CN109231259B - Method for preparing ultrafine ITO powder from metal indium and metal tin - Google Patents
Method for preparing ultrafine ITO powder from metal indium and metal tin Download PDFInfo
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Abstract
The invention discloses a method for preparing ultrafine ITO powder from metal indium and tin. Directly taking metal indium ingots and tin ingots as raw materials, carrying out gas oxidation in a hot ball mill at the temperature of 100-300 ℃ after composition design and alloying premelting to generate indium oxide and tin oxide, simultaneously stripping the just generated indium oxide and tin oxide from the surface of an alloy molten drop by utilizing the ball milling function of a ball mill, finishing fine milling to finally obtain ITO powder, and producing an ITO composite powder product with uniform granularity after air flow classification. Compared with the traditional process, the method has the advantages of short reaction flow, fine product granularity, less reagent consumption and the like, and solves the problem that the direct metal indium and tin generates an oxide film in the oxidation process to be difficult to further oxidize.
Description
Technical Field
The invention belongs to the field of material metallurgy, and particularly relates to a method for preparing ultrafine ITO powder by hot ball milling oxidation.
Background
Indium Tin Oxide (ITO) has the advantages of high light transmittance, low resistivity, high film-making hardness, good chemical stability and etching performance, and the like, and is widely applied to the field of tip manufacturing of liquid crystal displays, solar cells, thin film light-emitting devices, sensors, and the like. The existing preparation method respectively pulverizes indium oxide and tin oxide, mixes the powders, molds and sinters the powders into ITO target material, and has long flow and high pulverization cost. And because the stable tin dioxide film is formed after the metal tin is oxidized, the tin dioxide film is not dissolved in conventional acid and alkali, and the further proceeding of the oxidation reaction is hindered, so the tin oxide powder is prepared by a wet chemical method, and the common characteristics are that a tin salt precursor is synthesized in a solution, and then the tin oxide is obtained by calcining or not calcining, and the main problems are long flow path and large waste water amount.
Patent CN102923765A "an Indium Tin Oxide (ITO) nano powder and its manufacturing method" uses soluble salt raw materials of indium and tin, adds organic matter, and synthesizes ellipsoid indium oxide and tin oxide powder by combustion; in patent CN102417203, "a method for preparing ultrafine ITO powder by fuel synthesis" also uses indium and tin nitrate as raw materials, and obtains ultrafine ITO powder by reduction combustion, and this kind of method has large reagent consumption and high product cost. Patent CN105540647A discloses an ITO powder for preparing a rotary target by thermal spraying and a production method and application thereof, wherein a chemical coprecipitation method is adopted to obtain ITO coprecipitation powder in one step, ITO powder is obtained by thermal treatment, the process is short, the production concept of short process is met, and the similar methods also include a hydrothermal method and a sol-gel method. The spray oxidation method is also a direct synthesis method, and metal indium and tin are used as raw materials, so that the process is further simplified, but the spray equipment investment is large, and the process control requirement is high.
From the consideration of simplified process, the direct oxidation of metal indium and tin is the most direct method for preparing indium oxide and tin oxide, but the problem is that the passivation effect of the oxide film makes the further oxidation of metal difficult, especially the metal tin, once the tin oxide film is formed, the further proceeding of the reaction can be blocked, the oxidation reaction can be continuously proceeded only by timely stripping off the oxide layer, and the ball milling can achieve the effect. Therefore, the patent provides a method for preparing ultrafine ITO powder from metal indium and tin, which oxidizes the metal indium and tin by using air in a heating state and synchronously performs ball milling to realize rapid oxidation of the indium and the tin, peeling of an oxide layer and refining and mixing of oxidation products.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides a method for preparing ultrafine ITO powder from metal indium and metal tin, which adopts a hot ball mill as reaction equipment to complete the synchronous oxidation of the metal indium and tin and the synchronous refinement of oxides, thereby realizing the economical, efficient, controllable and stable production of the ultrafine indium oxide and tin powder.
The purpose of the invention is realized by the following technical scheme:
a method for preparing ultrafine ITO powder from metal indium and metal tin comprises the steps of taking metal indium ingots and metal tin ingots as raw materials, firstly carrying out composition design and alloying premelting, carrying out hot ball milling oxidation in a hot ball mill at the temperature of 100-300 ℃ under the condition of introducing oxidizing gas, oxidizing the metal indium and the metal tin in a liquid state, simultaneously carrying out ball milling, and obtaining the ultrafine ITO powder after the hot ball milling oxidation is finished.
