Method of heat treatment and heat treatment apparatus

0001Specification

0002A heat treating method and thermal treatment equipment

0003Technical field

0004heat in the liquid phase epitaxial growth of the present invention and single crystal silicon carbide disposal method And -- it is related with thermal treatment equipment suitable for carrying it out. Background art

0005In the thermal treatment equipment used in the semiconductor manufacturing process from the former, place the heat history of Ritual is reduced -- in order to prevent generating of a slip, Processed material Thermal treatment equipment (patent-documents 1 : Provisional Publication No. 8 -- refer to No. 70008 gazette) heat-treated at high speed, it is considered as a high vacuum for a short time -- Line [ in Epitaxial growth ] with low pressure Thermal treatment equipment (patent-documents 2 : refer to Provisional-Publication-No. 1 1 1 No. 260738 gazette) which obtains and can do things etc. -- it has been reported.

0006To the thermal treatment equipment currently used for these and the conventional semiconductor manufacturing process, and the Lord Silicon carbide (henceforth S i C) It is used for Epitaxial growth. It is a Had been thing. Therefore, an operating temperature, For example, Patent documents It indicates to 1. Thermal treatment equipment, Temperature of a hot section It is 950degreeC. Patent documents. It is a statement to 2. Even if it sets to thermal treatment equipment, it is from 800"C. It is 900 degreeC.

0007However, come out as you excel in heat resistance and mechanical strength in recent years. To, it is strong also in radiation -- further -- addition of impurities -- an electron and valence electron of an electron hole Top where control is easy, It has wide prohibition belt width. (incidentally it is 3.3 e V at a 6 H type S i C single crystal with an abbreviation 3. O eV and 4H type S i C single crystal) To a sake, Silicon (henceforth S i) High temperature unrealizable in the existing semiconducting materials, such as gallium arsenide ( called the following and G a As.), The single crystal silicon carbide which can realize high frequency, and electric strength and a resistance to environment attracts attention as a next-generation power device and a semiconducting material for high frequency devices. And it is expected.

0008Hexagonal S i C, gallium nitride (it is called the following and GaN.) Rank The number of children is near and is expected as a substrate of GaN.

0009This kind of single crystal S i C, and patent documents 3 : Provisional publication of a patent 2001 -- 158695 It describes in the item gazette, it is fixed location about a seed crystal to the low temperature side in Ruppo it carries out -- arranging the powder which contains S i used as materials in the high temperature side -- a crucible -- inactive Atmosphere Heat to the high temperature of 1450degreeC thru/or 2400 degreeC in mind, S making the powder containing i sublimate and making it re-crystallize on the surface of the seed crystal by the side of low temperature -- single Connection Are formed by the sublimation re-crystallizing method (improvement Rayleigh Kazunori) for raising Crystal. There is To.

0010patent documents 4 : Provisional Publication No. 1 1 -- Describe in No. 315000 gazette. To -- like S Board constituted with the i C single crystal board, the S i atom, and C atom It is in the state where separated the minute crevice and it confronted material in parallel mutually, and is below atmospheric pressure. Inactive gas atmosphere, And it is a S iC single crystal board under S i C saturated vapor atmosphere. A side gives and heat-treats a temperature inclination so that Sheet material may also serve as low temperature. A S i atom and C atom are sublimation re-crystallized in a minute crevice, and it is S i. single -- Some which deposit a single crystal are on a crystal base board.

0011patent documents 5 : Patent Publication Heisei 10 -- Describe in No. 509943 gazette. To -- like after forming the Epitaxial layer of The 1 on a S i C single crystal with liquid phase epitaxial growth -- the CV D method -- the surface -- Up of The 2 a Taxial layer is formed -- there are some which remove a micro pipe defect.

0012To however, formation of these single crystals S i C and patent documents 3 thru/or 5 It heat-treats at like and the high temperature 1450"C thru/or 2400degreeC which are indicated. It is necessary to carry out. for this reason -- being indicated in patent documents 1 or patent documents 2 To -- in conventional thermal treatment equipment [ like ], formation of single crystal S i C is difficult To. For example, it is a growth rate in the case of the sublimation re-crystallizing method given in patent documents 3. One number 0 With 0 mu piiota/ *iota r, while it is very early, S i C powder is in the case of sublimation. Folding S i, S i C₂S i₂it is decomposed into C and evaporates -- it reacts to - part of a crucible further. For this reason, it reaches on the surface of a seed crystal by a temperature change. The kind of gas controls a difference and the partial pressure of these correctly stoichiometrically. It is very difficult technically. They are a crystal defect and microphone mouth pipe Lack of by the influence of distortion resulting from the mixed impurities and heat that it is easy to mix impurities. It is easy to generate Recess etc., Occurrence [ the crystal grain community resulting from many nuclear generation ] The problem that When and single crystal S i C stabilized in quality efficiently are not obtained It is.

0013On the other hand, it is liquid phase epitaxial growth (henceforth the L P E method) given in patent documents 4 or patent documents 5. In the case As [ see / by the sublimation re-crystallizing method ] There is little generating of a micro pipe defect, a crystal defect, etc., and it is Made with the sublimation re-crystallizing method. Single crystal S i C which was excellent in the quality target compared with that by which Construction is carried out is obtained. the -- anti- -- since a field and a growth process are controlled with the solubility of C to the inside of S i Melt -- a growth rate -- 1 it is very as late as below 0 mZ h r -- productivity of single crystal S i C it is low -- inside of a manufacture device Temperature control of the liquid phase must be carried out precisely. The manufacturing cost of a complicated next door and single crystal S i C is [ a process ] very expensive. It becomes a thing. The indication of an invention

0014the present invention was made in view of the above-mentioned problem -- a new material -- for example, -- following -- The suitable heat treating method And above-mentioned heat treating method for formation of a generation's single crystal S i C It aims at providing suitable thermal treatment equipment to carry out.

0015The heat treating method of the present invention, and how many [ following to achieve the above objects ] It mainly has the feature. In the present invention, the following main features are independent. Or it is put together suitably and has. And heat treatment of the present invention They are a device and a suitable device to enforce the heat treating method of the present invention.

0016The heat treating method concerning the present invention is abbreviation 8 at a short time about a processed material. 0 More than 0 °C is 2. 6

00170 Range below 0 °C -- Desirable -- Abbreviation 1 2 0 More Than 0 °C -- 2 3 0 Example below 0 °C Heat Chamber Heated to Predetermined Temperature in Enclosure, it connects with the above-mentioned heat chamber -- above-mentioned Callot Room before the transportation device for moving a processed material to a heat room is established, preliminary heating which is connected with the room before the above and heats the above-mentioned processed material to a predetermined temperature beforehand it is a heat treating method by thermal treatment equipment provided with a room -- the above-mentioned processed material -- Preliminarily -- pressure abbreviation 1 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P Preliminary addition of the vacuum below a a heat room -- abbreviation 8 0 after heating more than 0 °C -- beforehand -- abbreviation 8 0 more than 0 °C -- 2 6 0 0 °C -- with -- the lower range -- desirable Abbreviation 1 2 0 More than 0 °C is 2. 3 0 It is a place at within the limits below 0 °C. Pressure abbreviation 1 heated by the temperature of the law 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P the vacuum below a -- or -- beforehand -- pressure abbreviation 1 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P Addition under the thin gas atmosphere which introduced inactive gas after reaching the vacuum below a It is moving to a heat room, About the above-mentioned processed material, it is abbreviation 8 at a short time. 0 More than 0 °C is 2. 6 0 The range below 0 °C, preferably about 1 2 0 More than 0 °C is 2. 3 0 Example below 0 °C It heats to the temperature of a predetermined temperature in an enclosure.

0018according to the heat treating method of the above-mentioned present invention -- time -- about 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable about 1 2 0 more than 0 °C -- 2 3 0 Range below 0 °C since it can heat to the temperature of a predetermined temperature inside -- conventional thermal treatment equipment Then. -- a new material which was not obtained may be able to be created.

0019It can set to the above-mentioned heat treating method and the liquid phase epitaxial growth of single crystal SiC. It is suitable as a heat treating method.

0020Concretely, it is the liquid phase epitaxial growth of the single crystal silicon carbide of the present invention. Heat treating method which can be set, the single crystal silicon carbide board used as a seed crystal, and multi-crystal carbonization a silicon board is piled up -- it installs in an airtight container -- performing high temperature heat treatment By the above-mentioned single crystal silicon carbide board and the above-mentioned multi-crystal silicon carbide board ultra-thin metal silicon Melt is made to intervene during heat treatment in between -- the above-mentioned single crystal carbonization The -- base -- carrying out liquid phase epitaxial growth of the single crystal silicon carbide on a substrate It is considered as the feature.

0021and the liquid phase epitaxial growth of the single crystal silicon carbide of the present invention -- the heat treating method to kick -- the above-mentioned airtight container -- beforehand -- pressure abbreviation 10 --⁵P High truth below a While heating by an empty reserve heat chamber more than 800 degrees of abbreviation C, it is inside of the above-mentioned airtight container. Pressure abbreviation 10 --⁵P Decompress below to a and they are more than abbreviation 1400 °C and below 2300 °C beforehand. Pressure abbreviation 10_ heated by predetermined temperature by temperature within the limits²P the vacuum below a -- desirable -- abbreviation 10 --⁵the vacuum below Pa -- or -- beforehand -- pressure abbreviation 10 --⁵P Quantity below a Under the thin gas atmosphere which introduced some inactive gas after reaching a vacuum It is moving and installing in a heat chamber, The above-mentioned single crystal silicon carbide board and many crystals It is a temperature example more than abbreviation 1400 °C and below 2300 °C at a short time about a silicon carbide board. Surface microphone mouth in which it heats to a predetermined temperature in an enclosure, and a fine crystal grain community does not exist Pipe defective densities are abbreviation 1 / c m.²The single crystal silicon carbide which is the following is manufactured. Things are made into Special * Teach.

