold mill and a 15Â ° C atomic ratio was placed in the tube and was evacuated at -5Â ° C.

x 1C Icrr is sealed by melting the pipe and add? a 10 cr fia part rsis wide, so that the total depreciation was 43 fie cm primes to '. The sealed tube was placed in the dried oven and dried and the tissue described above.

Where the pipe between 6 and 49 CTj uses a thermal barrier at 16-19 cm and the other at about 38-46 cm₃the Eoneuxell was-uoafia programmer was used to apply an inverse gradient⁵At 30 ° C-490 ° C, 50 ° C for 10 hours, even if the force has cooled to its inherent velocity, the Kaneira displaced tube is between 12 and 53 cm. The thermal barriers were also rearranged to stand at 18.5-21.0 cr ε 44s5-47 ca. 0 programmer-controlled gradient to 60C2C, 485² © 50C²C for 64 hours. The programmer then yielded a controlled cooling sequence for a 1800 gradient 190_s 2002C which was left for 4 hours. The oven was then allowed to cool to room temperature with the velocity in; A: .towow oven cooling.

The tube was cut open under the ataosfers. dry annotate and 4.13 grams long synthetic ruby ​​and homogeneous rubber recovered from the addition tube 162 (Figure 5).

Some results are others in the words VII.

<img file="PT76047B_D0058.tif" />

I

<td colspan="2">O</td>

<td>-P rf © H to • rl 'H</td><td>z ~ \</td>

<td>'S rf</td><td>O</td>

<td>fl O</td><td>H</td>

<td>© a</td><td>Sz</td>

<td>A to</td><td></td>

!

<td colspan="5">son</td>

<td>j</td><td> ©</td><td>PS</td><td></td><td></td>

<td> 1 1</td><td>The</td><td>•P</td><td></td><td></td>

<td></td><td>• rl</td><td></td><td></td><td></td>

<td> • </td><td>P</td><td>O</td><td>The</td><td>zs</td>

<td></td><td> &amp;</td><td></td><td>O</td><td>σ \</td>

<td> ) 1</td><td>The</td><td></td><td></td><td>Sz</td>

<td>j</td><td>O</td><td>O</td><td>O</td><td></td>

<td>H</td><td>O</td><td>-P</td><td>THE</td><td></td>

<td>H</td><td></td><td></td><td></td><td></td>

<td> &gt;</td><td></td><td></td><td></td><td></td>

<td> &lt;1</td><td>O</td><td>frog</td><td></td><td></td>

<td></td><td>THE</td><td>here</td><td></td><td>Z- \</td>

<td>THE</td><td>The</td><td>P</td><td></td><td>co</td>

<td></td><td> ©</td><td>O</td><td></td><td>s — z</td>

<td>! PI</td><td>EJ</td><td>THE</td><td></td><td></td>

<td>i ^ffl</td><td></td><td></td><td></td><td></td>

<td> &lt;5</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>z-s</td>

<td></td><td colspan="2">mo</td><td></td><td>l&gt;</td>

<td> !</td><td>EJ</td><td>OJ</td><td></td><td>Sz</td>

Ί

OJ O kO

Cl '