The reaction temperature of the inner chamber of the hot ball mill is 100-300 ℃, metal indium and tin are easily oxidized by air to generate indium oxide and tin oxide, and as can be seen from figure 3, the Gibbs free energy variation value of the reaction is below-300 kJ/mol within the range of 0-1000 ℃, and the reaction temperature is not easily too high along with the temperature rise, wherein indium is easier to oxidize than tin. However, the indium oxide and tin oxide formed coat the surface of the metal droplet, and inhibit further progress of the oxidation reaction.
Sn+O2(g)＝SnO2
2In+1.5O2(g)＝In2O3
The reaction temperature in the method is 100-300 ℃, the melting point of the metal indium is 156.61 ℃, the melting point of the metal tin is 231.89 ℃, and the melting point of the indium-tin alloy melt is lower. Meanwhile, the reaction is exothermic, and excessively high temperature is not favorable for improving the oxidation degree and increasing the energy consumption.
According to the technical scheme, ultrafine ITO powder is directly prepared from metal indium and metal tin by utilizing a hot ball milling oxidation reaction, the newly generated indium oxide and tin oxide are subjected to ball milling refinement during oxidation, an oxide layer on the surface can be stripped, the newly generated indium oxide and tin oxide powder is continuously refined through ball milling, and the ultrafine ITO powder is directly produced.
Preferably, the mass ratio of the metal indium ingot to the metal tin ingot in the composition design is 9.45: 1.
preferably, the alloying pre-melting temperature is 250-300 ℃, and the indium metal ingot and the tin metal ingot are pre-melted at the temperature of 250-300 ℃ so that indium and tin form an alloy melt with uniform components, thereby ensuring the uniformity of oxidation reaction and the uniformity distribution of final oxides;
preferably, the oxidizing gas is air or oxygen.
Preferably, the blowing linear velocity of the oxidizing gas is 0.1-2 m/s, the oxidation of indium and tin can be accelerated by forcing the blowing of the oxidizing gas, a certain stirring effect is exerted on the molten alloy liquid, the oxidation diffusion mass transfer is strengthened, and the oxidation of indium and tin can be more sufficient; the blow-in linear velocity is more preferably 0.5 to 1.5 m/s.
Preferably, the ball milling strength in the hot ball milling process is 30-120 rpm, the filling rate is 10-50%, and the ball-to-material ratio is 3-9, and the parameters can ensure the ball milling efficiency and the production efficiency; further preferably, the filling rate is 20-40%, and the ball-to-feed ratio is 5-8.
The ball milling of the invention can play two roles, on one hand, the indium oxide and tin product layer on the surface of the alloy molten drop is continuously stripped, so that the oxidation reaction is continuously carried out, on the other hand, the generated indium oxide and tin oxide are immediately oxidized by the ball milling, and the superfine indium oxide and tin oxide are directly obtained. However, the ball milling operation is a high energy consuming process, so that it is not suitable to use an excessively high rotational speed.
Preferably, the ball material medium used for ball milling is one of zirconia, agate, hard alloy and corundum, and is made of inert materials, so that the high-temperature stability and the product purity can be ensured; preferably zirconia.
Preferably, the time of the hot ball milling reaction process is 1-5 h, so that sufficient oxidation and fine milling of indium and tin can be ensured; further preferably 1 to 3 hours.
The method for preparing the ultrafine ITO powder by using the metal indium and the metal tin specifically comprises the following steps:
s1, composition design: accurately weighing indium metal ingots and tin metal ingots according to a certain mass ratio;
s2, alloying and premelting: pre-melting the weighed indium metal ingots and tin metal ingots at the temperature of 250-300 ℃ to form alloy melt with uniform components from indium and tin;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, and starting electric heating to enable the temperature of an inner cavity of the ball mill to reach 100-300 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining a certain rotating speed, simultaneously blowing oxidizing gas into the inner cavity from the gas inlet, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: and after reacting for a certain time, stopping heating, ball milling and blowing oxidizing gas, opening a discharge opening to discharge the ITO powder, completely cooling to a greenhouse, then placing into a storage bin, and grading to obtain ITO products with different particle sizes.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method creatively adopts the premelting-liquid-phase low-temperature ball milling oxidation of the metal indium and the metal tin alloy to replace the current mainstream process of precursor preparation-calcining decomposition, greatly improves the productivity, simplifies the flow, adopts clean air or oxygen as the only auxiliary material oxidant, reduces the consumption of the reagent, greatly reduces the production cost, and realizes the green, low-carbon and high-efficiency preparation of the ultrafine ITO powder.
