CN114275807B - Preparation method of indium nitrate solution, preparation method and application of high-activity indium oxide - Google Patents
Preparation method of indium nitrate solution, preparation method and application of high-activity indium oxide Download PDFInfo
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- CN114275807B CN114275807B CN202210031987.8A CN202210031987A CN114275807B CN 114275807 B CN114275807 B CN 114275807B CN 202210031987 A CN202210031987 A CN 202210031987A CN 114275807 B CN114275807 B CN 114275807B
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- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 25
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 230000000694 effects Effects 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 74
- 229910052738 indium Inorganic materials 0.000 claims abstract description 52
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002244 precipitate Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 238000000975 co-precipitation Methods 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 10
- 239000007800 oxidant agent Substances 0.000 claims description 9
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000013543 active substance Substances 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 10
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 6
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001272 nitrous oxide Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a preparation method of an indium nitrate solution, a preparation method of high-activity indium oxide and application thereof, wherein the preparation method of the indium nitrate solution comprises the following steps: (1) adding water after metal indium is hot melted to obtain indium flower; (2) Adding dilute nitric acid into the indium flower, sealing the reaction kettle, heating, and stirring for reaction; the preparation method of the high-activity indium oxide comprises the following steps: 1) Preparing an indium nitrate solution; 2) Diluting an indium nitrate solution, adding ammonia water to perform coprecipitation reaction, separating a precipitation product, washing and drying an obtained indium precipitate to obtain indium hydroxide powder; 3) Adding deionized water into the indium hydroxide powder, ball milling, drying and calcining to obtain high-activity indium oxide powder; according to the invention, dilute nitric acid is added to react with indium flower, so that the indium nitrate In the obtained indium nitrate solution has high yield and high purity, and the subsequent preparation of indium oxide can prepare nano-scale In with no agglomeration, good uniformity, large activity and high purity without adding an active agent 2 O 3 And (3) powder.
Description
Technical Field
The invention belongs to the technical field of ITO targets, and particularly relates to a preparation method of an indium nitrate solution, a preparation method of high-activity indium oxide and application of the high-activity indium oxide.
Background
Indium oxide is usually In the form of white or pale yellow powder, in 2 O 3 The powder is used as a main raw material for preparing the ITO target material, and has the advantages of high purity, good dispersibility, fine and uniform granularity. In recent years, the ITO target is widely applied to the high and new technical fields such as photoelectric industry, semiconductor field, photovoltaic solar energy, integrated circuit and the like and military field. The preparation method comprises gel method, hydrothermal method, electrolytic method, chemical precipitation method, etc.
Compared with the method, the nitric acid method in the chemical precipitation method has the advantages of simple equipment and preparation process, easy control of operation, short production period and the like. However, in the process of preparing indium nitrate, concentrated nitric acid is often used as a reaction raw material, so that the operation safety requirement is high, and a large amount of nitrogen dioxide (NO) is released when the metal indium is dissolved in the nitric acid 2 ) The gas can cause serious pollution to the atmospheric environment. And In preparation 2 O 3 In the process of powder, the prepared powder is easy to agglomerate, and many researchers are In 2 O 3 The addition of an active agent during the powder preparation process reduces agglomeration, but this itself introduces impurities, reducing In 2 O 3 Purity of the powder.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects and shortcomings in the background art, and provides a preparation method of an indium nitrate solution, a preparation method of high-activity indium oxide and application of the high-activity indium oxide.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing an indium nitrate solution, comprising the following steps:
(1) Heating and melting metal indium, adding the metal indium into water, and filtering to obtain indium flower;
(2) And then placing the indium flower into a reaction kettle, adding dilute nitric acid, sealing the reaction kettle, heating, and stirring for reaction.
Preferably, in the step (1), the mass ratio of the metal indium to the water is 1:3-5;
in the step (2), the mass concentration of the dilute nitric acid is 10-30%, and the mass ratio of the indium flower to the dilute nitric acid is 1:5-8; the temperature is raised to 60-75 ℃, and the stirring reaction time is 2-6 h.
