CN1206418A - Method of producing organo indium chlorides - Google Patents
Method of producing organo indium chlorides Download PDFInfo
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- CN1206418A CN1206418A CN 97191495 CN97191495A CN1206418A CN 1206418 A CN1206418 A CN 1206418A CN 97191495 CN97191495 CN 97191495 CN 97191495 A CN97191495 A CN 97191495A CN 1206418 A CN1206418 A CN 1206418A
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Abstract
A method for producing organo metal chlorides directly from molten metal. The organo metal chlorides are formed by contacting an organo chloride directly with a metal melt. The preferred method includes the use of indium as the metal and methyl chloride as the organo chloride. The direct contact of the methyl chloride with the indium metal results in the production of dimethyl indium chloride or methyl indium dichloride depending on the contacting time and efficiency of the process. The resulting products are suitable for use as a precursor gas for chemical vapor deposition processes. Additionally, activator compounds such as oxides or halides are optionally added to the metal melt to enhance the reaction rate.
Description
Background
1. Field of the invention
The present invention relates to a process for producing organo-metal chlorides directly from molten metal. More particularly, the invention relates to a method for producing organo indium chlorides by contacting an organo chloride with molten metallic indium to form an organo indium chloride. Direct contact of the organo chloride with the indium metal melt results in the production of an organo indium chloride or organo indium dichloride depending on the contact time and process efficiency. In addition, an activator compound is optionally added to the molten metal to increase the reaction rate. Gallium metal is also suitable for use in the process of the invention to form organo gallium chlorides.
2. Brief description of the related Art
Organo-metal chlorides are organometallic compounds that decompose under the conditions of the pyrolysis reaction. This decomposition allows the use of these compounds as metal sources in chemical vapor deposition processes. Thus, organo-metal chlorides, particularly organo-indium chlorides, are expected to be useful as precursors in chemical vapor deposition processes for films or coatings that are coated with metal oxides or doped with metal oxides on substrates. In addition, the deposition or doping of indium oxide coatings using organo indium chlorides as precursors is faster than other conventional indium precursors. Higher deposition rates are desirable for applying coatings to substrates such as continuous glass ribbons in a float glass production process. Higher deposition rates produce thicker coatings on the substrate, which correspondingly improves the energy attenuation properties of the coated article.
Conventional methods for producing organo indium chlorides generally involve ligand exchange or alkylation of the indium compound to form the desired organo indium chloride. The described techniques require the use of solvents or pyrophoric compounds, which results in additional processing or separation steps to obtain the desired organo indium chlorides. In addition, the known techniques for producing organo indium chlorides require long reaction times. Handbooks of inorganic and organometallic chemistry Gmelin; indium, organo indium compound 1, 8 th edition; wolfgang Petz, Springer-Verlag, Berlin: 1991.
organo indium chlorides are produced by alkylating indium trioxide with an alkyllithium compound. This is the most commonly used step in the classical production of organo indium chlorides. The reaction is generally carried out in a solvent of diethyl ether, benzene or toluene, and is completed with stirring for 1 to 2 days. At the end of the reaction, the desired organic indium chloride is separated off by sublimation.
Another method for producing organo indium chlorides involves ligand exchange of indium trichloride and a pyrophoric compound, trialkyl indium. The reaction was carried out in ether, benzene or toluene, providing quantitative yields in less than 6 hours.
Furthermore, the metal organic chemistry Geoffrey Wilkinson is integrated; gordon a stone; edward w. able, Pergamon press, oxford, 1982, volI, chp.7 discloses that, in general, indium metal reacts slowly with alkyl bromides or alkyl iodides. The reaction rate is increased by using active metal lithium. The activation of the metal is accomplished by reacting indium trichloride and potassium in solution. The mixture was refluxed under nitrogen for 4-6 hours to finally obtain a dispersed ferrous metal powder. The powder reacts with the alkyl halide mentioned to form dialkyl indium bromide or iodide.