0022Thus, it is temperature within the limits more than 1400 degrees of abbreviation C, and below 2300 degreeC at a short time. Since heating to a predetermined temperature is possible, single crystal S i C can be formed efficiently. a fine crystal grain community does not exist in the inside of a growth crystal -- the density of a surface microphone mouth pipe defect -- 1/of abbreviation cm²Since it can do with the following single crystals S i C, it becomes applicable as various semiconductor devices. here, it is called a micro pipe defect also with a pinhole -- the growth direction of a crystal -- Along Number which recognizes intermediary existence It is a tubular opening of the diameter below muetaiota. Use The single crystal S i C board used as the seed crystal to carry out, and 4H -- Although it is possible in all the crystal faces of S i C and 6 H--S i C, it is To use about (0001) S i side preferably. To. In a multi-crystal S i C board, a mean particle size is abbreviation 5._muthe diameter of a particle more than m and below 10 zm -- the diameter of a particle -- abbreviated -- a uniform thing is preferred. For this reason, many crystals

0023S There is no limitation in particular in the crystal structure of i C, and it is 3 C. -- Although both S i C 4 H--S i C and 6 H - S i C can be used, it is 3 C preferably. -- It is S i C.

0024moreover -- according to the present invention, in Si, Wet permeates all the corners of an interface according to capillarity between a single crystal S i C board and a multi-crystal S i C board at the time of heat treatment The -- an ultra-thin metal S i melting layer is formed. C atom which flowed out of the multi-crystal S i C board is supplied to a single crystal S i C board through a S i melting layer -- the single Connection Liquid phase epitaxial growth is carried out as single crystal S i C on a Crystal S i C board. For this reason, indecement of a defect can be controlled from the early stages of growth to an end. Former Like, since it does not need to be immersed during fusion S i and it is not necessary to process, the quantity which removes S i used as a seed crystal decreases extremely after heat treatment. [ a single crystal S i C board and ] [ multi-crystal S i C ] Since ultra-thin metal S i Melt is made to intervene during heat treatment between a single crystal S i C board and a multi-crystal S i C board, only metal S i required for Epitaxial growth of single crystal S i C can be used for the liquid phase epitaxial growth of single crystal S i c. For this reason, in a S i layer thin at the time of heat treatment, contact surface products with the exterior are the minimum, therefore Entry confirmation of impurities. form ^ A rate can carry out decrease and high purity single crystal S i C.

0025The thermal treatment equipment of the present invention is pressure abbreviation 1 CT about a processed material.²P It is [ below a ] desirable. Abbreviation 1 0_⁵P the vacuum below a -- or -- beforehand -- pressure abbreviation 1 0 --²P It is preferably below in a. Abbreviation 1 0 -⁵P inactive gas was introduced after reaching the vacuum below a -- thin in the bottom of a gas atmosphere -- a short time -- about 1 2 0 more than 0 °C -- 2 3 0 Warm below 0 °C Heat chamber which is degree within the limits and it heats to a predetermined temperature, room before the transportation device for connecting with the above-mentioned heat chamber and moving a processed material to the above-mentioned heat chamber is established it connects with the room before the above -- the above-mentioned processed material -- abbreviation 1 0 --²P It is [ a or less ] desirable. About 1 0 --⁵P In the vacuum below a, it is abbreviation 8 beforehand. 0 Reserve heated more than 0 °C It has the heat chamber.

0026moreover Thermal treatment equipment of the present invention, Inside of a vacuum high temperature furnace Plurality of 2 or more Chestnut Consist of a separated tub. The insides of a tub of a plurality of are from the main heating tub and a preliminary heating tub. It is constituted and builds in gas and a sample by which the above-mentioned preliminary heating tub mainly stuck to a sample. It is abbreviation from room temperature because of Depart gas of gas. It is heated by 8 0 0 °C, It is Fast to above-mentioned main heating tub that heating vacuum exhaust air is beforehand carried out, and is held under pure high temperature after an end of Depart gas. It is moved to Or, Above-mentioned main heating tub is always abbreviation. Pressure below 1 0-3 P a, Or it is abbreviation once. After reaching pressure below 1 0-3 P a Some inactive gas It introduces, Under a thin gas atmosphere of arbitrary pressure from atmospheric pressure to abbreviation 1 0-3 P a Abbreviation More than 8 0 0 °C It is always to high temperature of a predetermined temperature at within the limits below 2 6 0 O °C. It is heated. From the atmospheric pressure for receipts and payments of the above-mentioned preliminary heating tub of a sample, It is required in order to move a sample between the above-mentioned main heating tubs, Above-mentioned main heating tub. It has a function which can be exhausted to equivalent pressure, From room temperature to abbreviation It is a sample to temperature of 8 0 0 °C. After carrying out preliminary heating It moves to above-mentioned main heating tub early, a sample -- the maximum -- . Proper place About management temperature More than 8 00 °C Temperature predetermined by temperature within the limits below 2 6 0 0 °C Have a high temperature heating furnace which attains high temperature and high purity atmosphere promptly. It is considered as the feature.

0027In order to heat the thermal treatment equipment of the present invention, and a sample quickly again, Vacuum High temperature furnaces are separation and a high purity atmosphere to two, the main heating tub and a preliminary heating tub. In order to maintain, each vacuum pumping system which each interior of a room became independent of -- or -- Are maintainable in each independent gas introduction system and atmospheric pressure atmosphere. And the main heating tub and preliminary heating Tank power By opening and closing of an interception valve, it is a phase about unification and separation. In the thermal treatment equipment which has the high-speed high temperature heating furnace currently maintained by Mutually, The above-mentioned main heating tub is always abbreviation 1 to civil time. 0 - Pressure below 3 P a, Or once Abbreviation 1 0 After reaching the pressure below -3 P a, Some inactive gas is introduced and it is abbreviation 1 from atmospheric pressure. 0 - It is abbreviation 8 under the thin gas atmosphere of the arbitrary pressure to 3 P a. 0 It holds to the high temperature condition of a predetermined temperature by temperature within the limits more than 0 degreeC and below 2600 degreeC. It is carried out, The above-mentioned preliminary heating tub is temperature within the limits beyond abbreviation room temperature and below 1000 degreeC. Built-in which occurs from a sample etc. in the state where it is held at a predetermined temperature The cold trap for adsorbing gas is built in, high temperature after the end of heating from -- the gas circulation device for rapid cooling for cooling promptly is built in room temperature It has a High temperature heating furnace. Brief explanation of the drawings

0028Liquid phase Epita Takisha of single crystal S i C which requires Drawing 1 for one embodiment of the present invention It is an outline sectional view of one embodiment of the thermal treatment equipment used for the Le growing-up method. Outline which shows an example of the airtight container in which Drawing 2 is used for one embodiment of the present invention It is a figure.

0029Drawing 3, It is a figure showing the inside of the airtight container in one embodiment of the present invention. The state where Drawing 4 installed the substrate in the lower container in one embodiment of the present invention It is a shown figure.

0030Drawing 5 (a) and Drawing 5 Reflector used for (b) and one embodiment of the present invention It is a schematic diagram showing an example.

0031Drawing 6 (a) and a figure -- 6 Heat treating method concerning (b) and one embodiment of the present invention Micro [ of the surface of the growth layer of single crystal S i C obtained by And thermal treatment equipment ] It is a figure showing a mirror photograph. Figure 6 (a) is surface morphology and Drawing 6. (b) is a figure showing the microphotograph in which the section is shown.

0032Drawing 7 (a) and a figure -- 7 (b) -- Drawing 6 (a) And figure 6 it is a figure showing the AFM image of the surface of single crystal S i C shown in (b) -- Drawing 7 (a) and surface morphology 1 and Drawing 7 (b) is a figure showing the AFM image in which the section is shown.

0033Drawing 8 (a) and Drawing 8 (b) and a figure -- 8 (c) and one embodiment of the present invention -- charge Growth fault of single crystal S i C obtained by Heat treatment method and thermal treatment equipment like -- it is a figure for explaining the step punching mechanism in which it can set.

0034Drawing 9 (a) figure 9 Heat treatment equipment in other embodiments which require (b). for the present invention It is a sectional view of the principal part of Place.

0035Drawing 1 figure in which 0 shows the relation of the spectrum radiation rate and reflectance under the high temperature of W it is . .

0036Drawing 1 1 is 1. 8 0 More than 0 °C is 2. 6 0 Wavelength energy of W below 0 °C It is a figure showing 1. '

0037Drawing 1 2 shows the spectrum reflective characteristic of A u covered on the surface of metal light reflector 5. It is a figure.

0038Drawing 1 The principal part of thermal treatment equipment applied to other embodiments furthermore it starts 3 and the present invention It is a sectional view.