HO Ef 01

THERE

Φ

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FM ω B 'íi fi kã hO

SM dog

OJ l 'u

O'H

<img file="PT76047B_D0059.tif" />

Hi

<td colspan="2">O</td><td>O</td><td colspan="2">O</td>

<td></td><td>O</td><td>O</td><td>O</td><td></td>

<td></td><td>Ή</td><td>• rl</td><td>• rl</td><td></td>

<td></td><td>-P</td><td>-P</td><td>•P</td><td></td>

<td></td><td>RV</td><td>RV</td><td>\ d</td><td></td>

<td></td><td>•P</td><td>•P</td><td>-P</td><td></td>

<td>O</td><td>f4</td><td>P!</td><td>rf</td><td></td>

<td>nJ</td><td>•H</td><td>• rl</td><td>• rl</td><td></td>

<td>csS laugh</td><td>frog</td><td>frog</td><td>frog</td><td></td>

<td>W H</td><td>M</td><td>M</td><td>M</td><td></td>

<td> 8</td><td>THE</td><td>THE</td><td>THE</td><td></td>

<td> 54</td><td>P!</td><td>PS</td><td>pi</td><td></td>

<td>Φ</td><td>P</td><td>PI</td><td>P</td><td></td>

<td>-P</td><td></td><td></td><td></td><td></td>

<td>Φ</td><td>B</td><td>The</td><td>The</td><td></td>

<td></td><td> 0</td><td></td><td> 8</td><td></td>

<td>O</td><td>tn</td><td>tn</td><td>O</td><td></td>

<td></td><td> ·*</td><td></td><td> *%</td><td>ω</td>

<td> 3</td><td>H</td><td>H</td><td></td><td>tn</td>

<td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>ο</td>

<td> ·*</td><td> ·*</td><td> ·»</td><td></td><td> ·»</td>

<td>Ε—</td><td>σ \</td><td>C0</td><td>ο</td><td>ο</td>

<td>φ</td><td>m</td><td>m</td><td>Μ ·</td><td>Μ ·</td>

<td>Φ</td><td></td><td></td><td></td><td></td>

<td>OJ</td><td>οο</td><td> 00</td><td> 00</td><td></td>

<td>Η</td><td>ι—</td><td> 0-</td><td>I—</td><td></td>

<td>• x</td><td> \</td><td></td><td> \</td><td></td>

<td>CKI</td><td>φ</td><td>φ</td><td>Φ</td><td>φ</td>

<td>Ε-</td><td>ΚΩ</td><td>ΚΩ</td><td>ΚΩ</td><td>ΚΩ</td>

<td></td><td></td><td>Ο</td><td>Ο</td><td></td>

<td></td><td></td><td>ο</td><td>Ο</td><td></td>

<td></td><td></td><td>&lt;Μ</td><td>CKI</td><td></td>

<td></td><td></td><td></td><td>-χ</td><td></td>

<td>ΙΧΑ</td><td>Ο</td><td>Ο</td><td>Ο</td><td>Ο</td>

<td>OJ</td><td>Ο</td><td>ο</td><td>ο</td><td>Ο</td>

<td>¡</td><td>m</td><td>m</td><td>m</td><td>¡</td>

<td>Ο</td><td>ο</td><td>ιη</td><td>tn</td><td>ιη</td>

<td>Φ</td><td>ΚΩ</td><td> 1—</td><td> 00</td><td> 00</td>

<td>Φ</td><td>Φ</td><td>Φ</td><td>Φ</td><td>φ</td>

<td>Ο</td><td>Ο</td><td>ο</td><td>ο</td><td>ο</td>

<td>Ο</td><td>Ο</td><td>ο</td><td>ο</td><td>ο</td>

<td>ΚΩ</td><td>ΚΩ</td><td>ΚΩ</td><td>ΚΩ</td><td>ΚΩ</td>

<td>Φ 1</td><td>Φ I</td><td>ιη I</td><td>ιη 1</td><td>ιη I</td>

<td>ο</td><td>ο</td><td>ο</td><td>ο</td><td>ο</td>

<td>Η</td><td>γΊ</td><td> 1—1</td><td>Η</td><td>Α</td>

<td>X</td><td>X</td><td>X</td><td>X</td><td>X</td>

<td>ιη</td><td>ΚΩ</td><td>Η</td><td>Η</td><td>ιη</td>

<td></td><td>CM</td><td> 1-</td><td>tn</td>

<td>Η</td><td>B-</td><td> 00</td><td>ο</td>

<td></td><td>ϊ W</td><td> *</td><td> *</td>

<td>ΚΩ V</td><td>□ ΙΑ</td><td>ΙΑ</td><td> 00</td>

<td>ΪΒ</td><td>ÍB</td><td>ΪΒ</td><td>g</td><td></td>

<td>α</td><td>Α</td><td>Α</td><td>Α</td><td>Α</td>

<td>tn</td><td>ιη</td><td>tn</td><td>ιη</td><td>ιη</td>

<td>.Η</td><td>Η</td><td>Η</td><td>Η</td><td>Α</td>

<td>Α</td><td>Α</td><td>Α</td><td>Α</td><td>Α</td>

<td> \</td><td></td><td> \</td><td>χ.</td><td> \</td>

<td>Μ</td><td> «</td><td>Μ</td><td>Μ</td><td>Μ</td>

<td>Ο</td><td>γ4</td><td>CK1</td><td>m</td><td>Φ</td>

<td>nt</td><td>CM</td><td>CKJ</td><td>CKJ</td><td>cki</td>

/ - “X

O

H

<img file="PT76047B_D0060.tif" />

<td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> -&amp;&lt;</td><td>ct</td><td>Çk</td>

<td>grandfather</td><td>OJ</td><td>CJ</td><td>ro</td><td></td><td>MD</td><td>H</td><td>H</td><td>ro</td><td>O</td>

<td>ro</td><td>THERE</td><td>rt</td><td>THERE</td><td>THERE</td><td>CO</td><td></td><td>IA</td><td>'sh</td><td>ro</td>

<td>O</td><td>O</td><td>O</td><td>LO</td><td>LO</td><td>O</td><td>I'm</td><td>O</td><td>THERE</td><td>IO</td>

<td>• k</td><td>and"</td><td>k</td><td>k</td><td> *</td><td>et</td><td>and*</td><td> *»</td><td>et</td><td>et</td>

<td></td><td>ro</td><td>ΐ — Ί</td><td>ro</td><td>IO</td><td>THERE</td><td></td><td>THERE</td><td>THERE</td><td>ro</td>

<td>xi-</td><td>sd-</td><td></td><td>M-</td><td>xf-</td><td>ro</td><td>ro</td><td>ro</td><td></td><td>ro</td>

Cont rt

E3 m

rt

MD

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Preparation of Metal Polyphosphides by Raw Techniques.

Polyphosphides have been prepared in two fundamentally different types of equipment which are both identified herein as two-source tonics or separate source thermals because in the two types of equipment the meth and phosphorus are separated and are heated independently of each other on each side. a deposition zone. All examples were performed on the KP system.

In the first process, as shown in Figure 12, the phosphorus and potassium charges are maintained at opposite ends of a sealed quartz tube 100. The tube is subjected to a fracture profile as shown in Figure 12 achieved by use of a 3 zone oven. The profile causes any independent charges to be heated at elevated temperatures relative to the central zone located between the two constituents. In this zone the vaporized constituents combine to form the KPijj product deposited as films on the reactor walls. (Fuller details are given in Example V below).

In the second apparatus, as shown in Figure 14, a substantial section, generally indicated by 102, is maintained at room temperature outside the three zone furnace 104. This section includes a valve 106 and ball joint 108 used to achieve low desired pressures to carry out the reaction. This alternate sealing technique requires lower temperatures for this part of the equipment but allows for quick, non-destroying insertion.¹, of glass that constitutes the sources of metal phosphorus. The boat * 112 (see Figure 5) is also intended to support glass substrates (Figure 14) for the metal onto which the films must be deposited. ”These film / substrate conflagrations serve as initial starting points for

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conceive ο dici.'Sitivo, as ee go.'ioa below ',

The external section of the oven sorbs cold, but the vaporized ones, in particular the phosphorus, which is charged in the area closest to the external cooking, &lt;5 deposited in the outer section in large quantities, usually as it is. lotropic rcnca -1 very pyrophoric. By virtue of docta rag's existence, we condition him under sir's vepor pressure.^f1the systems described above; .. It follows that the hard-working conditions that have been achieved with the intended success or pro-hitcc in the first apparatus are not suitable for the second apparatus, 'The proportional conditions for stump were determined independently,

In the 54 cn dc co-protonent quartz tube 100, 5 cm in diameter, with a neck of 10 cm in length by 1 In diameter 116, shown in Figure 11 *, the phosphorus and potassium are charged, in the presence of a dry nitrogen atmosphere, at opposite ends of the tubes in a tonic ratio of 15: 1. Potassium (39.95% pure) was charged first by leaving small pieces totaling 28 g in a cup 118 with the vertically oriented tube. The pieces were then fused and allowed to only solidify in the glass.

Phosphorus (99.999%) was then added to the tube, with 5.3 grams of pieces easily manipulated around cup 118.0 The tube was then sealed through the neck hole 136 at 5 x 10 Torr.

The tube was then placed in a 3 zone oven of Model iindberg 54357-5 so that it was centrally located between the three zones. Hiperenteaonte of Model 54357, which has zone lengths of 15.2, 30.5 or 13.5 ca (3.6.12; and 6 inches)

<img file="PT76047B_D0075.tif" />

ο nc-delo 3 testers with 20.3, 2Q, 3, 20.3 (8.8 and 8 inches). Two ribbons of asbestos fabric wound around the rib supported it at the junctions of zones 1 and 2 and zones 2 and 5. These ribbons not only supported the tube but also isolated the central zone from the outer zones. At a higher temperature, a schematic representation of the resulting temperature profile is shown in Figure 12. A Honejwell SUP-7700 Digital Control Programmer was used to control the heating of the three zones over a warm-up period - appropriate until a gradient of 450,> 00, 45-O was obtained.^The,. which was maintained for 72 hours and then by a 15 hour cooling sequence until room temperature was reached.

The materials formed in the tube were analyzed by the following procedure. First, in a dry nitrogen atmosphere, the tube was cut into seven tubular sections, about the length of which employing one. silicon carbide saw.

Parts of the films found in the sections (generally 10 microns or thicker) were removed and individually examined by X-ray diffraction technique. Q remaining of each. This section was wetted by wet method analysis.