Therefore, known methods for producing organo indium chlorides require alkylation or coordination exchange processes. The reaction is carried out in a solvent, thus requiring additional work-up or separation steps to recover the desired organo indium chloride. Conventional methods also require long reaction times. The addition of an activator to the indium metal may also enhance the reaction process with the halide. However, conventional indium activators involve some compounds, which results in additional processing steps to increase the recovery of the desired organometallic halide.
It is advantageous to produce organo indium chlorides directly from indium metal using organo chlorides as the source of organic radicals. The direct synthesis of organo indium chlorides from metallic copper can eliminate the use of pyrophoric compounds or produce organo indium chlorides in a manner that does not require additional solvents and processing or separation techniques. Furthermore, it would be advantageous to develop a process that greatly reduces the reaction time required for conventional organo indium chloride production. The direct synthesis of organo indium chlorides from molten metallic indium can therefore improve the economics of producing this compound by known methods.
The use of activators in the molten indium metal during the direct synthesis of the organo indium chlorides is also advantageous. The activator will accelerate the reaction rate of the formation of organo indium chloride from molten indium.
A further advantage of using an activator is that the activator can be regenerated in the molten indium metal once the production of organo indium chloride has begun. Regeneration of the activator can increase the continuity of the reaction with the addition of fresh reactants and without the addition of additional activator.
Summary of The Invention
In accordance with the present invention, a novel process for the production of organo indium chlorides by direct contact of an organo chloride with molten metallic indium is provided. The organo chloride reacts with the indium metal melt to form organo indium chloride suitable for use as a precursor gas in a chemical vapor deposition process. This process results in the production of an organoindium chloride or organoindium dichloride.
The process of the invention is carried out in a reaction vessel containing molten metal. A vaporous organic source, such as methyl chloride, is introduced into the molten indium metal where the components react to form an organo indium chloride. The produced organic indium chloride compound is directly led out from the reactor and recovered. The type of organo indium chloride produced is related to the contact time of the organo chloride with the molten indium. For example, shorter contact times result in the formation of organoindium dichloride. Increasing the contact time will produce an organoindium chloride.
The reaction of the process of the present invention may be enhanced by adding an activator to the molten indium metal. The activator increases the reaction rate of the organochlorine and the indium metal. Suitable activators include various halides and oxides.
The invention aims to produce organic indium chloride by directly contacting organic chloride with molten metal indium. The direct synthesis of organo indium chlorides from molten indium allows recovery of the desired compounds without the use of solvents during the reaction and without the need for additional separation steps during the reaction. In addition, the process of the present invention uses abundant and non-pyrophoric reaction components.
It is another object of the present invention to provide a method for the direct synthesis of organo indium chlorides which reduces the reaction time experienced in known organo indium chloride formation processes. The duration of the reaction of the process of the invention is considerably reduced compared with the processes of the known prior art. Theorganic indium chloride can be continuously produced by reducing the reaction time.
It is also an object of the present invention to use activators in the production of organo indium chlorides from molten metallic indium. The activator increases the reaction rate of the indium metal and the organic chloride.
It is also an object of the present invention to use an activator that can be regenerated in molten indium. Regeneration of the activator facilitates continuous production of the desired organo indium chloride by increasing the rate of continuous introduction of organo chloride into the melt by adding limited amounts of the reactant indium metal.
Brief Description of Drawings
The above and other advantages of the present invention will become readily apparent to those skilled in the art from the following detailed description of the preferred embodiments, when taken in conjunction with the accompanying drawings. Wherein:
FIG. 1 is a schematic diagram of an experimental setup suitable for illustrating the process according to the invention according to examples I-IV and prediction example I.
FIG. 2 is a schematic diagram of an experimental setup suitable for carrying out the invention according to example V.
Description of The Preferred Embodiment
According to the method of the present invention, it was found that an organo indium chloride compound can be directly synthesized from a molten metal indium by directly contacting an organo chloride. The process generally utilizes a flow of an organo-chloride gas through molten indium metal wherein the components react to form the desired organo-indium chloride compound. The process is suitable for forming diorganoindium chloride or organoindium dichloride or mixtures thereof.