0039Drawing 1 4 is Drawing 1. It is a figure showing the example of the heating temperature characteristic concerning the embodiment shown in 3, and is Ah. To.

0040Drawing 1 Thermal treatment equipment in other embodiments again furthermore 5 starts the present invention It is a sectional view of the principal part. The best form for inventing

0041hereinafter -- boiling and attaching an example of the thermal treatment equipment concerning the present invention, referring to drawings It explains.

0042Drawing 1, It is a section schematic diagram showing an example of the thermal treatment equipment concerning the present invention. In Drawing 1, it is [ thermal treatment equipment 1, heat chamber 2, reserve heat chamber 3, and ] preliminary heating. It comprises room 4, before following heat chamber 2 from room 3. And it is single Connection by processed material 5 moving to before room 4 and heat chamber 2 one by one from reserve heat chamber 3. It is constituted so that Crystal S i C may be raised.

0043it is shown in Drawing 1 -- as -- thermal treatment equipment 1, heat chamber 2, reserve heat chamber 3, and before room 4 are open for free passage. For this reason, thing for which each A room is beforehand controlled under predetermined pressure It becomes possible. It is also possible by providing gate valve 7 grade for every A room to carry out pressure regulation for every A room. The inside of the furnace under specified pressure is illustrated, without touching the open air by this also at the time of movement of processed material 5. Since it can be made to move by the transportation device which is not, it is mixing of impurities, etc. It can control.

0044Callot, such as lamps, such as reserve heat chamber 3 and a halogen lamp, or a rod heater heat means 6 is established -- rapid -- 8 0 more than 0 °C -- 1 a below 0 O 0 °C grade -- Addition It is a heating furnace in which heat is possible. as a heating method -- halogen lamp etc. a lamp type heating method -- good -- better! / moreover Reserve heat chamber 3 and before room Connection with 4 Portion Gate valve 7 provides -- It has. Room before reserve heat-chamber 3 And. Pressure control of 4 is made easy.

0045It is in the state laid in table 8 in processed material 5 and reserve heat chamber 3, and is a place. About 1 which is the pressure of a law 0"²P Below a is about 1 preferably. 0 --⁵vacuum below Pa the bottom -- eight 0 susceptor 9 of the rise-and-fall type provided in before room 4 as soon as the pressure regulation of reserve heat chamber 3 after being beforehand heated more than 0 °C, and before room 4 ends -- Install -- it is moved like.

0046Transfer of processed material 5 moved to before room 4, and the rise-and-fall type currently illustrated in part Dynamic means 1 It is moved to heat chamber 2 by 0 from before room 4. Abbreviation 1 which is predetermined pressure beforehand in heat chamber 2 this time in Les and vacuum Pump to illustrate 01¹P Below a is abbreviation 1 preferably. 0 --²P Below a is about 1 still more preferably. 01⁵the vacuum below Pa -- or -- beforehand -- pressure abbreviation 1 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P Introduce some inactive gas after reaching the high vacuum below a, and it is about 1. 0 -- It is abbreviation 1 preferably hereafter. 0_²P it carries out under the thin gas atmosphere below a -- heating Hee Tha 1 1 -- abbreviation 8 0 more than 0 °C -- 2 6 0 the range below 0"C -- desirable -- abbreviation 1 2 0 more than 0 °C -- 2 3 0 Being set below to 0 °C is preferred.

0047The state in heat chamber 2 is set up in this way, and processed material 5 is moved into heat chamber 2 from before room 4, processed material 5 -- abbreviation 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable -- about 1 2 0 more than 0 °C -- 2 3 0 Below 0 °C It can heat quickly to a predetermined temperature by within the limits.

0048moreover Heat chamber 2 Heating heater the circumference of 1 1 -- reflector 1 2 are arranged. ing. Heating heater. Heat of 1 1 is reflected and it is a heating heater. It is To position to an inside of 1 1. To be processed He is trying to concentrate on 5 sides.

0049this reflector 1 Even if it is a thing of the shape of a case as shown in Drawing 1, compare 2. The and a figure -- 5 (a) and Drawing 5 Reflector 1 of the shape of a dome as shown in (b) It is referred to as 2. Things are also made. thus, reflector 1 By making 2 into the shape of a dome, it is heating. Heater 1 1 -- plate-like it also becomes possible to use a heater -- plate-like Heating heater 1 Even if it is a case where 1 is used Heating heater 1 Heat from 1 It can be made to concentrate on processed material 5 efficiently.

0050Transportation device 1 Fitting part 2 of 0 and heat chamber 2 5 is transportation device 1. It is provided in 0. ing convex part 2 with the stage 1 and with the stage of the concave currently formed in heat chamber 2 Part 2 It comprises 2. and transportation device 1 Part 2 with the stage of 0 1 -- each -- sealing members, such as O ring which is provided in the step and which is not illustrated, -- Addition Heat room 2 will be in the state where it was sealed.

0051Heating heater 1 in heat chamber 2 In the inner side of 1, it is Leak out of processed material 5. About the contaminant come out of and carried out, it is heating heater 1. Contamination removal removed so that 1 may not be contacted Removal mechanism 2 0 is provided. By this, it is heating heater 1. 1 is a contaminant. It reacts and can control deteriorating. In heat treatment [ in / as the above-mentioned contaminant / the liquid phase epitaxial growth of single crystal SiC ], it is S i steam. It is mentioned.

0052thus, Stain, such as silicon steam leaked from an airtight container in a heat chamber Since the contaminant removal mechanism in which dyed goods are removed is established, provide in a heat chamber. , -- degradation by contaminants, such as silicon steam of the heating method of a Being done heater etc. It can prevent. Here, as a contaminant removal mechanism, he is vacuum Bon. A, other general exhaust means, etc. can be used.

0053This contaminant removal mechanism 2 The contaminant leaked out of 0 and processed material 5 is removed. If it carries out, it will not be limited in particular.

0054Heating heater 1 1, Metal resistance heating To, such as a product made from black lead, or tantalum It is - Tha. Susceptor. Base heater currently installed in 9 1 1 a, Flank And top heater with which the upper part was formed in one cylindrical It comprises l i b. It is. Thus, it is heating heater 1 so that processed material 5 may be covered. 1 is arranged. For a ing reason, it becomes possible to heat processed material 5 equally. '

0055It is Limit to the heating method of heat chamber 2, and the resistance heating heater shown in this embodiment. Constant may not be carried out and you may be a high-frequency-induction heating type, for example. As processed material 5, it is the liquid phase epitaxial growth of single crystal SiC. In the heat treatment which can be set, it is preferred to use airtight container 5 which comprises upper container 5 a as shown in Drawing 2, and lower container 5 b. Like and single crystal S i C board 1 which are mentioned below in this airtight container 5 They are lamination and Yield about 6 and a multi-crystal S i C board. It heat-treats by carrying out Payment (refer to Drawing 3).

0056as [ show / in Drawing 2 / airtight container 5 ] -- upper container 5 a and lower container 5 b -- style it accomplishes -- being formed by either tantalum or tantalum carbide, respectively -- Les and To.

0057The airtight container is formed by tantalum or tantalum carbide, and, for . To reason, it is Airtight container. While controlling S i C-ization of a vessel, it is pressure abbreviation 1 certainly about the inside of a heat chamber. 0 -²P Below a can carry out.

0058And it inserts in and is [ of upper container 5 a and lower container 5 b ] A play of the fitting part at the time. It is preferred that it is below abbreviation 2 mm. By this, it is to into airtight container 5. Mixing of impurities can be controlled. play -- below abbreviation 2 mm and To By To, below 10 P a does not become about the S i partial pressure in airtight container 5. It is also controllable for obtaining. For this reason, they are height and single crystal S i C board 1 about the S iC partial pressure And S i partial pressure in airtight container 5. 6 Many crystal S i C board 1 4 and 1 5 and ultra-thin metal S i Melt 1 It comes to contribute to prevention of sublimation of seven. When [ of this upper container 5 a and lower container 5 b ] it inserts each other in and play of the fitting part at the time is larger than abbreviation 2 m m, This which controls Si partial pressure in airtight container 5 to predetermined pressure For a certain reason, it is not preferred that it not only becomes difficult, but impurities invade in airtight container 5 via this fitting part. this airtight container 5 -- a figure -- not only the thing of a square but shape may be circular as shown in 2. thus, the above-mentioned airtight container is formed with an upper container and a lower container -- 'above top Capacity the grade to which silicon steam begins to leak from the fitting part of a vessel and the bottom container of the above -- being the above-mentioned -- dense Control so that the pressure in a closed container becomes higher than the pressure in the above-mentioned heat chamber. It controls that impurities mix in the above-mentioned airtight container.

0059making an airtight container into such a structure -- the inside of an airtight container -- impure Mixing of a thing can be controlled. By this, it is bag grand abbreviationX[ 5 ] 1. 0¹⁵/ c m³It can do with the following purity.

0060Like and three supporters 1 which are shown in lower container 5 b figure 3 And figure 4 3 is provided. This supporter 1 By 3, it becomes a seed crystal mentioned below. Multi-crystal S i C board 1 4 is supported. ', in addition supporter 1 3, this operation form It is not necessary to be a thing of the shape of a pin as shown in voice for example, and is a form at S i C etc. It may be the accomplished ring shape thing.

