Production of high-purity titanium oxide film

[Detailed Description of the Invention]

Field of the Invention The present invention relates to the manufacturing process of a high purity titanium oxide film. Conventional technology As a manufacturing process of conventional titanium hydroxide or titanium oxide, titanium salt, such as a titanium chloride, titanium sulfate, or alkoxy titanium, is used for materials, and combined use of the method of hydrolyzing, the method of oxidizing, or both is known. According to these methods, at the place of generation of titanium hydroxide or titanium oxide, either the ingredient leading to non-purity, i.e., sulfuric acid, chloride, chlorine or alcohol exists. Therefore, these substances were taken into output and made titanium hydroxide or titanium oxide impure. After dissolving alkoxy titanium in nonaqueous solvents, such as alcohol, considering it as solution as a method of forming a titanium oxide film and making this adhere on a solid, the method of making it follow hydrolysis gradually and forming a film with moisture, in the atmosphere of low humidity, is known. However, there was a fault from which the fixity for Alkyl consists large of, therefore the amount of organicity remains in a film, and the thing which has a big Alkyl machine, and which needs to use the big thing of a Alkyl machine in order to make a hydrolysis rate moderate according to this method serves as an impure titanium oxide film. The object of an invention The present invention cancels the fault in the conventional method, and it is providing the method the titanium oxide film of very high purity [ object / the ] which went to accumulate being manufactured easily. Constitution of an invention It is air-dried after making Viscous liquid which made hydrogen peroxide-ized titanium solution, hydrogen peroxide-ized alkoxy titanium solution, or Cough solution condense adhere on a solid as a result of inquiring, in order that these artificers may achieve the above-mentioned object, When the acid film was heated at the last which forms a solid film more than 450 degreeC, it has studied that a high purity titanium oxide film was obtained easily. The present invention was completed based on this knowledge. The gist of the present invention After making Viscous liquid which made Viscous liquid which made hydrogen peroxide-ized titanium solution condense thru/or the shape of jelly, or hydrogen peroxide-ized alkoxy titanium solution condense thru/or jelly-like liquid adhere on a solid, It is a manufacturing process of the high purity titanium oxide film making it dry, forming a solid film and Temperature rising(ing) an acid film gradually more than 450 degreeC. Introduction hydrogen peroxide-ized titanium solution is manufactured with either of the three following methods. When one makes the dissolution reaction of titanium hydride and hydrogen peroxide solution cause, titanium hydride has a catalytic action in the decomposition reaction of hydrogen peroxide, and the condensation reaction of hydrogen peroxide-ized titanium solution which arose previously, and promotes a re-reaction. In order to give priority to a dissolution reaction promptly, it is required to grind the massive titanium hydride which can usually be obtained under non-oxidizing atmosphere (for example, underwater), and to use it as fine powder. Although it can dissolve with 1% or more of hydrogen peroxide, a rate of solution becomes early, so that concentration is high. the alcohol which the alkoxy titanium which uses two by the present invention is replaced by hydrogen oxide water, and is generated -- volatility -- Rich -- things are preferred -- for example, methoxy titanium. There are ethoxy titanium and propoxytitanium. However, large [ they ] carbon number alkoxy titanium does not interfere by a case, either. Alkoxy titanium is mixed to pure hydrogen peroxide solution, a dissolution reaction is caused, and hydrogen peroxide-ized alkoxy titanium solution is manufactured. What has the concentration of hydrogen peroxide higher in order to avoid hydrolysis of alkoxy titanium by moisture in hydrogen peroxide solution at this time is more desirable, and it is 0.1% or more. Below 50''C cooling with ice water preferably, in order to suppress the rise in heat by reaction fever, since disassembly of hydrogen peroxide solution and hydrogen peroxide-ized alkoxy titanium will take place if it becomes about 30% and high temperature preferably, pure hydrogen peroxide solution is mixed and to dissolve is required. If the hydrogen peroxide-ized alkoxy titanium solution obtained by this method is decompressed for example, with an oil rotation pump to 10-2 thru/or 10-3torr, It is replaced by hydrogen peroxide, distillation removal of the ,, such as separated ketone or aldehyde of an oxidation product of alcohol and the alcohol of certain quantity, is carried out with water and the hydrogen peroxide of isolation, and pure hydrogen peroxide-ized titanium solution is manufactured. Although hydrogen peroxide-ized alkoxy titanium solution and hydrogen peroxide-ized titanium solution which were obtained are semi- stability under coldness and warmth, they disassemble the hydrogen peroxide of isolation into the beginning, and emit a lot of oxygen gas. High hydrogen peroxide-ized titanium changes to low hydrogen peroxide-ized titanium simultaneously, and the mandarin orange color of a color tone becomes thin with time, and condensation of low hydrogen peroxide-ized titanium takes place continuously, the degree of condensation is increased gradually, it goes, Viscosity increases and goes, and it becomes jelly-like. Generally, under the degree of room temperature, this state continues over several hours from for several minutes in [ several hours to ] several days or under 100 degreeC. Viscous liquid is made to adhere on a solid. Or hydrogen peroxide-ized alkoxy titanium solution and hydrogen peroxide-ized titanium solution are made to adhere on a solid. Then, if it may Viscous-ize and this tunic in which a uniform solid tunic will be formed if this is air-dried under normal temperature is gradually Temperature