The method of the present invention contemplates the use of indium as the molten metal. The organo indium chloride compounds produced by the process of the present invention provide a suitable source of metal for forming indium oxide coatings. For example, indium is a metal that is desirable for use in forming metal oxides on glass substrates because it enhances the optical, electrical, and energy attenuation properties of the coated article. However, gallium metal is also suitable for use in the present process to form organo gallium chlorides.
The organic source utilized in the present invention is typically an organic chloride. The preferred compound is methyl chloride, used to form dimethylindium chloride or methylindium dichloride. In the process the methyl chloride is supplied as steam. The vapor phase reactant is typically passed through the molten indium metal in the reactor as a (bubbling) bubble. Other organo chlorides more reactive towards indium metal are also suitable for use in the present process to provide organo indium chloride compounds. For example, these organochlorides may include ethyl chloride, propyl chloride, neopentyl chloride, chloromethyltrimethylsilane, chlorotrifluoromethane, or chlorobenzene. Some organic chlorides are liquids at room temperature. Thus, conventional vaporization techniques can be used in the process of the present invention to convert the organic chloride into a suitable phase.
In addition, the organic source may include other organic halides, such as organic bromides or iodides. Although the compounds mentioned are more costly than the preferred organic chlorides, they are also suitable for forming organic indium halides according to the process of the invention. The organic groups in the organic halide may includegroups similar to those previously disclosed for use as a source of organic chloride.
In addition, hydrogen may be added to the organic chloride vapor as a reducing agent. Hydrogen accelerates the reduction of indium and organic chlorides, thus increasing the reaction rate. Hydrogen is present in the organic chloride in an amount of 5 to 60 mol%. The preferred hydrogen content in the mixed organic chloride/hydrogen vapor is 10 mole percent. The primary characteristics of the reducing agent are to react with the molten indium halide functionality to produce a volatile halide product and a lower oxidation state of the indium. Thus, reducing agents that are stronger than hydrogen are also suitable for use in the process of the present invention. For example, trimethylsilane, dichlorosilane, ethylene or acetylene can be used as reducing agent.
The indium metal melt reacts with the selected methyl chloride to form dimethyl indium chloride or methyl indium dichloride. The product formed is related to the contact time of the organic chloride and the metallic indium. Shorter contact times result in more methyl indium dichloride. Longer contact times produce more indium dimethyl chloride. Thus, the reaction between molten metallic indium and methyl chloride is represented as follows: or
In accordance with the present invention, an optional activator may be included in the molten indium metal to increase the reaction rate. Melting the activator with the metal helps to initiate the reaction between the metal and the organic chlorideShould be used. In general, the activator may include various halides or oxides. The halide may comprise Cl2，HCl，InCl3，(PtCl4)2-，PdCl2. The oxide activator comprises In2O3，TiO2，NiO2，Fe2O3. The activator functions to react with the indium metal to produce a less reactive indium species. Thus, other metal halides or metal oxides that form a lower indium species in the melt are also suitable for use in the present invention.
According to the process of the invention, the activator is preferably an indium-containing compound, such as InCl3Or In2O3. Indium-containing active agents are preferred because they regenerate upon melting. Thus, once the melt is formed, the reaction is initiated without the need to continue adding the additive.
The activator is melted directly with the indium metal to form a melt at a level of from about 5 mole% to about 50 mole%. Preferably, the activator component is about 10 mole%.
The inventors theorize the following with respect to chemical reactions that may occur. The inventors do not wish to be limited to this possible explanation, however, and are therefore presented only to assist in understanding the success of the process of the invention.
Upon heating of the indium metal and activator, a melt is formed. The inventors have proposed that indium metal reduces the halide or oxide upon heating to produce a lower valent indium compound (In)IOr InII) As follows: the reaction is carried out with an excess of indium and is generally carried out around the melting point (159 ℃) of indium. The inventors believe that at this point, MeCl/H2And a rather mild reaction occurs between the lower indium compound. The initial reaction may be MeCl spanning the metal InICentral oxidative addition (reaction) to produce methyl indium dichloride, which undergoes the following transformation to [ InMe2][InCl4]： Upon heating, [ InMe]2][InCl4]The complex can be decomposed into dimethylchlorinesIndium and InCl3. Then, InCl3Reactive lower groups that can react with excess indium to reform reaction are shown below:
in practice, the process of the invention is carried out in a conventional reaction vessel in which molten indium is formed and the organochloride is contacted with the melt. The vapor phase of the organochloride is generally introduced at the bottom of the vessel and bubbled through the melt to allow the reaction of the invention to occur. However, other conventional methods of vapor/liquid contacting may be suitable for carrying out the process of the present invention.