0061To the inside of airtight container 5 in the state where upper container 5 a and lower container 5 b fitted in in Drawing 3 6 H type single crystal S i C board 1 used as the seed crystal currently installed 6, this -- single -- Crystal S i C board 1 Multi-crystal S i C board 1 which puts 6 Between 5 and these Ultra-thin metal S i Melt 1 formed The state of 7 is shown. ultra-thin metal S i Melt 1 7 is formed at the time of heat treatment -- this ultra-thin metal S i Melt 1 Become a source of S i of 7, Single crystal S i C board 1 used as a seed crystal The 6 surfaces It is abbreviation 1 by CVD etc. about metal S i beforehand. It is set to 50 muiotaeta from 0 mupiiota. Bat is formed or the methods in particular, such as placing S .i powder, are not limited. it is shown in Drawing 3 -- as -- * Place is carried out at supporter 13 formed in lower container 5 b which constitutes these single crystal S i C boards 16, multi-crystal S i C board 14, 15 and ultra-thin metal S i Melt 17, and airtight container 5 -- the inside of airtight container 5 -- storage -- Being done. Single Connection produced by single crystal S i C board 16 and the sublimating method here Crystal 6H -- It is started by desired size (more than 10 X 1 Omm below 20 X 2 Omm) from Ayer of S i C. What was started by the desired size from S i C used as Dummy Wave by the S i semiconductor manufacturing process by which multi-crystal S i C board 14 and 15 were produced by the C V D method It can be used. each of these substrates 16, 14, and 15 -- the surface -- specular surface polish processing is carried out -- oil adhering to the surface, an oxide film, metal, etc. -- washing etc. It is removed. multi-crystal S i C board 14 located in the lower part side here -- single -- the erosion from airtight container 5 of crystal S i C board 16 is prevented -- quality of single crystal S i C which carries out liquid phase epitaxial growth on single crystal S i C board 16 It contributes to improvement.

0062It can also install with the piece of S i for controlling sublimation of S i C at the time of heat treatment in this airtight container 5, and evaporation of S i. S i pieces By installing simultaneously, it sublimates at the time of heat treatment, and they are height, single crystal S i C board 16 and multi-crystal S i C board 14, 15, and ultra-thin metal S i Melt 1 about the S i C partial pressure and S i partial pressure in airtight container 5. It comes to contribute to prevention of sublimation of seven. it becomes higher than the pressure in heat chamber 2 about the pressure in airtight container 5 -- as -- it can adjust -- this -- usual state from the fitting part of upper container 5 a and lower container 5 b S i steam can be emitted and invasion into airtight container 5 of impurities can be prevented. About 10 after airtight container 5 constituted in this way was installed in reserve heat chamber 3 --²P Below a is about 10 preferably. --⁵P it is set below to a -- reserve Callot the lamp formed in heat room 3 -- and -- or it is heated by heating methods 6, such as mouth Dod heater, more than 800 degrees of abbreviation C, preferably more than 1000 degrees of abbreviation C. Under the present circumstances, the inside of heat chamber 2 is about 10 similarly. --²P Below a is about 101 preferably.⁵P Heat the range more than about 800 degreeC and below 2600 degreeC, and good It is to a predetermined temperature of the range more than 1200 degrees of abbreviation C, and below 2300 degreeC after being set below to a. Carrying out is preferred.

0063Airtight container 5 by which preliminary heating was carried out within reserve heat chamber 3, It is Open about gate valve 7. It comes, it moves to susceptor 9 of before room 4, and is moved by ascending and descending means 10 into the range more than 800 degrees of abbreviation C, and below 2600 °C, and heat chamber 2 currently preferably heated by the predetermined temperature of the range more than abbreviation 1200 °C and below 2300 °C. this -- airtight container 5 -- a short time for less than about 30 minutes -- rapid -- abbreviation 80 the range below 0 or more and 2600 degreeC -- desirable -- about -- more than 1200 °C -- 230 It is heated by the predetermined temperature of the range below 0 °C. It is that at the heat treatment temperature in heat chamber 2, and the temperature which the piece of metal S i currently simultaneously installed in airtight container 5 fuses. Although The is good, in this embodiment, it is an example more than 1200 degrees of abbreviation C, and below 2300 degreeC. It is considered as a predetermined temperature of an enclosure. the wettability of fusion S i and S i C goes up, so that treatment temperature is performed at high temperature -- fusion S i permeates easily according to capillarity between single crystal S i C board 16, multi-crystal S i C board 14, and 1 *. By this, it is single crystal S i C board 16, multi-crystal S i C board 14, and 15. Making ultra-thin metal S i Melt 17 below thickness abbreviation 50 muiotaeta intervene in between It can do.

0064according to the thermal treatment equipment concerning this embodiment -- a short time -- 800 degrees of more than abbreviation C -- 26 the range below 00"C -- desirable Example more than about 1200 degreeC and below 2300 degreeC Since it is possible to consider it as a predetermined temperature in an enclosure, it is The end at a short time about crystal growth. It becomes possible to complete and the increase in efficiency of crystal growth is attained.

0065heat treatment time and single crystal S i C generated serve as desired thickness It is possible to choose suitably for obtaining. here, if metal S i used as the source of S i and quantity increase, the quantity fused at the time of heat treatment will increase -- ultra-thin metal S i Melt Abbreviation 5 If it becomes the thickness more than 0 mu m metal Si Melt becomes unstable -- transportation of C is checked again -- not suitable for training of single crystal S i C S i which is not required for formation of single crystal S i C fuses, and accumulates in the bottom of airtight container 5 -- it will be necessary to solidify again and to remove . Metal S i after single crystal S i C formation this For -- single crystal S i C formed about the size And thickness of metal S i -- a large -- It unites with Tears and chooses suitably.

0066By the way, when the growth mechanism of single crystal S i C is explained briefly, It follows on heat treatment and is single crystal S i C board 1. Multi-crystal S i C board 1 of 6 and the upper part S i fused among 5 invades and they are both substrates 1. 6 and 1 It is thickness abbreviation 3 to the interface of 5. More than 0 mu etaiota is 5. Metal S i melting layer 1 below 0 mu m 7 is formed. This metal S i melting layer 1 It becomes thin as 7 and heat treatment temperature become high temperature, and it is about 3.

00670 It becomes a mu etaiota grade. and C atom which flowed out of multi-crystal S i C board 2 letting a S i melting layer pass -- single crystal S i C board 1 6 is supplied -- this single crystal S

00681 It is 6 H on C board 1. -- Liquid phase epitaxial growth is carried out as a S i C single crystal (henceforth L P E). Thus, single crystal S i C machine used as a seed crystal Board 1 6 and multi-crystal S i C board 1 Since between 4 is small, it is a heat convection at the time of heat treatment. It does not generate. for this reason, it becomes single crystal S i C and the seed crystal which are formed -- single -- Crystal S i C board 1 6 and an interface become very smooth -- this interface -- distortion etc. It is not formed. Therefore, very smooth single crystal S i C is formed. Since nuclear generation of S i C is controlled at the time of heat treatment, generation of the minute crystal grain community of single crystal S i C formed can be controlled. He is charge to this embodiment. In the training method of Single crystal S i C, fused S i -- single crystal S i C board 1 6 and multi-crystal S i C board 1 Invading-only among 5 power , -- others -- un--- in order not to invade into single crystal S i C in which a pure thing grows -- Bagdha land abbreviationX[ 5 ] 1 0¹⁵A c m³The following single crystals S i C of high purity are generated. It becomes possible.

0069The thermal treatment equipment concerning these above embodiments is pressure abbreviation 1 about a processed material. 01²P Below a, preferably abbreviation 1 0 --⁵P the vacuum below a -- or -- beforehand -- pressure abbreviation 1 0"²P Preferably [ below a ] it is abbreviation 1. 0 --⁵P after reaching the vacuum below a -- non-Active in the bottom of the thin gas atmosphere which introduced sex gas -- a short time -- about 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable abbreviation 1 2 0 more than 0 °C -- 2 3 0 Below 0"C it connects with the heat chamber heated in the temperature range, and the above-mentioned heat chamber -- the above-mentioned heat chamber The room before the transportation device for moving a processed material is established, and front [ 'above ] room being connected -- the above-mentioned processed material -- abbreviation 1 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P In the vacuum below a, it is abbreviation 8 beforehand. 0 It is Provision 7 To about the reserve heat chamber heated more than 0 °C.

0070And according to the thermal treatment equipment concerning this embodiment, it is pressure abbreviation 1. 0 --²P Below a is abbreviation 1 preferably. 0 -⁵P the vacuum below a -- or -- beforehand -- pressure abbreviation 1 0 --²P Below a Preferably it is abbreviation 1. 0 --⁵P After reaching the high vacuum below a, it is some inactive gas. It introduces and is abbreviation 1. 0 -¹P Below a, preferably abbreviation 1 0 -²P thin gas below a it sets under atmosphere -- a short time -- abbreviation 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable About 1 2 0 More than 0 °C is 2. 3 0 Since it can heat to a predetermined temperature by within the limits below 0 °C, It is the surface which was difficult in the liquid phase growing-up method of conventional single crystal S i C (the L P E method) the case where single crystal S i C is formed as a processed material. Abbreviation 1 This which forms single crystal S i C with the broad terrace more than 0 mu m It becomes possible.