Preferably, the method further comprises the following steps: collecting generated gas in the stirring reaction process; and after the stirring reaction is finished, adding an oxidant into the reaction kettle, introducing the collected gas into the reaction kettle, and continuing the stirring reaction to obtain the indium nitrate solution.
Preferably, the oxidant comprises at least one of oxygen and hydrogen peroxide; when the oxidant is hydrogen peroxide, the mass concentration of the hydrogen peroxide is 15-25%, the mass ratio of the indium flower to the hydrogen peroxide is 1:3-5, and the time for continuous stirring reaction is 3-6 h.
According to the invention, the oxidant is added into the system after the reaction of the dilute nitric acid and the indium flower, so that nitrogen dioxide or nitric oxide waste gas generated in the process of the nitric acid reaction can be further oxidized into nitrous oxide, and then the nitrous oxide and water react to generate nitric acid, thereby avoiding the generation of atmospheric pollutants in the process of the reaction, and saving the input amount of nitric acid. Meanwhile, hydrogen peroxide or oxygen is used as an oxidant, and the concentration and the dosage of the oxidant are controlled, so that nitrogen dioxide can be completely oxidized to generate nitric acid and water effectively, and other oxidation byproducts, impurities and the like can not be generated to influence the purity of the indium nitrate product. And nitric acid is regenerated in the preparation process, so that energy sources can be saved.
As a general inventive concept, the present invention provides a method for preparing high-activity indium oxide, comprising the steps of:
1) The indium nitrate solution is prepared by adopting the preparation method;
2) Diluting the indium nitrate solution by adding water, adding ammonia water, performing coprecipitation reaction, and separating a precipitation product to obtain an indium precipitate; washing and drying the indium precipitate to obtain indium hydroxide powder;
3) Adding deionized water into the indium hydroxide powder, performing ball milling treatment, drying and calcining to obtain high-activity indium oxide powder; no active agent is added in the process of preparing the high-activity indium oxide powder.
Preferably, in the step 2), the indium nitrate solution is diluted to 3-6% of mass concentration, if the indium nitrate solution is too high in concentration and is not easy to dissolve, the solution is easy to be turbid, and the mass concentration of the ammonia water is 18-25%;
the temperature of the coprecipitation reaction is 30-55 ℃; when the pH value of the reaction system reaches 3.5-5.0 during the coprecipitation reaction, a filtering system is used for filtering and separating a precipitation product to obtain indium precipitate, and the obtained filtrate (containing unreacted indium nitrate) is returned to the precipitation reaction kettle again to continue the coprecipitation reaction; stopping the reaction when the pH value of the reaction system reaches 7-7.5, standing for 2.5-3.5 h, and filtering to collect indium precipitate. If the pH is too high, other nitrate impurities precipitate, and the quality of the nitrate impurities is affected.
Further preferably, the indium nitrate solution is diluted to a mass concentration of 5 to 6%; the mass concentration of the ammonia water is 18-20%.
Preferably, in the step 3), after deionized water is added into the indium hydroxide powder, the viscosity of the indium hydroxide powder is regulated to 120-150 CPS; the ball milling temperature is 50-80 ℃ and the ball milling time is 5-10 h. Through the ball milling process, the particle size of the indium hydroxide powder can be reduced, the particle size range distribution is narrowed, the concentration is more uniform, and the sintering performance can be improved.
Preferably, the calcination temperature is 650-850 ℃ and the calcination time is 3.5-6.5 h.
In the steps 2) and 3), the drying mode is spray drying or vacuum drying.