For continuous production of the organo indium chloride, the vessel must also be provided with a suitable device for extracting the organo indium chloride produced, thus enabling continuous production of the desired compound. Then the organic indium chloride is recovered from the container along the flowing direction. Furthermore, for continuous production, the vessel must have an inlet device for the introduction of the additional indium metal, which is the limiting reactant in the process of the invention.
The preferred process of the invention begins in a reaction vessel where indium and activator are heated to form a red indium metal melt. This red liquid is typically formed at around 240 ℃. The melt is typically maintained at a temperature of between about 240 ℃ and about 350 ℃ during the reaction, preferably between about 280 ℃ and about 300 ℃.
Upon formation of the melt, the preferred methyl chloride and optionally hydrogen are bubbled through the melt, wherein the reaction of the present invention takes place. The contact time of the steam and the melt influences the form of the organic indium chloride produced. The contact time is not more than 0.5 second to prepare the monomethyl indium dichloride. The contact time of 10 seconds or more produces dimethyl indium chloride. Contact times between the two will produce an organo indium chloride mixture.
The recovery of the organo indium chloride is carried out downstream of the reaction vessel. The organo indium chloride is preferably recovered in the vapour phase. However, system limitations related to a given recovery method and apparatus can lead to condensation and further solidification of the desired organo indium chloride product. Conventional recovery equipment or vessels are suitable for use in the practice of the present invention. Alternatively, argon or other inert gas may be used to carry or bring the desired organo indium chloride to a recovery vessel.
In addition, recovery of the organo indium chloride can be improved by dissolving the organo indium chloride in a polar aprotic solvent. For example, ethyl acetate may be used as a solvent to carry solidified organo indium chloride from a recovery vessel. Moreover, polar, aprotic solvents are suitable for use in transporting organo indium chlorides to vaporizers in chemical vapor deposition processes. Thus, the use of a polar, aprotic solvent not only aids in the recovery and collection of the desired organo indium chloride, but also places the materials used in the chemical vapor deposition process in a desired form.
The organo indium chlorides obtained from the process of the present invention are suitable for use as precursor gases for overlying or doped indium oxide coatings by conventional chemical vapor deposition processes. Moreover, the use of dimethyl indium chloride greatly increases thedeposition rate of indium oxide coatings over other known indium precursor gases. For example, with dimethylindium chloride, the deposition rate is on the order of 800 angstroms/second, while with other known indium precursor gases, it is 20 angstroms/second. In a float glass production process, higher deposition rates lead to thicker coatings on the substrate. A thicker coating phase layer improves the optical, electrical and energy attenuation properties of the coated article.
The following examples, which are included to best explain the best modes contemplated by the inventors for carrying out the invention, are presented for the purpose of further illustration and disclosure and are not to be construed as limitations of the invention.
Example I
FIG. 1 depicts a 0.500L round bottom flask 12 for use as a laboratory scale reaction vessel 10 for carrying out the process of the present invention. The bottom of the flask is provided with a 2.5 cm diameter elbow 14 which contains a 1 cm thick frit 16 of fritted glass. The bent tube portion 14 at the bottom of the flask 12 is connected to a gas inlet tube 18. The upper portion of flask 12 has two narrow neck openings 20 and 22. A narrow neck 20 serves as a gas outlet 26. The second opening 22 is covered with a rubber plate 24. About 40 grams of indium metal and 3.5 grams of indium trichloride are added to the reactor 10 at the glass frit 16. The reactor is equipped with a water cooled condenser 28 having an inlet 30 and an outlet 32 at the other end. The condenser 28 is connected to the gas outlet 26 of the reactor 10. The thermometer 34 is in contact with the glass frit 16 through the rubber plate 24. An oil bubbler (not shown) was piped to the condenser overhead gas outlet 32 to detect the flow of gas out of the reactor 10. Another bubbler (not shown) is connected to a gas supply at the bottom gas inlet line 18 of the reactor 10. A gas inlet pipe 18 is used to convey the organic chloride to the reactor 10.