rising(ed) more than 450 degreeC, an amorphous titanium oxide film will be obtained. If it heats more than 600 more degreeC, it will become a titanium oxide film of crystalline material. EFFECT OF THE INVENTION Since according to the method of the present invention any elements other than titanium, hydrogen, and oxygen are not included in order to use hydrogen peroxide-ized titanium solution or the condensation thing of This place as a manufacturing raw material of a high purity titanium oxide film, Since what is necessary is just unlike the conventional method not to add an additive to the materials and to merely decompose thermally, moreover it does not generate impurities from the materials themselves, mixing of impurities is avoided and the titanium oxide film of Iron purity is obtained extremely. Materials are water and handling is also simple for them. If content for the carbon of small quantity is allowed into titanium oxide, hydrogen peroxide-ized alkoxy titanium solution using ethoxy titanium, small alkoxy titanium, i.e., methoxy titanium, of a molecular weight, and propoxytitanium can be used as it is. Example 1 While putting 2 g of tetraisopropoxy titanium into a beaker, dipping this beaker into ice water and cooling, 8 ml of 30% quantity purity hydrogen peroxide solution is added on it, and after agitating gradually to make hydrogen peroxide-ized isopropoxy titanium solution of a uniform mandarin orange color, pure water 500 ml is added and diluted to this, As it filtered just to make sure and there was nothing about an undissolved thing, this solution was put into the glass container of a flat bottom at the 5CI11 depth, and it was neglected to the interior of a room under normal temperature, and the film of yellow 5■/cd was slightly manufactured by advancing condensation of steam of water, and Solute gradually. This film was removed from the glass container of the flat bottom, and in the air, it Temperature rising(ed) to 700degreeC at the rate of 5 degree/m C, and obtained the colorless Anatase type titanium oxide film. Example 2 It Crushing in a mortar, dipping massive titanium hydride with a small amount of water, and titanium hydride of the fine powder 47■ is added to the 30% quantity purity hydrogen peroxide solution of 1 10 m, and it mixes, After a while, after having dissolved, obtaining yellow hydrogen peroxide titanium solution and diluting this liquid with pure water 100 ml, this solution was put into the glass container of a flat bottom at the 2CIL1 depth, it was neglected to the interior of a room under normal temperature, and the light yellow film was slightly manufactured by advancing evaporation of water, and condensation of Solute gradually. This film was removed from the glass container of the flat bottom, and in the air, it Temperature rising(ed) to 700degreeC at the rate of 5 degree/m C, and obtained the colorless Anatase type titanium oxide film. Written amendment It will be moon 27 day about Showa 62. The Showa 61 patent application No. [ two ] 93580, the title of an invention Manufacturing process 3 of a high purity titanium oxide film, those that do amendment Relation with an incident Applicant for a patent 5, the number of the inventions which increase by amendment It makes and they are column 7 of the detailed description of the invention of 6 and the object specification of amendment, and the contents of amendment. The passage of an attached sheet Attached sheet (1) The 2nd page specification "sulfuric acid and chloride" of two lines "sulfate. It corrects with a chloride." (2) Correct the 2nd page of 12 lines, and 13 lines "Alkyl machine" with an "alkoxyl group." (3) Correct the 2nd page "part for Alkyl" of 13 lines with "alcohol." (4) Correct the 3rd page "acid liquid" of four lines with "this both liquid." (5) Correct the 3rd page "based" of nine lines, saying "be based." (6) Correct the 3rd page The end line "hydrogen peroxide solution" with "hydrogen-peroxide-solution solution." (7) Correct the 4th page "hydrogen peroxide-ized titanium solution" of two lines with "hydrogen peroxide-ized titanium." (8) Correct the 4th page "1%" of seven lines with "0.1%." (9) Correct the 4th page "hydrogen oxide water" of nine lines with "hydrogen peroxide." (10) Correct the 4th page "Is" of ten lines with "But." (11) Correct the 4th page "large" of 13 lines, saying "Size becomes." (12) Correct the 4th page "pure hydrogen peroxide solution" of the 15th line with "hydrogen-peroxide-solution solution." (13) Correct four lines "hydrogen peroxide solution" with "hydrogen-peroxide-solution solution" from 4th right under [ the ]. (14) said -- the 5th -- page 1 line~2 line "hydrogen water -- and ...... since he is absorbed -- " -- correct as follows. "since disassembly of hydrogen and hydrogen peroxide-ized alkoxy titanium takes place" violently (15) -- said -- four lines of page [ 5th ] "pure hydrogen peroxide solution" are corrected with "hydrogen-peroxide-solution solution." (16) Delete the 5th page "pure" of 11 lines. (17) Insert the following sentence in the 5th page of 12 lines, and 13 spacing. The next of six lines "it is" is joined "above room temperature" from 5th right under [ (18) "which there are various purity articles in this although commercial item may be sufficient as hydrogen-peroxide-solution solution used by the present invention, and is not restricted to this although it is highest purity article in which stabilizer is not most preferably contained" said ]. (19) said -- five lines of page [ 6th ] -- ""and " -- or " -- correct. (20) Join the next of seven lines "as materials" in "of" from 6th right under [ the ]. (21) Delete six lines "Is" from 6th right under [ the ]. (22) Correct three lines "additive" with a "decomposition agent" from 6th right under [ the ]. (23) Correct the 7th page "hydrogen water" of 11 lines with "hydrogen water solution." (24) Correct five lines "steam" the bottom of [evaporation from under the 7th page. (25) Correct the 8th page "hydrogen peroxide solution" of five lines with "hydrogen-peroxide-solution solution." (26) Correct the 8th page "hydrogen" of seven lines with "hydrogenation."