As a general inventive concept, the invention provides an application of the high-activity indium oxide prepared by the preparation method in ITO targets.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation process of the indium nitrate, dilute nitric acid is added to react with the indium flower, and the reaction is ensured to be complete by optimizing each reaction parameter, so that the indium nitrate solution is obtained, and the overall yield and purity are high. If concentrated nitric acid is added, the product with higher yield and purity cannot be obtained, meanwhile, the reaction is severe in the process of dissolving the metal indium by the nitric acid, a large amount of nitrogen oxide gas can be generated, a large amount of nitric acid is wasted, the cost is increased due to the later treatment of the nitrogen oxide, and meanwhile, a certain influence is brought to the environment.
2. The indium oxide prepared by the indium nitrate solution prepared by the method of the invention can be prepared into nanoscale In with no agglomeration, good uniformity, large activity and high purity by combining a proper process without adding organic matters such as an active agent and the like In the preparation process 2 O 3 The powder provides a reliable raw material for preparing the high-end ITO target.
Detailed Description
The present invention will be described more fully hereinafter with reference to the preferred embodiments for the purpose of facilitating understanding of the present invention, but the scope of the present invention is not limited to the following specific embodiments.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1:
a method for preparing an indium nitrate solution, comprising the following steps:
1) Heating metal indium to be molten, then slowly introducing the metal indium into a water tank filled with deionized water at a constant speed, cooling, and filtering to obtain indium flower, wherein the mass ratio of the metal indium to the water is 1:3;
2) Placing the indium flower into a reaction kettle of a constant temperature system and a stirring system, adding a nitric acid solution with the mass concentration of 20%, wherein the mass ratio of the indium flower to the nitric acid solution is 1:6, sealing the reaction kettle, setting the temperature of the constant temperature system to 60 ℃, and simultaneously starting the stirring system, wherein the reaction time is 4 hours;
3) Collecting generated gas in the stirring reaction process; after the stirring reaction is finished, hydrogen peroxide with the mass concentration of 18% is added at a constant speed through a charging port of the reaction kettle, the mass ratio of the indium flower to the hydrogen peroxide is 1:4, and the collected gas is introduced into the reaction kettle to continue stirring reaction for 6 hours, so that the indium nitrate solution is obtained.
The yield of indium nitrate in the indium nitrate solution was found to be 99%, and the purity of indium nitrate separated from the indium nitrate solution was found to be 99.999%.
Example 2:
a method for preparing an indium nitrate solution, comprising the following steps:
1) Heating metal indium to be molten, then slowly introducing the metal indium into a water tank filled with deionized water at a constant speed, cooling, and filtering to obtain indium flower, wherein the mass ratio of the metal indium to the water is 1:4;
2) Placing the indium flower into a reaction kettle of a constant temperature system and a stirring system, adding nitric acid solution with the mass concentration of 15%, wherein the mass ratio of the indium flower to the nitric acid solution is 1:5, sealing the reaction kettle, setting the temperature of the constant temperature system to 75 ℃, and simultaneously starting the stirring system, wherein the reaction time is 3 hours;
3) Collecting generated gas in the stirring reaction process; after the stirring reaction is finished, hydrogen peroxide with the mass concentration of 25% is added at a constant speed through a charging port of the reaction kettle, the mass ratio of the indium flower to the hydrogen peroxide is 1:4, and the collected gas is introduced into the reaction kettle to continue stirring reaction for 5 hours, so that the indium nitrate solution is obtained.
The yield of indium nitrate in the indium nitrate solution was 95%, and the purity of indium nitrate separated from the indium nitrate solution was 99.998%.
Comparative example 1:
unlike example 1, nitric acid was used at a mass concentration of 50%.
The yield of indium nitrate in the indium nitrate solution was 93.8%, and the purity of indium nitrate separated from the indium nitrate solution was 99.995%. This yield was significantly lower than example 1, with a slightly lower purity than example 1.
Comparative example 2:
in the preparation method of the indium nitrate solution, unlike in example 1, in step 2), the temperature of the constant temperature system was set to 80 ℃.