The F / K ratios of the positons found in the various cookings are shown in Figure 13. Far central regions were. which was approximately 30020, the compositions in volume are about 14/1, which falls within the precision limits of the methods employed to identify the materials as such. More telling were the powder X-ray diffraction spectra for the materials found with an F / E ratio of about 14, which clearly showed that they were similar to those of either single crystal strands or polycrystalline material. pasta. In addition, the spectra showed significantly the presence of polycrystalline and amorphous materials.

<img file="PT76047B_D0076.tif" />

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Already one device in this example has been modeled for use in Example Y. The tube "quartz 112" was manufactured with "nozzles" 120 and 122 repeating two extreme cavities of the plant. (see Figure. 16) '. Under a dry nitrogen atmosphere, molten potassium (0.4-7%, 93.95% purity) was added to the indicated internal column when the addition tube 124 was melted closed. Phosphorus (5.50 g, 52.9252% of the purine.) Was added along with the field indicated by F and the apparatus. Whole ovacuadc and sealed at 1 x 10³ Torr, by fusion of the second addition tube 126. Λ phosphorus: potassium ratio in the cistern cr-?

The sealed tube 119 was 41 cm long and was centered between three consecutive zones of 20.3 cm in a 3-sided oven of Model II-idbcrg 54357-5. Two thermal barriers (TB) made up of woven asbestos ribbons, wrapped around the pipe around each other, are the same at the junctions of zones 1 and 4, and are zones 2 and 3. * 3 In addition to the pipes, they insulated the central zone from outside temperatures. The Programmer Be used iloney &amp; ell ÍXaP-7700 Digital Control to control the three heating zones, up to a gradient of 5C0, 355, 7002C. (The phosphorus was at 500Â ° C; the potassium at 70Â ° C. Central zone temperature was chosen at 30Â ° C, but the core characteristics of the asbestos woven tape were limited. heat spill from the side cariaras raised the central zone temperature to 355 ° C^The0). The gradient was maintained for GO hours and then followed by a 24 hour cooling sequence.

When tube 119 was cut open,

<img file="PT76047B_D0077.tif" />

under conditions of the presence of dry nitrogen; Using a silicon carbide saw, the nozzle 122 between the potassium zone K and the central zone was found to be clogged with polyphibroid-like material. The central zone contained thin, light green film; thicker, darker red films; some relatively large monolithic synthetic rubies. The two largest pieces were each 4 cm in length by 1 cm wide. a maximum thickness of^; about 4 mm. One side of each piece is relatively fuller, while the other has a convex configuration associated with the creping of the inner walls of the circular reaction tube.

Wet analysis of this material showed that the potassium content is sometimes extremely low; in a voluminous analysis and its content is equal to us than 60 parts per million. A. electron spectroscopy. for chemical analysis (SSOA) indicated that the potassium content of this material would rapidly decrease outside the tube wall into which it primarily deposited. At 100 angstroms, a. proportion. of B / K was about 50. As measured by AESOA the B / I ratio deposited was on the order of ΙϋΟΟζ Os. X-ray diffraction studies showed that the material was. amorphous.

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Under an atmosphere of dry nitrogen, 0.19 g of dehydrothione potassium (99.95% purity) was transferred to one of the outer sections 3.28. (5 cm in length) from a pyrex glass boat 112 (Figural5). Two flat substrates of glass 114. (See Figure. 14%, each about 7.5 cm long by 1 card, wide, were laid with one end against the other, filling the center section. 130 with

15.3 cm dc length, 3n then 1.36 grams of

<img file="PT76047B_D0078.tif" />

match (S3₆Purity (obtained from Johnson Latthey) were added to the opposite outer section 132 of the boat, the phosphorous phosphorus falling under an easily sized, medium-sized phosphor that fills the bottom of section 132 '. Pyrex dividers 113 prevent substrates P and Z from slipping on the little boat 112, the little boat. 122 con 35 <23 in length was then carefully forced to decline in. cafcurs. pyrex reaction tube 135 color 60 cr in length ε 2_s5th The diameter of the potassium section 128 has come into contact with the rounded bottom closed end of the chamber 13 in the Bunã-M circular ring, size 124® has been attached to the joint. > «. 102 of the circular ring the leflcaa valve 1C6. (provided by ^ ChcxYac, Inc³⁷) was screwed tightly, Ruma tubager. vacuum₅ Valve 106 has been reopened and the case has been rebuilt up to 8 x IC ϋ = ΐ₅ Br br br foi 'was then closed closed sealing the reaction house_O

The reaction chamber is placed in a Tiodelo lindberg 54357-5 3-probe oven * As shown in Figure 24® two strips of glass fabric wrapped around the tube and spiral back_The supported the camera at the junctions of zones 1 and 2 and the sonas 2 and 3. These ribs forming thermal barriers (TB) have been tail-fitted to be fully positioned within the central zone. * The third ribbon, in ecpiral 138, was used to support It is terribly important that the device comes out of the camera:. of heating the stove. Wow. Cylindrical lid 140 of ceramic-type material was used to hold the heat slit from the oven opening in the other. · end of the camera *

This apparatus causes the section 128 of the potassium-containing boat 112 to be in the third heating zone 150 with strands containing substrates in the central zone or the second heating zone and the section 152 of the vessel. . . that contain the PHEFFECT stay in the first zone.

<img file="PT76047B_D0079.tif" />

cement 'This also results in a large part of the appliance being located outside the oven at room temperature'.

An IZ Model Honcywell DOR 7700 Digital Control Programmer was used to control the three heating sections during. a heating period in which temperatures have been required to rise to 100, 150, 100 ° C in the phosphorus zone, the substrate zone and the potassium zone respectively. Then, as quickly as possible (approximately 18 minutes) the gradient was set to 500, 300, 400 ° C, values ​​which were maintained for about 8 hours *. The oven was then allowed to cool to its inherent speed until a profile of 100,100,000 ° C was taken which took about 10 hours. The temperature was then allowed to cool to room temperature.

tube 134 was removed from the furnace. The section outside the furnace contained deposits of white, yellow and yellow-red materials, all of which were likely to be phosphorous in various polymerization phases. The phosphorus heating zone was free of any material, while the potassium zone contained a \^rrange of materials, brown, yellow and orange in color »

The latter extended slightly to the central zone which, on the other hand, was covered to half its extent, near the potassium zone, with a dark film, which transmitted red light when the light of a lamp shone through it, The other half of the zone was without material.

The apparatus was aborted under a dry nitrogen atmosphere, the pyrex boat 112 was removed and the glass substrates, covered with the red foil, were removed from the boat and placed in a tightly sealed flask for later release '' (when The remaining materials were exposed to ambient conditions. Phosphorus deposits in the section / exposed tube generally burned vigorously, although those closest to the source of phosphorus lacked this receptivity. The materials that were in the section.of the source of

<img file="PT76047B_D0080.tif" />

petácsiô · 'ο - p-Tv-gross raw receptive when exposed to age. They usually burned vigorously, rprrcitem.cnte color. hydrogen release (reduced water reduction) '.