The lower half of the reactor 10 is placed on a sand bath 36 with a sand level about 5 cm above the glass frit 16. The sand bath temperature is controlled to maintain the desired melting temperature. The indium metal and indium trichloride melt 38 is heated to a temperature above the melting point of indium metal to 240 c, during which the indium and indium trichloride react to produce a red liquid. Methyl chloride and another argon hydrogen mixture containing 5% hydrogen enter reactor 10 through gas inlet tube 18. A stream of methyl chloride vapor is first introduced into the reactor and the gas is slowly bubbled through the melt 38. An equal amount of an argon stream containing 5% hydrogen was then added to the methyl chloride vapor stream.
After 5 minutes, white crystals began to grow in the cooler part of the reactor. The melt temperature rose to-290 ℃ during which white crystals formed rapidly in the cooler part of the reactor. After 12 hours, the reactor was cooled to-21 ℃ and then taken to a drying oven. The reactor was inverted, and the reaction product was removed by scraping material from the inner wall of flask 12. 42 grams of dimethylindium chloride was recovered from the reactor. The product was dimethyl indium chloride, confirmed by proton NMR spectroscopy and comparison to the known sample melting point.
Example II
The same procedure as described in example i is substantially repeated in this example. The reactor used in example I contained some residual reactive metallic indium solids. The reactor was then charged with another 40 grams of indium metal. The indium metal was heated to 280 c and then a combined stream of methyl chloride, hydrogen and argon vapor was bubbled through the melt. White crystalline dimethylindium chloride is formed in the cooler part of the reactor. About 51 grams of dimethyl indium chloride was recovered from the reactor. The composition was confirmed to be dimethyl indium chloride by proton NMR spectroscopy and comparison with the melting point of a known sample of dimethyl indium chloride.
Example III
The same procedure as described in example I was carried out in this example, except that a reactor with a larger elbow 14 to support a 7.7 cm diameter glass frit was used. About 5 grams of indium metal and 0.5 grams of indium trichloride were charged to the reactor and heated. At-300 c a red melt was formed which did not completely cover the glass frit. A stream of methyl chloride and 5% hydrogen in argon was slowly bubbled through the melt for 5 hours. The reactor was cooled and a white crystalline product was taken out, which was confirmed by the same method as described in example I, to give 6.6 g of methyl indium dichloride.
Example IV
This example substantially repeats the same steps described in example I. 20 grams of indium metal was charged to reactor 10 and heated above its melting point. Chlorine gas was slowly bubbled through the molten indium metal at-300 c for about 5 minutes to obtain a red melt. Methyl chloride and argon containing 5% hydrogen were bubbled through the melt for 6 hours. White crystalline dimethylindium chloride was formed in the reactor. About 26 grams of product was recovered from the reactor and was confirmed to be dimethyl indium chloride by NMR spectroscopy and melting point comparison tests.
Example V
Fig. 2 depicts a laboratory scale reactor 50 suitable for carrying out the process of the present invention. The reactor 50 comprises a U-shaped tube 52 having an internal diameter of 10 mm and a length of 7 cm. The U-tube connects two cylindrical vessels 54, 56. Each cylindrical container is 8 cm high and 4 cm in inner diameter. The cylindrical vessel 54 has a gas inlet 58 connected to a gas supply (not shown). A rubber plate 60 is placed at the open end of the cylindrical container 54, and a thermocouple wire 62 is placed through the plate 60 to measure the temperature of the indium metal melt. The opposite cylindrical vessel 56 was fitted at its top with an outlet tube 64 15 cm long and 3 cm in diameter. The outlet tube 64 is angled downward at about 45 deg. and the other end is attached to a 0.5 liter flask 66. A condenser 68 having an outlet 70 is connected to the flask 66. The outlet 70 of the condenser 68 is connected to an oil bubbler (not shown).