The yield of indium nitrate in the indium nitrate solution was 88.9%, and the purity of indium nitrate separated from the indium nitrate solution was 99.99%. This yield and purity were significantly lower than in example 1.
Example 3:
the preparation method of the high-activity indium oxide comprises the following steps:
1) The indium nitrate solution prepared in example 1 was diluted (diluted with water) to a mass concentration of 5%. Placing the mixture into a precipitation reaction kettle with a constant temperature system and a stirring system. Setting the temperature of the constant temperature system to 45 ℃, starting the stirring system, and adding ammonia water with the mass concentration of 18% at a constant speed to perform coprecipitation reaction. When the pH value of the reaction system reaches 4.5, a filtering system is used for filtering and separating a precipitation product to obtain an indium precipitate, and the obtained filtrate (containing unreacted indium nitrate) is returned to the precipitation reaction kettle again to continue the coprecipitation reaction; stopping the reaction when the pH value of the reaction system reaches 7.5, standing for 3 hours, and filtering and collecting indium precipitate;
2) Washing the indium precipitate obtained by filtration by deionized water, and then placing the indium precipitate into a vacuum dryer for drying for 10 hours at the drying temperature of 100 ℃ to obtain indium hydroxide powder;
3) Adding deionized water into the dried indium oxide powder, adjusting the viscosity of the powder to 130CPS, and performing ball milling for 4 hours at 70+/-5 ℃; calcining at 700 deg.C for 6.5 hr, and naturally cooling to room temperature to obtain spherical high-activity pale yellow In 2 O 3 Particles having an average particle diameter of 32nm; the yield was 98.6% and the purity was 99.997%.
Example 4:
the preparation method of the high-activity indium oxide comprises the following steps:
1) The indium nitrate solution prepared in example 2 was diluted (diluted with water) to a mass concentration of 6%. Placing the mixture into a precipitation reaction kettle with a constant temperature system and a stirring system. Setting the temperature of the constant temperature system to 45 ℃, starting the stirring system, and adding ammonia water with the mass concentration of 20% at a constant speed to perform coprecipitation reaction. When the pH value of the reaction system reaches 4.5, a filtering system is used for filtering and separating a precipitation product to obtain an indium precipitate, and the obtained filtrate (containing unreacted indium nitrate) is returned to the precipitation reaction kettle again to continue the coprecipitation reaction; stopping the reaction when the pH value of the reaction system reaches 7.5, standing for 3 hours, and filtering and collecting indium precipitate;
2) Washing the indium precipitate obtained by filtration by deionized water, and then placing the indium precipitate into a vacuum dryer for drying for 10 hours at the drying temperature of 120 ℃ to obtain indium hydroxide powder;
3) Adding deionized water into the dried indium oxide powder, adjusting the viscosity of the powder to 140CPS, and performing ball milling for 4 hours at 70+/-5 ℃; then vacuum drying and calcining at 850 ℃ for 5 hours, and then naturally cooling to room temperature to obtain the spherical and uniformly distributed high-activity pale yellow In 2 O 3 Particles having an average particle diameter of 40nm; the yield was 91.3% and the purity was 99.995%.
Comparative example 3:
unlike example 3, in step 1), the indium nitrate solution prepared in example 1 was diluted (diluted with water) to a mass concentration of 10%.
In obtained 2 O 3 The average particle diameter of the particles is 50nm; the yield was 87% and the purity was 99.991%.
Comparative example 4:
unlike example 3, in step 1), the reaction was stopped when the pH of the reaction system was 8.5.
In obtained 2 O 3 The average particle diameter of the particles is 45nm; the yield was 79% and the purity was 99.99%.