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<td></td><td>Α</td><td>rd</td><td></td><td></td><td></td><td></td><td></td><td></td><td>ΙΑ</td><td></td><td>Η</td>

<td></td><td></td><td>• Η</td><td>φ</td><td></td><td></td><td></td><td></td><td></td><td> \</td><td></td><td></td>

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<td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td>laugh</td><td>-tf</td><td>• laughs</td><td>-tf</td>

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<td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td>Η</td><td></td><td>Η</td>

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<td>• k</td><td>«K</td><td></td><td>Vk</td><td>• k</td><td>«K</td><td>• k</td><td>Vk</td><td>and"</td>

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<img file="PT76047B_D0082.tif" />

Limiting conditions for the preparation of the scum cue transmitted red lus films. If the temperatures of the two source sera are slightly decreased, as is the case with table 49 in table HI, the amount shown in the table is shown by the length of the deposit._çdecreases dramatically. From this Ksneira₈ very small differences between the features â € “operation two we went to 5 reindeer &amp; iiodelo 543575 qus₉And otherwise they are identical to the requirements that in the second oven (2), n the temperature. the source of the phosphorus is raised to the lowest value (see tests 50, 51 and 52). Raise the temperature to the source δε phosphor to 550^£C ãá na baá result in sub-là psrs.

525 ^£With result Eclhct.

Analysis of the materials from Assay 46, 47, 4-S, with a scanning electron microscopy using the electrodefraction analysis (SSi-ADX) showed that the material is formed of C-7 orb films. had come their specs_ç and what character © sorfo® is the discernible structure evident in the photograms?

Summary of Conditions for Fraagoorte õg Steam

Characteristic aspects of process control for types If products are as follows.

1) use of a three zone furnace to achieve 'control' of most fractures; 2) Prolonged reaction tube cospriseat, o) Thermal barrier use for temperature gradient control, 4) Turbulent insulating bodies at the ends of the sea 5 5) Prolonged narrow addition tube to obtain eile Synthetic rubies £ ndrices_O

The conditions are processed. for transportation to and from a steam source are as follows

a) The temperatures of the reaction range vary. between £. . · «

<img file="PT76047B_D0083.tif" />

550-Ji the temperatures of the deposition of sleep, cold vary: between 450-50020;

Z) the deposition temperature to obtain noncrystals of the found which could vary more or more than 25^y0 in particular, a central value is comprised of four / 65-475-0;

The temperature of the deposition for its pollutant has been found to vary depending on the crown 455-0 to 575-05! 4; the deposition temperature to obtain the for! The new nostril of phosphorus ranges from about 375-0. up to about 300 ° C. (lions have been found so far, lower temperatures / '.

| The right conditions for carrying steam • with two sources for ·! performing the formation of bulk materials (now / hr and Figure 11) is as follows: phosphorus, tomperatu; r 45020, potassium at 45020 and deposition sounds at 50 ° C; cc deposits pray. consisting of films ^:^ra, a mixture of E. coli polycrysaline c amor15 f; to Kr ,,. amorphous in bulk (x much larger than the 15th newfem, phosphorus, apparatus of Figure 16): phosphorus n 5C-CSC, potassium at 70GSÇ z deposit sum at 555⁹0 The theft of K was formed, the deposit now constituted by bulk amorphous; amorphous firm films (apparatus of Figure 14) match at 50d2g_f potassium at 400^sP θ substrate at 3OO2Q_and • All thin films of a ten! The phosphorus source fracture can be raised to

5252a and still produs If the temperature of the source of SOcforc drops to 475-0? The system did not cost! The temperature of the potassium source bai = 'nr to 375²Ç? and the system not at which substrate temperatures may be raised to; 7152a 0 0 system will still produce Eè,_ç but this happens only to rise to 325^The0.

<img file="PT76047B_D0084.tif" />

frcm r · \ .c of metal polyphosphs • nlllorlstalfnoe en grrçççççççititodes pop utilihfcão ..

If they are formed in a cst-dà fr-ioc, it is appropriate to derive their precursors from the alkaline metals of the type ΙΡ - ,, ρ Ιχγ, Kt, -. can easily be prepared in quantities of cr. of magnitude of yrz, &amp;. ·. It is by a technique which the Applicant calls itself. condensed ”. Prior to using this technique, 33 millimeters are generally brought into close contact by a ball milling mill. In the ball mills, quantities of the elements of the order of or greater are placed under tact-to-water conditions at the desired atomic ratio of ketol / phosphorus, for example Ϊ / Κ 15 per 1 for ΓΤ-, η. Vc i-.cinho t_ Ον.Οϋν-.Οβ kJi? »Then use it for 40 hours and reduce the components to a smooth, homogeneous, easily slipping powder. The mills are generally heated for approximately 20 hours. hours during grinding at about 100 ° C.

This is done to increase the flowability of the metal component during grinding »

A portion of the milled mixture, usually 1 gram or more, is transferred to a quartz vial under dry conditions. The ampoule ranges in size from 2.5 cm in diameter to 6.5 cm in length up to 2.5 cm; 25 cm in length, depending on the size of the load to be processed. The pipe is sealed under reduced pressure (generally; where greater than 10 Torr).

The reaction is carried out by subjecting the tube to ever-increasing numbness, under isothermal conditions, until the applied temperature reaches 5 ° C to 52520 ° C. For isothermal conditions, it is intended that the total time of the material be obtained. always finds almost b. same feasible way possible

<img file="PT76047B_D0085.tif" />

I to ζ '/ ίϊ-: ·? steam transport If hot parts rotate! which would have resulted in the obtainment of non-organic yields. The 'high impregnation temperature' has been added over a substantial time interval, during which an crystalline crystalline powder product is supplied. Typical impregnation is 72 longer, however long the reaction time, or soybean and tango, and the more crystalline the product will be (colony expressed by the grain, sharpness (diffraction lightning h in dust, etc.) 0 title

j] η ,, - η + s &lt;-C; / c7 '. cooled for a period of time - cool; 10 hours) to room temperature

A slow reaction is not necessary for the reaction. but prevents the pipe from breaking due to different j | Co-dilation coefficients of products and jp amp^nothe quartz '.

Slow heating times such as cooling have only been found to be very long (more than 10 hours; with impregnation and intermediate temperatures (eg 200 ° C).

30C, 400, 450ug) for 4 hours. The fact that. m Failure to perform such heating or cooling generally resulted in the explosion of the | The reaction tubes, however, the products of the condensed-spindle reactions were the same as in slow cooling, except that a small amount of residual phosphorus was found. white phosphorus instead of

1;

It's gonna be red phosphorus.

<img file="PT76047B_D0086.tif" />

19.5 one-week syremas are transferred; phosphorus nirturr- the reactant-grade droplet, having an atomic ratio of 15 to 1, milled i; of the pure balls a quartz tube with 5.5 cm of length by 2.5 cm in diameter, which in a section with a length of cm decreased to 1.0 cm in diameter, p. fc-roalizade. : 1 conditions of'atr.os¹ ff-r · dc nitrogen punch. 0 tube was pressurized rc ~

<img file="PT76047B_D0087.tif" />

(1 :: 104 Torr) the section of the smallest diameter is about one centimeter or so above the gurinti c i.argc. from the tube '.