In an argon dry box, a mixture of 10 grams of indium and 0.5 grams of indium trichloride was added to reactor 50. The cylindrical vessel 56 connected to the outlet pipe 64 was filled with a glass single ring 72 (scientific glass, model J-121, single ring inside (diameter) 1/16 inches) to 1/4 of the vessel volume. The reactor 50 and outlet tube 64 are coiled with heating tape (not shown) and heated to 290 c to form a red indium melt 76.
Methyl chloride and an argon mixture containing 5% hydrogen were fed into the reactor 50 through gas inlet 58 to slowly bubble the gas mixture through the indium metal 76. Within three minutes, white crystalline product began to accumulate in 0.5 liter flask 66. A slow argon flow was passed to the outlet tube at gas inlet 78 to help move the white crystalline product into the 0.5 liter flask. After 3.5 hours, bubbling through the indium metal melt was stopped due to a small amount of gas mixture remaining in the reactor. The reactor was cooled and then taken to an argon drying oven. The product was collected and tested by the same technique as described in example 1, yielding 9.6 grams of dimethylindium chloride.
Prediction example I
A0.500 literround bottom flask was used as reactor for carrying out the process of the invention. The reactor was set up as illustrated in FIG. 1 according to example I. About 40 grams of gallium metal and 3.5 grams of gallium trichloride were added to the glass frit in the flask. Then the reactor is equipped with a water condenser, and the two ends of the condenser are provided with an inlet and an outlet. The condenser was connected to the gas outlet of the reactor. The thermometer is brought into contact with the frit through the plate. An oil bubbler was connected to the top outlet of the condenser and the vapor from the reactor was monitored. In addition, a bubbler was connected to a gas supply at the gas inlet line at the bottom of the reactor. The gas inlet tube is used to deliver the organochlorine reactant to the reactor.
The lower part of the reactor was placed on a sand bath, the sand surface being about 5 cm higher than the glass frit. The sand bath temperature is controlled to maintain the desired melting temperature. The mixture of gallium metal and gallium trichloride is heated to a temperature above the melting point to 240 ℃ where the gallium and gallium trichloride react to produce a red liquid. Methyl chloride and another argon mixture containing 5% hydrogen were fed into the reactor through the gas inlet tube. A stream of methyl chloride vapor was first introduced into the reactor and the gas was slowly bubbled through the gallium melt. An argon stream containing 5% hydrogen was then added to the methyl chloride vapor stream.
After a short period of time, crystals should grow on the cooler parts of the reactor. The melt temperature is then increased slightly to allow crystalline material to form rapidly in the cooler portion of the reactor. The reactor was then cooled and sent to a drying oven for recovery to obtain crystalline dimethylgallium chloride.
Claims (30)
1. A method of producing organo indium chloride comprising contacting an organo chloride with an indium metal melt to produce organo indium chloride.
2. The method of claim 1, further comprising adding an activator to the indium metal melt prior to contacting the organo chloride with the indium metal.
3. The method of claim 2, wherein the activator is selected from Cl2，HCl，InCl3，FeCl3，(PtCl4)-2，PdCl2A halide of (1).
4. The process of claim 2, wherein the activator is selected from In2O3，TiO2，NiO2，Fe2O3An oxide of (2).
5. The method of claim 2, wherein the amount of activator is about 5 to about 50 mole percent of the indium metal melt.
6. The method of claim 1 wherein the organic chloride is included in a reducing agent vapor mixture.
7. The method of claim 6, wherein the reducing agent is hydrogen present in the vapor mixture in an amount of from about 5 mole% to about 60 mole%.
8. The process of claim 1, wherein the organo indium chloride produced is dimethyl indium chloride.
9. The process of claim 1, wherein the organo indium chloride obtained is methyl indium dichloride.
10. The method of claim 1, wherein the organo chloride is contacted with the indium melt for a time of no greater than about 0.5 seconds to form methyl indium dichloride.
11. The method of claim 1, wherein the organic chloride is contacted with the molten indium to form dimethylindium chloride for a period of time of not less than about 10 seconds.