0071It is Pressure beforehand about the heat treating method concerning the embodiment of the present invention, and the above-mentioned processed material. Power 1 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P reserve heat chamber of the vacuum below a Abbreviation 8 0 after heating more than 0 °C -- beforehand -- abbreviation 8 0 more than 0 °C -- 2 6 0 Below 0 °C the range -- desirable Abbreviation 1 2 0 More than 0 °C is 2. 3 0 It is predetermined at within the limits below 0 °C. Pressure abbreviation 1 heated by temperature 0 --²P Below a is abbreviation 1 preferably. 0 --⁵P below a a vacuum -- or -- beforehand -- pressure abbreviation .1 0 --²P Below a is abbreviation 1 preferably. 0_⁵P Below a Heat chamber under the thin gas atmosphere which introduced inactive gas after reaching a vacuum It is moving, the above-mentioned processed material -- a short time -- abbreviation 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable -- about 1 2 0 more than 0 °C -- 2 3 0 Range below 0 °C It is a heat treating method heated to the temperature of a predetermined temperature inside.

0072Liquid phase Epita Takisha of the single crystal silicon carbide concerning the embodiment of the present invention Heat treating method in the Le growing-up method, single crystal silicon carbide board used as a seed crystal a multi-crystal silicon carbide board is piled up and it installs in an airtight container -- high temperature heat treatment Carry out, the above-mentioned single crystal silicon carbide board and the above-mentioned multi-crystal carbonization Cay base -- doing . intervention of ultra-thin metal silicon Melt during heat treatment between substrates -- the above -- single -- a crystal silicon carbide board top -- single crystal silicon carbide -- liquid phase epitaxial growth It is a heat treating method to carry out.

0073And it is pressure abbreviation 1 beforehand about the above-mentioned airtight container. 0 --²P With the reserve heat chamber below a About 8 0 While heating more than 0 °C, it is pressure 1 [ about ] about the inside of the above-mentioned airtight container. 0 --⁵P it decompresses below to a -- beforehand -- abbreviation 1 40 0 -- the above -- 2 3 0 within the limits below 0 °C -- predetermined Pressure abbreviation 1 heated by temperature 0 --²P Below a is abbreviation 10 preferably. -⁵below Pa a vacuum -- or -- beforehand -- pressure abbreviation 1 0 --⁵P Inactive gas is introduced after reaching below a. It is moving and installing in the heat chamber under the thin gas atmosphere carried out, the above-mentioned single crystal a silicon carbide board and a multi-crystal silicon carbide board -- a short time -- abbreviation 1 more than 400 °C -- 2 3 0 heating to a predetermined temperature by temperature within the limits below 0 °C -- Existence of a fine crystal grain community In is not carried out -- the microphone mouth pipe defective density of the surface -- abbreviation 1 / c m²it is the following -- single -- Crystal silicon carbide is manufactured.

0074in addition, the time of moving the above-mentioned airtight container to the above-mentioned heat chamber -- the above-mentioned airtight container a difference in temperature is not provided in the direction of an axis -- the field inboard of the above-mentioned airtight container -- a temperature gradient -- Establishment controlling Over and the above-mentioned temperature gradient arbitrarily -- generation of a fine crystal grain community -- Depression It controls. The direction of an axis of the above-mentioned airtight container is the above-mentioned single crystal charcoal within the above-mentioned airtight container. Meaning the direction where a-izing silicon board and a multi-crystal silicon carbide board are laminated, the field inboard of the above-mentioned airtight container means the perpendicular direction, i.e., the plane direction on the surface of a crystal, to the above-mentioned laminating direction.

0075in order not to provide a difference in temperature in the direction of an axis of an airtight container -- single crystal S i C machine since a difference in temperature is not formed between a board and a multi-crystal S iC board -- thermal equilibrium state it becomes possible to heat-treat -- since metal S i Melt is thin again -- heat convection It is controlled. For this reason, indecement of a defect can be controlled from the early stages of growth to an end. Since nuclear generation is controlled at the time of heat treatment, generation of the minute crystal grain community of single crystal S i C formed can be controlled. Simple thermal treatment equipment is used. Made since the strict temperature control at the time of heating is unnecessary while things are made Large reduction-ization of Construction cost is attained. To in addition, the field inboard of an airtight container This temperature gradient is arbitrarily controlled by establishing a temperature gradient, the time of growth of single crystal S i C -- a fine crystal grain community -- the low temperature side from the high temperature side of a temperature gradient single crystal S i C can be grown up so that it may be made to move -- as a result -- microphone mouth pipe defective density -- abbreviation 1 / c m²The following single crystals S i C are formed. Things are made.

0076The above-mentioned ultra-thin metal S i Melt is about 5. It is the thickness below 0 mu m.

0077It intervenes during heat treatment between a single crystal S i C board and a multi-crystal S i C board. To ultra-thin metal S i Melt is abbreviation 5. Below 0 mu m is abbreviation 3 preferably. It is Ah below in 0 m. To sake, C dissolved from the multi-crystal S i C board -- a single crystal S i C substrate face -- Expansion it is conveyed by Scatter -- growth of single crystal S i C is promoted. above-mentioned ultra-thin metal Si recon Melt -- abbreviation 5 When it becomes the thickness more than 0 mu m, metal silicon Melt is uneasy. it becomes a law -- transportation of C is checked again -- it is not suitable for training of single crystal S i C. the same as that of high temperature heat treatment environment, such as the conventional sublimating method, according to such the present invention High temperature can perform local liquid phase epitaxial growth in an environment. a sake -- a seed crystal -- containing -- having -- a micro -- a pipe -- a defect -- not succeeding -- Mike Lopa An eve defect can be blockaded. The growth surface is always S i Melt. In order to touch, while generating of the defect which the state where S i is superfluous is formed and originates in shortage of S i is controlled, contact surface with the exterior of S i Melt currently used since the product is minute, mixing of the impurities on the surface of growth can be controlled -- it is a crystal at high purity Quality highly efficient single crystal S i C excellent in the sex is raisable. deer it compares with the conventional LP gas E method -- the Motoshige chief method is very high temperature -- it is growth in a short time comparing with the conventional L P E method, since it is possible -- a growth rate -- remarkable -- quick -- To do is made -- making very high training efficiency of quality single crystal S i C It can do. The necessity of carrying out temperature gradient control strict at the time of single crystal growth It becomes possible to be based on To and a simple device. It compares with the existing departments of semiconductor material, such as S i G a A s, from these things, and they are high temperature, high frequency, electric strength, and environment-proof. It excels in a sex and is expected as a department for a power device and high frequency devices of semiconductor material. Utilization of ing single crystal S i C can be promoted.

0078Drawing 6 (a) and a figure -- 6 It is a figure showing the microphotograph in which (b) and the surface state of single crystal S i C where it grew up by the above-mentioned method are shown. Drawing 6 (a) -- surface Morphology 1 and a figure -- 6 (b) shows the section. Drawing 6 (a) -- and -- Drawing 6 as [ show / in (b) ] -- the growth surface of the crystal by the LPE method -- very much -- common A Rugged terrace and step structure are observable.

0079Drawing 7 (a) and a figure -- 7 (b) and this surface -- atomic force microscope (henceforth A FM) It is a figure showing the observed result. Drawing 7 (a) -- and -- Drawing 7 observable from (b) -- as -- the height of a step -- respectively -- about [ abbreviation 4. 0 nm and ] -- it turns out that it is 8. 4 nm. height of the integral multiple [ this ] based on three molecular layers of a S i C molecule (the height of S i C 1 molecular layer is 0. 25 etapiiota) it is . Thus, it turns out that it is the very flat surface. thus, the surface of the above-mentioned single crystal S i C made three molecular layers the minimum unit it has an atomic order step and a broad terrace -- the width of the above-mentioned terrace -- abbreviation

00801 It is more than 0 m.

0081Since terrace width is more than abbreviation 1 omicron mupiiota, it is not necessary to carry out the surface treatment by machining etc. after the growth surface and single crystal S i C formation. For this reason, processing It becomes possible to also use When as a product not through a process.

0082Drawing 6 (a) and a figure -- 6 from the Appearance * Floor mirror photograph of the surface form of (b) -- Become -- a micro pipe defect is not observed on like and the surface. these things , -- single crystal S i C and the surface which were obtained by the thermal treatment equipment by the present invention the density of the micro pipe defect formed -- abbreviation 1/c²very as few as the following the width of the terrace formed in To and the surface is as wide as more than abbreviation 1 O^m -- it turns out that it is flat and there are few defects.

0083It is carried out for every [ generally and ] Epitaxial growth of a crystal, and molecular layer. however -- single crystal S i C concerning this embodiment -- the surface -- more than abbreviation 1 omicron mu** the step of the height which made a broad terrace and three molecular layers the minimum unit -- composition -- Being done. Step bunching is Cause at the process of this to crystal growth. It is thought that it came. The surface in this step bunching mechanism and crystal growth The effect of free energy can explain. He is charge to this embodiment. Single crystal 6 eta -- The direction of AB C and two kinds of lamination cycles called ACB is in S i C and a unit lamination cycle. Then, from the layer in which a laminating direction bends They are Drawing 8 and Drawing 8 by numbering with 1, 2, and 3. (b) And figure 8 As shown in (c), three kinds of surfaces can be specified. and energy of each field Ruki 1 The following like -- Demand -- , -- Have been -- It is (T. Kimoto, et al., J.Appl. Phys.81 (1997) 3494 - 3500).