The pipe was placed in the central zone of its furnace of three zones of the 1 H Mndberg 54357 sup ply by a second quarter pipe or lining which in turn rests on the radial center. oâ ”'ra dc heating blocks. The elements of the 3-zone emerror were controlled by 'a .. Kodclo Digital Control Pre-Generator DOe-7700 cuc allows processing to be reproducibly pre-programmed. Using the programmer, the reaction tube is subjected to the following temperatures for the indicated time intervals: 10C20.1 hour 45020, 6 hours; 30020.10 hours; 525^sG, 72 hours; 30020, 2 hours, and LOCaC, 4 hours, (when all three zones are correlated at a lower temperature, the central zoo is highly isothermal, color; a temperature range of r at dc 120 along the water).

After the furnace was cooled to room temperature, the inherent cooling rate of the furnace and reaction tube was withdrawn from it. Under dry nitrogen atmosphere conditions, the quartz vial was sheared using A silicon carbide saw was removed and removed in the dark purple polycrystalline pot. Submitting one. master of matter '?, the analysis to determine its cevp &lt;' sçãoc.

Wet analysis by wet gave a w / w. equal to about 14.2 to 1, which corresponds to a crown of 6 / c in relation to the thermal value of 15 g-1. similar assays: torsalizing the E / P gas showed the Vilares moires axorally as shown in Table SIII,

<img file="PT76047B_D0088.tif" />

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<img file="PT76047B_D0089.tif" />

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Alir. fiicco, sub ctercc-c .. morphological analysis shows several different assays', Ac fcws do? X-ray diffraction patterns and powders of these X-rays are easily equated with the Menocriatal Masters of the United Kingdom.lusíèoc poles; fear of steam cit ·:

Ic rictoàolcèi-. · Was applied, also other metal-phosphorous hazards, eoxx is indicated no. 3? '. there. The correlation between the fingers of the diin / n spectra; In the light of these materials, I try some of the cuttings obtained in the first place to establish a product in the catalog, that is to say, all of them have been converted into these tulle. pentagonal jg.rn cells of the covalently bonded phosphorus atoms.

Mo.agon of the rectal ov &lt;sfcro Red

Introduction

Λ Applicant has used the ennobolene notation to prepare homogeneous, mixed-intuition, amounts of red phosphorus with dc metals. ^r'-ruro 1a from Group 5a.

The ground products are relatively air-stable and provide breakable materials, co-handled for the technical purposes._Gdescribed above and single source conveyor condensate. The suc. stability indicates that they formed at least partially phosphorus diaphorides; n.tc- the grinding process.

Cc: 'd: po la (with the exception of lithium) have been found to be able to easily grind cc. . · = Phosphorus v? sauce in ball mills. The faoilidedu dc ηοε.ηοη becomes even more pronounced with or: easy merger notais such flight o ruhídio oor?^zreally. A problem arises when the ratio E of group l? ./ ®x- dc 1/15 to 1/7. θ increase in the content of

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crà 1 ·! · &amp; ».; gora? .r · te as a result reindeer crowding Γύ -. 'ΰ -.' ΐ. fia &lt;n.rga vas gjarefies from K &amp; ivho fie balls. Reli;

Agonorated products are easily scraped off and made to pass through a 12-inch sieve. Is lithium or ursium somewhat difficult to chew? • ucr / o only uses the standard grinding procedure c? oiv.h.on^f1&lt;5 balls due to their hardness and their wire melting points may rites.

x \ V.¹ uSi »'u3 -W.^j· .Ο-?

Ho o o vimental work. At first, use reagent grade metals and reagent grade photophoto. However, only high grade pure puresc metals are used. and red electropavable grade phosphorus and 39,999 $ (pure) purchased from Johnson uni mg.

Ih nnyv Xq Rrtrav or fig. mooing

- ·, P? ÀrÃSLAxxJiGiSho .. £ and balls .Íafiiíilll

This was originally the process chosen for the alkaline K-E systems. However, more intensive grinding processes (crimping vibratory grinding) are currently used for the other group 5a yarn. .

Stainless Steel Wire Mesh Screens Liners Fabricated »in oasa^{! l} , as shown in Figure 17, comprise a cylinder 150 cc having dimensions 11.43 and: i of outer diameter x 15.24 in height x fi, 35 mm wall thickness (4.5 ”of 0.2). x 6 ”high x 1/4 thick). The top of the mpinho has an internal flrage 151 to receive ?? a circular washer of 75.to 152. A stainless steel top 154 ​​θ nm held in place by a tight bar 155 cov. screw 1 ° C „in the ter mills. inner walls half. A second mill was built with three welded fiefleeters on the walls from top to bottom.

<img file="PT76047B_D0093.tif" />

jF.oc cc: l-varfadorra 'hr bola.sc des rf.gv.tec o origirun: u: ncagcn, more efficient, convenient to load. total â € “people less than 50-60 grenades. The hopes itials are noager. bake stainless steel balls cc. 0.655 cm in diameter (1/4 ”) was then obtained mell5.cr.; The result is one. stainless steel fool mixture dc · 0.635 c .: 0.3175 cn of the ditro (1/4 and 1/8 Λ Hcagon Crochronic. (.-196 * 0).

Rough arrow '·'¹ r-: 'i'm using a ::: - 1nio co * -gnte.ior Spcx (forced by .. Spex Industrie s, Lotuçhrn. 1I_O J.}

3-cvidc Lg Equipment Limitations,

However, the amounts (2-3 grams) may be no more than one portion; however, it may be made only at the same time as the liquid ascending times of the time. (a few minutes' grandeur). So, until; t-ionic enters another application in the furnace reduction όρο gave vaio -'uros the highest fusion bridge such as lithium or arsenic. They may then be ground together with the head in a rotary or milling rotary mill. vibratory mill.

tele-teftefteite equipment (VILItiSOl) is supplied by Tlhh. Inc., Cincinaati, Ohio.

Ho o ecseaci? Lm.er_te one. Ball mills are believed to use a mm - .. rotary mouse, produBcn-sc Circular vibrations - similar to those of a d-batteor: paint, and mill dc are 13,335 cm. -the outer diameter x 8.9 cm high x 3.175 rsa ~ c. breastfeed thickness (5 1/4 ”from 0.Ϊ). x 3 172 ”dc height x 1/8 of the thickness)» mill not containing deflectors. uses • --a oteo mainhp because of the difficulty in grinding elements such as As.

gcm 0 4 e, Ho mg om

There was a considerable variation in this shard. Generally the duration of hot milling is not less than 40 hours nor more than 100 hours. To some extent this has been determined by the system that is being milled. A shorter time is required for lower melting point Ge and Rh systems.