Claims (6)
1. The preparation method of the high-activity indium oxide is characterized by comprising the following steps of:
1) Preparing an indium nitrate solution; the preparation method of the indium nitrate solution comprises the following steps:
(1) Heating and melting metal indium, adding the metal indium into water, and filtering to obtain indium flower;
(2) Then placing the indium flower in a reaction kettle, adding dilute nitric acid, sealing the reaction kettle, heating, and stirring for reaction; the mass concentration of the dilute nitric acid is 10-30%, and the mass ratio of the indium flower to the dilute nitric acid is 1:5-8; the temperature is raised to 60-75 ℃, and the stirring reaction time is 2-6 h;
collecting generated gas in the stirring reaction process; after the stirring reaction is finished, adding an oxidant into the reaction kettle, introducing the collected gas into the reaction kettle, and continuing the stirring reaction to obtain an indium nitrate solution;
2) Diluting the indium nitrate solution by adding water, diluting the indium nitrate solution to 3-6% of mass concentration, adding ammonia water, wherein the mass concentration of the ammonia water is 18-25%, and performing coprecipitation reaction, wherein the temperature of the coprecipitation reaction is 30-55 ℃; when the pH value of the reaction system reaches 3.5-5.0 during the coprecipitation reaction, a filtering system is used for filtering and separating a precipitation product to obtain indium precipitate, and the obtained filtrate is returned to the precipitation reaction kettle again to continue the coprecipitation reaction; stopping the reaction when the pH value of the reaction system reaches 7-7.5, standing for 2.5-3.5 h, and filtering to collect indium precipitate; washing and drying the indium precipitate to obtain indium hydroxide powder;
3) Adding deionized water into the indium hydroxide powder, adjusting the viscosity to 120-150 CPS, performing ball milling treatment at 50-80 ℃ for 5-10 hours, drying and calcining to obtain the high-activity indium oxide powder.
2. The method according to claim 1, wherein in the step (1), the mass ratio of the metal indium to the water is 1:3-5.
3. The method according to claim 1, wherein the oxidizing agent comprises at least one of oxygen and hydrogen peroxide; when the oxidant is hydrogen peroxide, the mass concentration of the hydrogen peroxide is 15-25%, the mass ratio of the indium flower to the hydrogen peroxide is 1:3-5, and the time for continuous stirring reaction is 3-6 h.
4. The method for producing highly active indium oxide according to claim 1, wherein the indium nitrate solution is diluted to a mass concentration of 5 to 6%; the mass concentration of the ammonia water is 18-20%.
5. The method for producing highly active indium oxide according to any one of claims 1 to 4, wherein the calcination temperature is 650 to 850 ℃ and the time is 3.5 to 6.5 hours.
6. Use of the high-activity indium oxide prepared by the preparation method according to any one of claims 1 to 5 in ITO targets.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| CN108557872A (en) * | 2018-05-22 | 2018-09-21 | 韶关市锦源实业有限公司 | A kind of preparation method of indium tin oxide |
| CN109824081A (en) * | 2019-03-27 | 2019-05-31 | 云南锡业集团（控股）有限责任公司研发中心 | A method of producing nano indium oxide powder |
| CN111362298A (en) * | 2020-03-06 | 2020-07-03 | 郑州大学 | Preparation method of indium oxide spherical powder with controllable particle shape |
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2022
- 2022-01-12 CN CN202210031987.8A patent/CN114275807B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092781A (en) * | 2010-12-10 | 2011-06-15 | 株洲冶炼集团股份有限公司 | Method for preparing battery grade indium hydroxide and indium oxide |
| CN108557872A (en) * | 2018-05-22 | 2018-09-21 | 韶关市锦源实业有限公司 | A kind of preparation method of indium tin oxide |
| CN109824081A (en) * | 2019-03-27 | 2019-05-31 | 云南锡业集团（控股）有限责任公司研发中心 | A method of producing nano indium oxide powder |
| CN111362298A (en) * | 2020-03-06 | 2020-07-03 | 郑州大学 | Preparation method of indium oxide spherical powder with controllable particle shape |
Non-Patent Citations (1)
| Title |
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| 纳米氧化锡和氧化铟粉体液相法制备研究;仇晨;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;B020-1244 * |
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