12. The method of claim 1, wherein the contacting occurs at a temperature of about 240 ℃ to about 350 ℃.
13. The method of claim 1, wherein the contacting occurs at a temperature of 280 ℃ to 300 ℃.
14. The process of claim 1 wherein said organochloride is selected from the group consisting of methyl chloride, ethyl chloride, propyl chloride, neopentyl chloride, chloromethyltrimethylsilane, chlorotrifluoromethane, and chlorobenzene.
15. A method of producing an organo indium chloride comprising:
(a) a melt of indium metal and an activator is formed,
(b) an organo chloride is contacted with the indium metal melt to form an organo indium chloride.
16. The method of claim 15, wherein the indium metal melt is at a temperature of 240 ℃ to 350 ℃.
17. The method of claim 15, wherein said organo chloride is methyl chloride and said organo indium chloride is dimethyl indium chloride or methyl indium dichloride.
18. The process of claim 15, further comprising adding a reducing agent to said organo chloride prior to contacting said organo chloride with said indium metal melt, said reducing agent being selected from the group consisting of hydrogen, trimethylsilane, dichlorosilane, ethylene or acetylene.
19. The method of claim 15, wherein the activator is selected from Cl2，HCl，InCl3，FeCl3，(PtCl4)-2，PdCl2A halide of (1).
20. The method of claim 15, wherein the activator is selected from In2O3，TiO2，NiO2，Fe2O3An oxide of (2).
21. The method of claim 15, further comprising collecting the organo indium chloride.
22. A method of producing an organo indium chloride comprising:
(a) filling metallic indium and an activating agent into a reactor,
(b) heating the indium metal and activator above the melting point of the indium metal to form an indium metal melt, and
(c) an organo chloride is contacted with the indium metal melt to form an organo indium chloride.
23. The method of claim 22, wherein
(a) The metallic indium and the organic chloride are continuously fed into the reactor to continuously form the organic indium chloride.
(b) The organo indium chloride is withdrawn from the reactor.
24. The method of claim 23, further comprising collecting the organo indium chloride.
25. The method of claim 24, wherein the collecting step further comprises collecting the organo indium chloride into solution using a polar, aprotic solvent.
26. The method of claim 24, further comprising depositing the indium oxide or indium oxide doped coating on the glass substrate using an organo indium chloride as a precursor gas.
27. The method of claim 23, wherein the activator is selected from Cl2，HCl，InCl3，FeCl3，(PtCl4)-2，PdCl2，In2O3，TiO2，NiO2Or Fe2O3The active agent is present therein at about 5 mole% to about 50 mole%.
28. The process of claim 23 wherein the organic chloride is contained in the hydrogen-containing vapor mixture in an amount of from about 5 mole percent to about 60 mole percent.
29. A process for producing an organo-metal chloride wherein the metal is selected from indium or gallium, said process comprising contacting an organo-chloride with the metal to produce an organo-indium chloride or an organo-gallium chloride.
30. A method for producing an organo indium halide comprising contacting an organo halide selected from the group consisting of chloride, iodide and bromide with an indium metal melt to produce an organo indium halide.
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| CN105986314B (en) * | 2015-02-05 | 2018-06-08 | 东莞市中镓半导体科技有限公司 | A kind of reactor for vapor phase epitaxial growth semiconductor single crystal material |
| CN107250139A (en) * | 2015-02-13 | 2017-10-13 | 优美科股份公司及两合公司 | Method for preparing alkyl indium compound and application thereof |
| CN107250139B (en) * | 2015-02-13 | 2020-09-04 | 优美科股份公司及两合公司 | Method for producing alkyl indium compounds and use thereof |
| CN109824495A (en) * | 2019-02-02 | 2019-05-31 | 盐城锦明药业有限公司 | A kind of novel coupling reaction is preparing the application in carbon-carbon bond structural compounds |
| CN109824495B (en) * | 2019-02-02 | 2022-12-09 | 盐城师范学院 | Application of novel coupling reaction in preparation of carbon-carbon bond structure compound |
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