Grinding Temperature

The milling temperature employed was room temperature or the mills were externally heated to approximately 100 ° C with a heat lamp.

Ambient temperatures are suitable for low melting metals such as Ge (23,720) and Sb (33,92 0). The external application of the heat lamp to get 75-10020 for 3-4 hours was very beneficial for Na (97,820) and K (63,7) istsmaj.^ftG) Heating to 10f 'd was of no interest to li (108.59). It was concluded that stable products are the result of milling phosphorus with molten alkali metals.

K / P ^^ Grinding on Ball Mills

EXAMPLE IX (Reference No 88, Table XIV)

Under nitrogen atmosphere in a dry cabin, a deflector-free stainless steel ball mill was loaded containing 884 g of 0.635 cm (1/4) diameter stainless steel balls at 6.14 g (0.157 atom-gram). 99.95% pure A (from United and Chem. Co) and 72.95 g (2.36 gram atoms of 99.999% pure red P (from Johnson Natthey Chemicals). sealed are rotated in a roller station for a total of 71 hours. 0 Mill 5? heated to approximately 100 ° C for 4 hours by placing a heat lamp on its surface. The mill contents were discharged into the dry cabin to a 12 mesh screen and re-spiked. No agglomeration of the product was observed. The steel balls were separated from the product in the sieve. It obtained a total of 76.4 gd © a black powder product

Moageia_.de Ca / P? in Ball Mill

EXAMPLE X (Ref. No. 115 ₅ table XIV)

Under nitrogen atmosphere, in a dry cabin, a deflector stainless steel ball mill containing 450 g of 1/4 0.635 cm stainless steel balls^M) of diameter and 45 g of 0.3175 ca (1/8) diameter balls with 12.12 g (0.0912 atom-gram) of $ 99.98 purity (from Alpha / Ventron Corp_and) and 19.77 2 (0.638 gram-atom) of 99.999% pure worms (from Lotos and Matthey Chemicals).

was the mill sealed and rotated at a ro3 station? last 46.5 hours at room temperature. (This is only applicable; no external heat source). When the mill was opened in the dry cabin, an almost complete agglomeration of the product was observed on the mill walls. This material was scraped off with a spatula and placed in a 12 mesh sieve and container. The product pellets were then smashed into the container.

27.8 g of product.

Table XIV shows the results of milling various metals with red phosphorus. As noted earlier, these materials are surprisingly stable.

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<td> •</td><td> •</td><td></td><td> «</td><td> •</td><td> «</td>

<td>There is</td><td>h&gt;</td><td></td><td>THE</td><td>THE</td><td></td>

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<td>fc</td><td>κ</td><td>Ç</td><td></td><td>s</td><td></td>

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<td colspan="4"></td><td colspan="5">O</td>

<td></td><td></td><td></td><td></td><td></td><td>OK</td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>O)</td><td></td><td>O</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td> 3</td><td></td><td>OK</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>d</td><td></td><td>O)</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>φ</td><td></td><td>you</td><td></td>

<td></td><td></td><td></td><td></td><td>Φ</td><td>The</td><td></td><td>P</td><td></td>

<td></td><td></td><td></td><td></td><td>»D</td><td>O</td><td></td><td>φ</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>rd</td><td></td><td>The</td><td></td>

<td></td><td></td><td></td><td></td><td>good</td><td>good</td><td></td><td>O</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>G $</td><td></td><td>rd</td><td></td>

<td rowspan="2">C3</td><td></td><td></td><td></td><td>CO</td><td></td><td></td><td>good</td><td></td>

<td></td><td></td><td></td><td> »»</td><td>s</td><td></td><td>d</td><td></td>

<td>Ρ</td><td></td><td></td><td></td><td>rd</td><td>φ</td><td></td><td></td><td></td>

<td>• Η</td><td></td><td></td><td></td><td></td><td>cq</td><td></td><td>The</td><td></td>

<td>φ</td><td></td><td></td><td></td><td> 1</td><td></td><td></td><td>φ</td><td></td>

<td>good</td><td></td><td>The</td><td></td><td></td><td> \</td><td></td><td> 03</td><td></td>

<td>Ή</td><td></td><td>φ</td><td></td><td>XO</td><td></td><td></td><td></td><td></td>

<td>Η</td><td></td><td>QC</td><td></td><td>THE</td><td>O</td><td></td><td>Ό</td><td></td>

<td></td><td></td><td> \</td><td></td><td></td><td>* rj</td><td></td><td rowspan="2">THE</td><td></td>

<td>Ό</td><td></td><td>ΧΟ</td><td></td><td>φ</td><td>M</td><td></td><td></td>

<td>Α</td><td>ο</td><td>Α</td><td>O</td><td>* d</td><td>O</td><td></td><td>Φ</td><td></td>

<td></td><td>OK</td><td></td><td>OK</td><td></td><td>The</td><td></td><td>^rd</td><td></td>

<td>Φ</td><td>Οι</td><td>φ</td><td>O"</td><td rowspan="2">good</td><td></td><td></td><td></td><td></td>

<td>d</td><td>CÔ</td><td>rd</td><td>d</td><td>O</td><td></td><td rowspan="2">good</td><td></td>

<td></td><td>fl</td><td></td><td>ft</td><td>in</td><td></td><td></td><td></td>

<td>good</td><td>φ</td><td>good</td><td>φ</td><td></td><td></td><td></td><td>MO</td><td></td>

<td></td><td>The</td><td></td><td>The</td><td>CO</td><td></td><td></td><td> «»</td><td></td>

<td>d *</td><td>ο</td><td>σλ</td><td>O</td><td>CM</td><td rowspan="2">THE</td><td></td><td>CM</td><td></td>

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<td>tn</td><td>αΐ</td><td>d ·</td><td>&lt;tí</td><td>^ —S</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>ζ — w</td><td></td><td>rd</td><td></td><td></td><td></td><td></td>

<td>φ</td><td></td><td>Α</td><td></td><td>tn</td><td></td><td></td><td></td><td></td>

<td> 4-2</td><td></td><td></td><td></td><td>λ</td><td></td><td></td><td>tn</td><td></td>

<td>d</td><td></td><td> &lt;0</td><td></td><td>m</td><td></td><td></td><td></td><td></td>

<td>φ</td><td></td><td></td><td></td><td>z</td><td></td><td></td><td>m</td><td></td>

<td>• Η</td><td></td><td> - '</td><td></td><td>O</td><td></td><td></td><td>d *</td><td></td>

<td> &lt;2</td><td></td><td>Ο</td><td></td><td>ot</td><td></td><td></td><td></td><td></td>

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<td> 3</td><td></td><td> 00</td><td></td><td>O</td><td></td><td></td><td>Ot</td><td></td>

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<td></td><td></td><td></td><td></td><td></td><td></td><td></td><td>r-</td><td></td>