00846 H 1 = 1. 3 3 m e V

00856H2 = 6. 56 m e V

0086Since 6H of energies change with fields in this way 3 = 2.34 me V, the speed at which a terrace spreads differs. namely, terrace 'and Ho [ that the surface free energy of each field is high ] Growth rate is quick -- Drawing 8 (a) and Drawing 8 (b) and a figure -- 8 it is shown in (c) -- as -- Step hunching occurs every three cycles. in this embodiment, it has come out from the step side by the difference in a lamination cycle (ABC or AC B) -- un--- the number of joint hands differs every other step -- uncombined hand which has come out from this step end By the difference in a number, step punching breaks out further per three molecules. It thinks. Uncombined hand which has come out of the forward speed of one step, and a step By one place, it is late and it is thought in two places that it is quick. Thus, in 6 H-S i C, it is step Banchin at the height unit of the half-integral multiple of a grating constant. Quantity to which, as for the progress and growth back and the surface of single crystal S i C, A made three molecular layers the minimum unit It is thought that it is covered on the step of To and a flat terrace.

0087Like, single crystal S i C concerning the present invention, and the step which were explained above The terrace is formed of bunching. Therefore, step It concentrates near the end of single crystal S i C, and comes to be formed. mentioning above It was figure 6 (a) and Drawing 6 (b) and a figure -- 7 (a) and a figure -- 7 (b) and step portion In order to observe, the end portion of single crystal S i C is observed.

0088Single crystal S i C obtained by the thermal treatment equipment in this embodiment the growth temperature -- the range more than 1400 degrees of abbreviation C, and below 2300 degreeC, and the former -- single -- compared with the liquid phase growth temperature of crystal S i C, it is very high -- again -- a short time -- abbreviation 14 It can heat in the range more than 00"C and below 2300 degreeC. S i Fusion which will be formed between single crystal S i C and many crystals S i C used as a seed crystal if growth temperature goes up The dissolution concentration of C to the inside of liquid increases. It is among S i Melt in the rise of temperature. It is thought that diffusion of C becomes large. Thus, the source of supply and kind of C Quick growth called about 500 Mm/h r since the crystal is very close According to conditions, it also becomes possible to consider it as speed. Thus, single crystal S i C and the surface micro pie concerning this embodiment The densities of a A defect are 1/c m.²It is the following and is about 1. Broad terrace 0 / more than m They are surface treatments, such as machining, after single crystal S i C formation since it is formed. It becomes unnecessary. Since there are few crystal defects etc., it becomes possible to use it as a light emitting diode and various semiconductor diodes. in addition, growth of crystal -- temperature (it does not This dependence -- since it is dependent on surface energy 1 of the crystal of the source of supply of seed crystal And C, the necessity for the strict temperature control in a processing furnace is lost [ ] -- things -- large reduction-ization of power and manufacture Kos A is attained.) seed crystal An interval with many crystals S i C which are the sources of supply of single crystals S i C and C is extraordinary. small To -- the heat convection at the time of the heat treatment from things can be controlled. Seed It is Warm among many crystals S i C which are the sources of supply of single crystals S i C and C used as Crystal. Since a degree difference is hard to be formed, it can heat-treat by a thermal equilibrium state. as [ mentioned / above ] -- the crystal growth of single crystal S i C, and the plane direction on the surface of a crystal -- Along Since intermediary growth is carried out, provide a temperature gradient in the plane direction of an airtight container. it is -- This which gives directivity to low !/and a direction for the growth direction of a crystal from the one where temperature is higher It comes to be able to do. Heater 1 formed in the temperature gradient and heat chamber 2 Sai located in the side wall side of airtight container 5 of 1 De Heita 1 Difference in temperature between 1 b Methods, such as providing, can be illustrated. this time, it is control about the size of a temperature gradient by carrying out, the growth rate of a crystal is controllable -- the crystal surface It becomes possible to control generation of a fine crystal grain community.

0089Although 6 H--S i C was used as a seed crystal in this embodiment, it is also possible to use 4 H - S i C.

0090in addition -- although S i was used as a seed crystal (0 0 0 1) in this embodiment -- for example, -- etc. (1 1 -- 2 0) etc. -- it is also good to use the thing of other plane directions It is ability.

0091comparing that a surface plane direction (0 0 0 1) is a S i side with other crystal faces surface energy is low -- therefore, the nucleation energy under growth becomes high -- it is hard to carry out nucleation. It can do with single crystal S i C with wide terrace width after the liquid phase growth from the above reason. in addition -- being limited to a surface plane direction (0001) and a S i side it is not To -- it is possible to use all the crystal faces of 4 H--S i C and 6 H-S i C.

0092What the size of the multi-crystal S i C board used as the source of supply of single crystals S i C and C used as single crystal S i C concerning the present invention and a seed crystal is suitably chosen for The size of single crystal S i C by which intermediary formation is carried out is controllable. distortion is formed between single crystal S i C and the seed crystal which are formed -- things -- it hurts -- since it can do with single crystal S i C of the very smooth surface, applying as a surface property modification film is also possible.

0093What many crystals S i C which are the sources of supply of single crystals S i C and C used as a seed crystal are arranged in lamination or horizontally by turns, and is heat-treated by the above-mentioned method It is also possible to manufacture a lot of single crystals S i C simultaneously. With the manufacturing method of single crystal S i C concerning the present invention, Multi-crystal S i C board And or [ adding the impurities of III fellows metal, such as A 1 or B, beforehand in metal S i ], It is Growth conclusion by sending in the gas containing the element which controls the conducted type of S i C, such as nitrogen, A 1, or B, into the atmosphere under growth. It is possible to control arbitrarily p type of Crystal and an n type conducted type.

0094next, other suitable thermal treatment equipments to enforce the heat treating method of the present invention are started an embodiment -- a figure -- 9 (a) and Drawing 9 (b) thru/or a figure -- it explains, referring to 15. Drawing 9 (a) and Drawing 9 It is suitable to enforce the heat treating method of (b) and the present invention. It is a sectional view of the principal part of other embodiments concerning thermal treatment equipment.

0095Drawing 9 (a) and Drawing 9 as [ show / in (b) ] -- thermal treatment equipment concerning this embodiment It has high temperature heating furnace 50. The above-mentioned high temperature heating furnace 50, the main heating tub 51, and preliminary heating tub 52, it is a free passage about these main heating tubs 51 and preliminary heating tub 52 And vacuum valve 5 whose separation is enabled 9 and sample 5 which is processed materials 6 -- this , -- the main heating tub 5 1 and preliminary heating tub 5 Jigging which can move between two Lifting table 5 7 is constituted as the principal part. The main heating tub 5 1 And reserve heating tub 5 In two, it is high melting point metal main heating heater 5, respectively. 3, reserve Heating heater 5 4 is provided.

0096The main heating tub 5 In one, it is high melting point metal main heating heater 5. Heating by 3 High melting point metal light reflector 5 which makes it possible to carry out efficiently 5 is provided. It is. preliminary heating tub 5 the inside of two -- adsorption trap 5 8 is provided -- preliminary heating tub 5 Make it possible to maintain the pressure in two to predetermined pressure. To.

0097(The heating unit, i.e., above-mentioned heating heater 5, of the above-mentioned main heating tub 3) high-melting point it consists of metal -- although not illustrated -- the cylindrical main heater and planate auxiliary heater from -- becoming heating control of these two heaters and change of a sample position the inside of the improvement in uniformity of heating of the temperature in the Soaking field of an intermediary and the shape of a disk, and a disk-like heating field -- It is possible to provide a temperature gradient in the field inboard to kick.

0098The main heating tub 5 1 And preliminary heating tub 5 Above-mentioned Addition, the source of heating, i.e., the heater, in two and, In the keeping-warm material which takes and rolls a heat source, use of the graphite leading to the generation of gas it avoids -- Tha of a high melting point metal with little gas adsorption as a heating element and a light reflector for keeping warm Tungsten (W) is mainly used.

0099the thermal treatment equipment concerning this embodiment -- first -- preliminary heating tub 5 2 -- sample 5 6 if installed -- preliminary heating tub 5 Vacuum pump which 2 does not illustrate from atmospheric pressure While being exhausted by the intermediary vacuum the gas and sample 5 which stuck to sample 56 6 -- Built-in the Depart gas of To gas sake -- preliminary heating heater 5 4 -- room temperature to abbreviation 8 0 it is heated by 0 °C -- gas with built-in absorption gas And -- the outside of a tub -- a vacuum pump -- Drain Mind is carried out.

0100in order to heat quickly [ short time ] as a source of heating of the above-mentioned preliminary heating tub -- it has a reflector for condensing near-infrared rays in a sample -- halogen and X e run Infrared heat which added the infrared generating functional film to the tare external surface of A or a lamp a lamp -- To be fisted.

0101and sample 5 vacuum exhaust air is heated and carried out beforehand the end back of Depart gas of 6 -- purification The main heating tub 5 currently held under high temperature (refer to figure 9 (b)) moved to 1 within 1 minute. Movement is faced and it is vacuum valve 5. They are a difference and lifting table 5 about 9. It carries out by raising 7. The main heating tub 5 1 is always abbreviation 1. 0 --³P Introduce inactive gas of some once reaching [ the high vacuum of the pressure below a, or ] a high vacuum, and it is about 1 (T).²P the bottom of the thin gas atmosphere set as a -- abbreviation 8 0 More than 0 °C, preferably abbreviation 1 8 0 more than 0 °C -- 2 6 0 within the limits below 0 °C -- predetermined -- high -- It is always maintained by Warm.