<td>ιη</td><td></td><td>ο</td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>η</td><td></td><td>0k</td><td></td><td>tn</td><td></td><td></td><td>m</td><td></td>

<td>d *</td><td></td><td>LD</td><td></td><td> ·»</td><td></td><td></td><td>ç*</td><td></td>

<td>cn</td><td></td><td>LD</td><td></td><td>d ~</td><td></td><td>í &gt;&gt;</td><td>ΓΠ</td><td></td>

<td></td><td></td><td></td><td></td><td>cn</td><td></td><td>Φ</td><td>d</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td></td><td>THE</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td> «</td><td></td><td>-P</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>d</td><td></td><td>-P</td><td></td><td></td>

<td>Η</td><td>d</td><td>FH</td><td>d</td><td>• d</td><td></td><td>ώ</td><td></td><td></td>

<td>φ</td><td>φ</td><td>ro</td><td>φ</td><td></td><td></td><td rowspan="2"></td><td>4</td><td>Fh</td>

<td>ά</td><td></td><td>Λ4</td><td>Í-í</td><td></td><td></td><td>Φ</td><td>ro</td>

<td>CÔ</td><td>CÔ</td><td>d</td><td>right</td><td>φ</td><td></td><td>d</td><td>Λ4</td><td>U</td>

<td>Α</td><td>Α</td><td>THE</td><td>THE</td><td>Tj</td><td></td><td>O</td><td>d</td><td>rf</td>

<td> •</td><td> «</td><td> «</td><td> •</td><td>Φ</td><td> •</td><td>ω</td><td>THE</td><td>THE</td>

<td>ΕΗ</td><td>Η</td><td>THE</td><td>E4</td><td>-P</td><td>The</td><td>d</td><td></td><td> •</td>

<td> •</td><td> •</td><td></td><td> •</td><td>•H</td><td>ro</td><td>THE</td><td>H</td><td>EH</td>

<td>Η)</td><td> ·“□</td><td>P)</td><td>Hd</td><td>d</td><td>THE</td><td>O</td><td></td><td> •</td>

<td></td><td></td><td></td><td></td><td>THE</td><td>O</td><td>l ·?</td><td>THE</td><td>THE</td>

<img file="PT76047B_D0095.tif" />

<td colspan="9">«S5 |</td>

<td>ro</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>4</td><td></td><td></td><td></td><td></td><td></td><td>m</td><td></td><td></td>

<td></td><td></td><td></td><td></td><td></td><td></td><td>ro</td><td></td><td></td>

<td>ro rd</td><td>₌</td><td> -</td><td>and</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>ro</td><td></td><td></td><td>LO</td><td>cn</td><td>ro</td><td></td><td></td>

<td> 3</td><td> +³</td><td></td><td></td><td>cn</td><td>cn</td><td>rd</td><td></td><td></td>

<td>here</td><td>ΰ</td><td></td><td></td><td> ·.</td><td>cn</td><td></td><td>Φ</td><td></td>

<td>Fh</td><td>ro</td><td></td><td></td><td>cn</td><td> ·»</td><td>d</td><td> +³</td><td></td>

<td>good</td><td>bD</td><td></td><td></td><td>cn</td><td>cn</td><td>d</td><td>d</td><td></td>

<td> \</td><td></td><td></td><td></td><td></td><td>cn</td><td>d</td><td>ro</td><td></td>

<td></td><td></td><td></td><td></td><td>M</td><td></td><td>good</td><td>bD</td><td></td>

<td></td><td></td><td></td><td></td><td></td><td>THE</td><td> \</td><td></td><td></td>

<td>ro</td><td></td><td>ro</td><td> \</td><td>ro</td><td></td><td rowspan="2">M</td><td></td><td></td>

<td>THE</td><td>THE</td><td>rd</td><td>THE</td><td>THE</td><td>ro</td><td></td><td></td>

<td rowspan="2">bD</td><td></td><td></td><td></td><td></td><td>THE</td><td></td><td></td><td></td>

<td>ro</td><td>good</td><td>Φ</td><td>bD</td><td></td><td>bD</td><td></td><td rowspan="2">THE</td>

<td></td><td>rd</td><td></td><td></td><td></td><td>bD</td><td></td><td></td>

<td>O</td><td></td><td>O</td><td></td><td>ω</td><td></td><td>O</td><td></td><td rowspan="2">bD</td>

<td>OJ</td><td>good</td><td>OJ</td><td>good</td><td>CD</td><td>GO</td><td>OJ</td><td></td>

<td> «*</td><td></td><td>Λ</td><td></td><td>«L</td><td>Λ</td><td>ç%</td><td></td><td>O</td>

<td>d</td><td>O</td><td>d</td><td>O</td><td>OJ</td><td>rd</td><td>d</td><td></td><td>LO</td>

<td></td><td>LO</td><td></td><td>m</td><td></td><td>m</td><td></td><td></td><td></td>

<td>LO</td><td>LO</td><td>LO</td><td>LO</td>

<td>THE</td><td>H</td><td>H</td><td>THE</td>

<td>THE</td><td>THE</td><td>THE</td><td>THE</td>

<td></td><td></td><td></td><td></td>

<td>M</td><td>M</td><td>M</td><td>M</td>

<td>Z ~ X</td><td>Z * “X</td><td>Z ~ S</td><td>z—</td>

<td>Φ</td><td>Φ</td><td>Q&gt;</td><td>φ</td>

<td>«V</td><td>O</td><td> ·«</td><td> «&gt;</td>

<td>d</td><td> 0$</td><td>you</td><td>you</td>

<td>XZ</td><td>XZ</td><td>X_Z</td><td>Xz</td>

<td>genius</td><td>hi</td><td></td><td>v-2</td>

<td>THE</td><td>THE</td><td>THE</td><td>THE</td>

<td>m</td><td>d</td><td>tn</td><td>M0</td>

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<td>Φ frog</td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td>

<td>Ό</td><td></td><td>Ό</td><td>Ό</td>

<td>ΡΜ</td><td>Ο</td><td>Α</td><td>Ρί</td>

<td></td><td>ϊσ5</td><td></td><td></td>

<td>Φ</td><td>Οι</td><td> (0</td><td>Φ</td>

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<td></td><td></td><td></td><td></td>

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<td> ·%</td><td>Η</td><td> ·*</td><td>"s</td>

<td>Μ-</td><td>hp</td><td>V0</td><td>Μ-</td>

<td>ΙΑ</td><td>CD</td><td>F-</td><td>Α</td>

<td></td><td></td><td></td><td>Η</td>

<img file="PT76047B_D0097.tif" />

<td colspan="4">fl</td>

<td></td><td></td><td></td><td></td>

<td>THE</td><td>✓ '' N</td><td rowspan="2">fl</td><td>x—</td>

<td>• t</td><td>cP</td><td rowspan="2">rP</td>

<td>THE</td><td></td><td>no</td>

<td>GRANDFATHER</td><td> *4-</td><td></td><td>M *</td>

<td>s""*</td><td> *</td><td></td><td></td>

<td rowspan="2">O</td><td>O</td><td>O</td><td>O</td>

<td>OJ</td><td>Hello</td><td>OJ</td>

<td>Hello</td><td>O</td><td>O</td><td>' O</td>

<td>THE</td><td>O</td><td>O</td><td>O</td>

<td>F-</td><td>rH</td><td>H</td><td>H</td>

<td>O</td><td></td><td></td><td></td><td></td><td>in</td><td></td><td>Lf \</td><td></td>

<td> ·»</td><td></td><td></td><td></td><td></td><td> ·*</td><td></td><td> »</td><td></td>

<td>CO</td><td></td><td>O</td><td></td><td></td><td>H</td><td></td><td>kO</td><td></td>

<td>co</td><td></td><td>• w</td><td></td><td> !&gt;&gt;</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>H</td><td></td><td>tD</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td>C ~</td><td></td><td>fl</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td></td><td></td><td>-P</td><td></td><td></td><td></td><td></td>

<td></td><td></td><td> »</td><td></td><td>-P</td><td></td><td></td><td></td><td></td>

<td>laugh</td><td>P</td><td>P</td><td></td><td>o3</td><td>ç,</td><td>laugh</td><td>P</td><td>laugh</td>

<td>you</td><td>Φ</td><td>• rj</td><td></td><td>isj</td><td> -/</td><td>I'm</td><td>φ</td><td>I'm</td>

<td>ç3</td><td></td><td>) g3</td><td></td><td></td><td>r- ^ ·</td><td>ϋ</td><td>Λ4</td><td>Λ4</td>

<td>nJ</td><td></td><td></td><td></td><td>laugh</td><td> &amp;</td><td>o3</td><td>CD</td><td>laugh</td>

<td>THE</td><td>THE</td><td>* d</td><td></td><td>O</td><td>THE</td><td>THE</td><td>THE</td><td>THE</td>

<td> •</td><td> »</td><td>φ</td><td> •</td><td>M</td><td> «</td><td> •</td><td> •</td><td> •</td>

<td>EH</td><td>THE</td><td>-P</td><td>s</td><td>laugh</td><td>EH</td><td>EH</td><td>EH</td><td>EH</td>

<td> •</td><td> »</td><td>•H</td><td>I'm</td><td>fl</td><td> «</td><td> •</td><td> •</td><td> •</td>

<td>ba</td><td> 1-3</td><td>P</td><td>fl</td><td>O</td><td>there is</td><td>h&gt;</td><td>H)</td><td>H)</td>

<td></td><td></td><td>THE</td><td>O</td><td>* Ί&gt;</td><td></td><td></td><td></td><td></td>

<td colspan="3">Φ</td><td colspan="2"></td><td colspan="5">O</td>

<td>Ό</td><td></td><td></td><td></td><td>THE</td><td>-d</td><td></td><td></td><td></td><td></td>

<td></td><td>Φ</td><td>«X</td><td>THE</td><td>THE</td><td></td><td>I'm</td><td></td><td></td><td></td>

<td>laugh</td><td> 4°</td><td></td><td>&lt;A</td><td>THE</td><td>laugh</td><td>-P</td><td></td><td></td><td></td>

<td>o3</td><td>P</td><td></td><td> »</td><td>THE</td><td></td><td>laugh</td><td> 5</td><td></td><td>ss</td>

<td>laugh</td><td>Φ</td><td></td><td>The</td><td> ·»</td><td>laugh</td><td>I'm</td><td></td><td></td><td></td>

<td>fcuO</td><td>fcuO</td><td></td><td>THE</td><td>THE</td><td>fccO</td><td rowspan="2">good</td><td></td><td></td><td></td>

<td></td><td></td><td></td><td> \</td><td>THE</td><td> \</td><td></td><td></td><td> \</td>

<td>w</td><td></td><td></td><td>W</td><td rowspan="2">\ THE</td><td>M</td><td></td><td>THE</td><td>THE</td><td>THE</td>

<td>I'm</td><td></td><td></td><td>I'm</td><td>I'm</td><td></td><td>I'm</td><td></td><td></td>

<td>all</td><td></td><td>THE</td><td>'d</td><td>ω</td><td>rd</td><td></td><td>rçj</td><td></td><td></td>

<td rowspan="2">bo</td><td></td><td></td><td></td><td>at</td><td></td><td></td><td></td><td></td><td></td>

<td></td><td>I'm</td><td>ω</td><td></td><td>good</td><td></td><td rowspan="2">good</td><td></td><td></td>

<td></td><td></td><td>&gt; d</td><td></td><td>uncle</td><td></td><td></td><td></td><td rowspan="2">bo</td>

<td>O</td><td></td><td rowspan="2">good</td><td>Μ-</td><td>THE.</td><td>Μ-</td><td></td><td>THE</td><td></td>

<td>OJ</td><td></td><td>Η</td><td>THE</td><td>Η</td><td></td><td>THE</td><td rowspan="2">good</td><td>M-</td>

<td> —</td><td></td><td></td><td> ·»</td><td></td><td> ·.</td><td></td><td> ·»</td><td> ·&gt;</td>

<td>M-</td><td></td><td>O</td><td>ko</td><td>cvi</td><td>grandfather</td><td></td><td>cvj</td><td rowspan="2">THE</td><td>THE</td>

<td></td><td></td><td>THE</td><td></td><td>F-</td><td></td><td></td><td>F-</td><td>THE</td>

The

Η

THE

Η

LTV ρΓ *

Μ

A αΓ¹

<td></td><td>Z-&gt;</td><td colspan="2"></td>

<td>Φ</td><td>Φ</td><td></td><td></td>

<td> ·»</td><td> ·»</td><td></td><td> »*</td>

<td>CD</td><td>you</td><td>O</td><td>O</td>

<td>z</td><td></td><td></td><td></td>

<td></td><td>S'"</td><td></td><td></td>

<td>THE</td><td>THE</td><td>THE</td><td>THE</td>

<td>F-</td><td>THE</td><td>THE</td><td>O</td>

<td>THE</td><td>THE</td><td>THE</td><td>THE</td>

'• '40 ^ QQi

ΒΜ (ΐ), β) Κ / Ρ- ^ 4.89 g E / 99.95% United Min-Chem 79.0 10020 (1 h) 44.6 g powder / un agglomerated

42.61 g of F / about Atomergics

<td colspan="4">frog</td>

<td>XD</td><td>hello</td><td></td><td></td>

<td>í&gt;</td><td>r4</td><td></td><td></td>

<td>CD</td><td>at the</td><td></td><td></td>

<td></td><td>CD</td><td></td><td></td>

<td>-P</td><td></td><td></td><td></td>

<td>CD</td><td>frog</td><td></td><td></td>

<td></td><td>CD</td><td></td><td></td>

<td>O</td><td>cP</td><td></td><td></td>

<td>-P</td><td>H</td><td></td><td></td>