0102(The temperature range of the above-mentioned main heating tub, for example, liquid phase A of single crystal silicon carbide, In the cases of the heat treatment in the Pitaxial growing-up method, etc.) Abbreviation 1 2 0 More than 0 °C is 2. 3 0 It is abbreviation 1 still more preferably with preferred it being a range below 0 °C. 4 0 More than 0 °C is 2. 3 0 It is a range below 0 °C.

0103subsequently, sample 5 The main heating tub 5 of 6 The end back of a move to 1, and sample 5 6 -- abbreviation 1 2 0 more than 0 °C -- 26 0 High temperature predetermined by within the limits below 0 °C, i.e., sample 5, 6 -- the maximum -- It attains promptly to proper place Temperature. and the main heating tub 5 1 -- beforehand -- heating -- For a Being done reason, a uniform high temperature condition is maintainable between required processing time. To. High-melting reflective metal plate 5 Since 5 is provided, it is heat radiation. The and sample 5 6 can be heated efficiently.

0104above-mentioned main heating tub 5 it consists of a high melting point metal, the heating unit, i.e., the heater, of 1, -- cylindrical It consists of the main heater and a planate Assistance heater.

0105The wavelength energy which W heater emits is expressed by the following formula.

0106wavelength energy of the spectrum radiation rate X ideal black body of wavelength energy =W of W in addition -- the wavelength energy of an ideal black body -- from the radiation rule of P 1 a n k -- easy -- Request -- To -- it is possible.

0107Drawing 1 It is a figure of 0, the spectrum radiation rate of W, and reflectance. Spectrum radiation rate in a figure It computed from the lower type indicated to literature 'The Science Of Incandescence' Dr. Milan R. Vukcevich. '

0108epsilon -- [ -- T] = a *lambda -b [lambda, T] {(tau 1 1 6 0 0) /1 0 0 0} -- here -- epsilon : A radiation rate and lambda : It was considered as wavelength [mupiiota] and tau:temperature [kappa].

0109Drawing 1 About the reflectance in zero, it is Kirchhoff's law of a lower type. It computed.

0110'R = 1 -- epsilon

0111here -- R:reflectance,_epsilon: It was considered as the radiation rate.

0112high temperature region 1 of W by the radiation rule of rho 1 a n k 8 0 more than 0"C -- 2 6 0 the wavelength energetics below 0 °C -- a figure -- 1 It is shown in 1.

0113Drawing 1 High temperature region 1 of result of 1 to W 8 0 More than 0"C is 2. 6 0 Below 0"C Wavelength energy, 1. It has a peak between below or more [ 0^ ] 1111. 5 mupiiota, and is 0.4. It is Ho of wavelength energy between the wavelength areas below or more 1113. 5 mu*eta. It turns out that But is contained. That is, it is [ in / more than wavelength abbreviation 0. 4 mu m / below / 3. 5 mu piiota ] quantity! The reflective material which has /and the reflective characteristic is the quantity of the sample of the furnace inside of the body. Efficiency heating is enabled.

0114In this temperature range, an usable metal and a compound are examples some. It was shown in Table 1.

0115[table 1]<img file="WO2004088734A1_D0001.tif" />

0116The treatment temperature of the above-mentioned main heating tub is abbreviation 1 considering these as reference. 2 0 More than 0"C is 2. 6 0 High temperature addition of the high purity atmosphere set as a predetermined temperature of the range below 0"C It is an heat furnace, The exothermic part of a high temperature furnace is a high temperature territory from the high melting point metal of W or T a. A region is taken and rolled, the component of a thermal reflex and a keeping-warm field -- inside of W, T a, and Mo from -- having compound structure which consists of a selected high melting point metal material The luminescence wavelength area of an exothermic part is reflected in the surface of the high melting point metal of the component of a heat interception field. The wavelengths of more than abbreviation 0. 4 mum are the arbitrary wavelength areas in the range below abbreviation 3. 5 mu m. The infrared reflection film is formed.

0117W And T a was mainly concerned with the infrared area for being concrete and W as a heater. A wavelength is abbreviation 0. It used as a light reflector below 3. 5 muiotataualpha above.

0118Drawing 1 peak of the wavelength energy of W radiation [ in / from 1 / 2200 degreeC ] about -- it is 1. 1 mu m, and the reflectance of W at this time is abbreviation 0.65. More than abbreviation 1.1 mu m with comparatively high wavelength energy is Area below 3. 0 mu m. Reflectance increases and it sets it to 3.omicronmuetaiota as a wavelength becomes long in a region. It amounts to 0.8. That is, it can be said that the reflective characteristic of W is enough as a light reflector of W To 1 Tarr in a pure high purity atmosphere.

0119W heater from the related characteristic of the radiation rate under the high temperature of W of Drawing 10, and reflectance and a sample is taken and rolled -- the example of a design of metal light reflector 55 -- a table -- it is shown in 2. An enclosure and the interval of each light reflector 55 are abbreviation 3 mm in the state of sealing about each light reflector 55, heater 53, and sample 56. ' -- again -- high melting point metal light reflector 55 the example of composition of the high heat-resistant metal oxide formed upwards and an infrared reflection film -- a table -- it is shown in 3.

01202]

0121Nine-layer type Ta/Ta/Ta/Ta/Mo/Mo/Mo/Mo/Mo

012211-layer type W/W/W/W/W/Mo/Mo/Mo/Mo/Mo/Mo

0123[table 3] I* Warm region w metal light reflector +WC moderate temperature field Mo metal light reflector +Au -- here, It is a high melting point metal. W, the melting point -- abbreviation It is 3400 °C. M o is about 2620degreeC. WG raised by this embodiment as an example -- abbreviation 27 it is 20"C -- Au is abbreviation 1060degreeC. therefore, W top -- high-melting point good WC of There, a substrate, and familiarity is used -- comparatively low A u of the melting point was used on Mo. Common [ according / the reflectance of the near-infrared field of WC / to membrane formation conditions / smooth ] In the state of a field, it is comparatively high. A u in the field is high reflection more than reflectance abbreviation 95 %. Although it is material, since the melting point is low, it is in the second half from a moderate temperature field. (outside) On Mo Membranes were formed. To Drawing 12, it is 0.4 of 8 11 reflecting layers. Below or more 1113. 5 mu ** wavelength The part light reflex characteristic in a field is shown.

0124Thus, in this embodiment, the heater part of the above-mentioned main heating tub is taken, and it is Roll. The keeping-warm field which comprises a High melting point metal plate, It consists of a keeping-warm layer and a Heat wire reflecting layer. It has compound structure and has a function in which each class carries out high temperature maintenance and Heat wire reflection, The high melting point metal board surface which constitutes a keeping-warm field is '-proof [ high ] pyrogenetic metallic carbide, such as WC, Ta C, Mo C, Z r C, H f C, and B N, Or it is that metal nitride is covered with independence or composite, degradation of a high melting point metal and modification -- Prevention it has Function to stop -- and the high melting point metal surface used as a Heat wire reflecting layer -- Au etc. being covered with an infrared reflection film -- example below or more about 0.43. 5 mu m It has the function for it to be efficient and to reflect the arbitrary luminescence wavelength areas of an enclosure.

0125The inside of a vacuum high temperature furnace consists of thermal treatment equipment concerning this embodiment, and a separated tub of the plurality of two or more tubs in this way, The insides of a tub of a plurality of are the main heating tub and Prediction. The gas and the trial which it comprised Heating tank and the above-mentioned preliminary heating tub mainly stuck to the sample It is heated by 800 degrees of abbreviation C from room temperature for the Depart gas of the gas built in a charge, Evacuation heating vacuum exhaust air is carried out beforehand the end back of A -- the above currently held under pure high temperature being promptly moved to the main heating tub -- the above-mentioned main heating tub -- always -- abbreviation 1 0 --³P It is [ the pressure below a, or ] abbreviation 1 once. 0 --³P some after reaching the pressure below a inactive gas is introduced -- atmospheric pressure to abbreviation 1 0 -³P The arbitrary pressure to a is thin. It is abbreviation 8 under a gas atmosphere. 0 More than 0 °C is 2. 6 0 It is always to high temperature at within the limits below 0 °C. It is heated, It is required in order to move a sample between the above-mentioned main heating tubs from the atmospheric pressure for receipts and payments of the above-mentioned preliminary heating tub of a sample, above-mentioned main heating tub it has a function which can be exhausted to equivalent pressure -- room temperature to abbreviation 8 0 the temperature of 0 °C -- sample Move to the above-mentioned main heating tub after carrying out preliminary heating early, a sample -- the maximum -- Proper place About management temperature 8 0 it is [ more than 0 °C ] desirable -- 1 2 0 more than 0 °C -- further -- good -- better To -- 1 8 0 more than 0 °C -- 2 6 0 temperature within the limits below 0 °C -- high temperature and high Purity atmosphere It has a high temperature heating furnace which attains The atmosphere promptly.

0126(The temperature range of the above-mentioned main heating tub, for example, liquid phase A of single crystal silicon carbide, In the cases of the heat treatment in the Pitaxial growing-up method, etc.) Abbreviation 1 2 0 More than 0 °C is 2. 3 0 It is abbreviation 1 still more preferably with a preferred range below 0 °C. 4 0 More than 0 °C is 2. 3 0 It is a range below 0 °C.

0127In order to heat quickly the thermal treatment equipment concerning this embodiment, and a sample, a vacuum high temperature furnace is divided into two, the main heating tub and a preliminary heating tub, -- and high purity Atmosphere In order to maintain The atmosphere, there is each interior of a room with each independent vacuum pumping system. it is -- being maintainable in each independent gas introduction system and atmospheric pressure atmosphere And the main heating tub and a preliminary heating tub are unification and separation by opening and closing of an interception valve. In the thermal treatment equipment which has the high-speed high temperature heating furnace currently maintained mutually, the above-mentioned main heating tub is always abbreviation 1 to civil time. 0 --³P Pressure below a, or once About 1 0 --³P Introduce the inactive gas of some after reaching the pressure below a, and it is abbreviation 1 from atmospheric pressure. 0 --³P It is abbreviation 8 under the thin gas atmosphere of the arbitrary pressure to a. 0 More than 0 °C It is abbreviation 1 preferably. 2 0 More than 0 °C is abbreviation 1 still more preferably. 8 0 0 ° Tooth Top 2 6 0 It is held by temperature within the limits below 0 °C at the high temperature condition, The above-mentioned reserve Beyond in abbreviation room temperature, a heating tub is 1. 0 State currently held at the temperature range below 0 o °c It sets, Cold tiger for adsorbing the built-in gas emitted from a sample etc. Urgency for A being built in and cooling from the high temperature after the end of heating promptly to room temperature It is the feature about having the high temperature heating furnace with which the gas circulation device for the colds is built in. It carries out.

0128The temperature range of the above-mentioned main heating tub, for example, liquid phase Epita of single crystal silicon carbide, In the cases of the heat treatment in the Quicar growing-up method, etc. About 1 2 0 More than 0 °C is 2. 3 0 The range below 0 °C is abbreviation 1 desirable still more preferably. 4 0 More than 0 °C is 2. 3 It is a range below 0 o °c.

0129thus, the thermal treatment equipment concerning this embodiment, the main heating tub, and a preliminary heating tub it divides -- dividing each work assignment clearly -- Leader of the optimal treatment temperature The high purity atmosphere in A heat bath is maintained and it enabled it to maintain the optimal processing conditions. Here, they are a preliminary heating tub and a sample 1 0_³P in the bottom of the pressure below a -- beforehand -- About 8 0 heating more than 0 °C -- removal and In the middle stage of out gas Temperature rising is performed. They are the main heating tub and a sample 1 0 --³P Below a In the bottom of pressure, it is the optimal treatment temperature, for example, 1, to a short time. 8 0 It heats more than 0 °C. It carries out.

0130straight line movement according to air starting in movement of the sample between the main heating tub and a preliminary heating tub or -- high-speed movement for less than 1 minute by circle movement by a motor drive is possible -- is there. It is the Tank dedicated the case where new gas discharge is in the main heating tub. By installing a vacuum pump with sufficient exhaust air capability of for, it is polluted gas. It is promptly removable to the tub exterior. Preliminary heating Auxiliary physical adsorption removal mechanisms, such as a cold trap, are put side by side in a tub. It is further The end about degradation of the heater formed in the main heating tub, a light reflector, etc. It can prevent to all.

0131The fault [ case of conventional thermal treatment equipment ] that the Soaking field of a sample is narrow and the temperature control of the area within Soaking territory is difficult, and heating atmosphere are high vacuums. (1 0 --)³P Impure gas mixes the bottom of the pressure below a, or the case of some rare gas atmosphere. There was a fault that maintenance of the high temperature region which is not was difficult. A lot of absorption gases which is emitted in the early stage of heating from a sample according to this embodiment, such as hydrogen, and built-in gas, it sets to a preliminary heating tub -- one by one -- heating (room temperature * 8 0 0 °G) exhaust air -- After Was done, rapid movement is carried out into the main heating tub of a high purity processing atmosphere -- further -- the heating optimal treatment area of a sample -- abbreviation 1 2 0 more than 0 °C -- 2 6 0 Time of being the high temperature below 0 °C To beforehand -- the main heating tub -- abbreviation 8 0 more than 0 °C -- 2 6 0 Preheat below to 0 °C. there is nothing to the former -- a high speed -- uniform heating is possible -- Noodle. ' -- the conventional heat The heat-treatment back and a sample are cooled to the work temperature near room temperature the case of a processing unit. although that took the long time, it sets to this device -- the inside of a preliminary heating tub -- gas Cooling By building in Place, the forced cooling of the sample became possible.

0132Drawing 1 The embodiment of further others of the thermal treatment equipment applied to the present invention 3 is shown. This operation In a form, they are thermal treatment equipment and high temperature heating furnace 7. It has 0. Drawing 1 It is shown in 3. Preliminary heating tub 5 in this embodiment 2, a halogen lamp or mouth Heater 5 4 is provided -- rapid -- abbreviation 8 0 more than 0 °C -- 1 8 0 within the limits below 0 °C -- place the temperature of a law -- the lamp or mouth A heater type heating furnace which can be heated -- Being. '

0133reserve heat chamber 5 Cassette 6 which can load both the sides of 2 with multiple samples 0 is arranged and a processed sample is placed on processing before to one side, and another side -- cassette ON A trough 6 with which it has loaded 1 and reserve heat chamber 5 2 a -- vacuum valve 5 9 -- partition , -- Being done . The main heating tub 5 Heater 5 made into 1 with the high melting point metal Metal light reflector 5 which serves as a heater of 3, for example, the mesh state of W, from a high melting point metal It constitutes from 5. It is carried out.

0134High temperature heating furnace 7 Cassette loaded with multiple unsettled samples in 0 A 6 0 to samples 56 are a jig and lifting table 5. It is put on 7 and is preliminary heating. Tub 5 At 2, it is abbreviation 8. 0 It is beforehand heated more than 0 °C. On the other hand, it is the main heating tub beforehand. Abbreviation 8 0 More than 0 °C is 2. 6 It heats to a predetermined temperature within the limits below 0 .0 °C. Sample 5 by which preliminary heating was carried out 6 is reserve heat chamber 5. 2 and the main heating tub 5 Pressure tone of 1 As soon as Adjustment ends, Preliminary heating tub 5 2 and the main heating tub 5 Vacuum valve 5 between 1 9 opens and it is sample 5. 6, a jig, and lifting table 5 7 moves and it is the main heating tub 5. 1 About 8 0 More than 0 °C is 2. 6 0 It is processed at a predetermined temperature within the limits below 0 °C. At this embodiment, it is abbreviation 2. 0 0 It is processed by 0 °C.

0135The main heating tub 5 After processing is completed in 1, they are a jig and lifting table 5. 7 is Down. Ri and preliminary heating tub 5 Vacuum valve 5 between 2 and the main heating tub 1 9 closes. And cassette 6 which receives a heat-treated sample A sample is conveyed by 0. By repeating this, it is a processing furnace Using short time of a batch type, and is mass production nature. It turns out that improvement is remarkable.

0136the example of the heating temperature characteristic at this time -- a figure -- 1 It is shown in 4.

0137Drawing 1 Other embodiments of the thermal treatment equipment applied to the present invention 5 further again are shown. Book The thermal treatment equipment concerning an embodiment is high temperature heating furnace 8. It has 0. high temperature heating furnace 8 they are 0 and a continuation type heating furnace -- preliminary heating tub 5 The main heating tub 5 of plurality [ 2 ] 1 -- Establishment it is kicked -- preliminary heating tub 5 2 power Vacuum valve 5 9 -- each main heating tub 5 It is divided so that it may correspond to 1. according to such composition -- the main heating tub 5 the preset temperature of 1 -- each [ each ] -- embracing different Lazar and each process -- each main heating tub 5 processing by 1 -- sample 5 It is possible to give continuously a heat history which is different in 6. It becomes. it compares with batch processing -- the improvement in mass production nature becomes remarkable.

0138Thermal treatment equipment explained in all the above-mentioned embodiments and Above It is limited only to operation of the heat treatment method in the liquid phase growing-up method of single crystal S i C. Use is not carried out.

0139a short time -- abbreviation 8 0 more than 0 °C -- 2 6 0 the range below 0 °C -- desirable 1 2 0 More Than 0 °C -- 23 0 Use the Feature Heated to Predetermined Temperature of Range below 0 °C. this Device after Pouring Ion into The, for Example, Semiconductor Substrate Surface, -- Short -- Time, It is an effect certainly [ portion / which poured in ion by heating to high temperature ]. It becomes possible to crystallize with a sufficient rate. Heat treatment concerning this embodiment They are others, such as ion implantation equipment, a device and since [ being small and since structure is comparatively simple ]. Connection to a device can be performed easily.

0140They are the more nearly special ones, such as laser and plasma, the case where high-speed heating is performed conventionally. The method was used. however, the thermal treatment equipment concerning this embodiment and structure while it is simple -- other devices, for example, an electron microscope and ion implantation equipment, etc. -- connecting is possible. for this reason, it obtains in the conventional method -- it has A cut new material may be able to be created.

0141It is a from book although indicated to the present invention and the above-mentioned desirable embodiment. Ming is not restricted only to it. deviating from the soul and the range of the present invention It should be understood that various examples of an embodiment which are not can otherwise be made. obtaining -- .