(2) The method disclosed by the invention is used for oxidation at a low temperature, the oxidation temperature is only 100-300 ℃, and compared with a high-temperature oxidation process used in the prior art, the method disclosed by the invention has the advantages that the requirement on equipment is reduced, the energy consumption is reduced, and the production cost is reduced.
(3) The method of the invention integrates the oxidation of the indium tin and the stripping and refining of the oxidation product into one process, has short flow, cleanness and high efficiency, and solves the defect that the oxidation reaction is difficult to proceed along with the generation of indium oxide and tin oxide films in the traditional oxidation process.
(4) The invention realizes the synchronous oxidation of indium and tin, and shortens the flow of respectively milling indium oxide and tin oxide to produce ultrafine ITO powder in the prior art.
Drawings
FIG. 1 is a schematic diagram of the process flow of the method for preparing ultrafine ITO powder from metal indium and metal tin according to the invention.
FIG. 2 is an XRD pattern of ITO powder obtained in example 1 of the present invention.
FIG. 3 is Δ G of the oxidation reaction of metallic tin and indiumθ-a T-relationship diagram.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art 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 limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
In the metallic indium ingot as a raw material: in is more than 99.99 percent, and the total amount of impurities is less than 0.01 percent; in the metallic tin ingot: sn is more than 99.99 percent, and the total amount of impurities is less than 0.01 percent.
The embodiment provides a method for preparing ultrafine ITO powder from metal indium and metal tin, a process flow chart of which is shown in the attached figure 1, and the method comprises the following specific steps:
s1, composition design: taking a metal indium ingot and a metal tin ingot according to the mass ratio of 9.45: 1, accurately weighing 1000 g;
s2, alloying and premelting: pre-melting weighed indium metal ingots and tin metal ingots in a crucible at the temperature of 280 ℃ to enable indium and tin to form alloy melt with uniform components, and stirring for a plurality of times;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, putting a corresponding number of zirconia balls according to the ball material ratio of 5, and starting electric heating to enable the temperature of the inner cavity of the ball mill to reach 200 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining the rotating speed at 100rpm, simultaneously blowing air into the inner cavity from the air inlet at a linear speed of 0.5m/s, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: after reacting for 2h, stopping heating, ball milling and air blowing, opening a discharge opening to discharge the ITO powder, naturally cooling to a greenhouse, and then placing into a storage bin.
The product ITO composite powder is analyzed and tested for oxygen content to obtain the indium tin oxide (In)2O3+SnO2) More than 96.9 percent, the particle size range of the particle size measured by a laser particle sizer is between 0.40 and 8.4 mu m, the average particle size is 4.33 mu m, wherein 5.0 mu m accounts for 76 percent. The XRD pattern is shown in figure 2, and the high diffraction peak intensity and good crystallinity of the ITO composite powder can be seen from the XRD pattern; the product has high purity, and all the products are indium oxide and tin oxide.
Example 2
The raw materials of the indium metal ingot and the tin metal ingot were the same as those in example 1.
The embodiment provides a method for preparing ultrafine ITO powder from metal indium and metal tin, a process flow chart of which is shown in the attached figure 1, and the method comprises the following specific steps:
s1, composition design: taking a metal indium ingot and a metal tin ingot according to the mass ratio of 9.45: 1, accurately weighing 1000 g;
s2, alloying and premelting: pre-melting weighed indium metal ingots and tin metal ingots in a crucible at the temperature of 300 ℃ to form alloy melt with uniform components of indium and tin, and stirring for a plurality of times;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, putting a corresponding number of corundum balls according to the ball-to-material ratio of 9, and starting electric heating to enable the temperature of an inner cavity of the ball mill to reach 120 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining the rotating speed at 120rpm, simultaneously blowing air into the inner cavity from the air inlet at a linear speed of 1.0m/s, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: after reacting for 1h, stopping heating, ball milling and air blowing, opening a discharge opening to discharge the ITO powder, naturally cooling to a greenhouse, and then placing into a storage bin.
The product ITO composite powder is analyzed and tested for oxygen content to obtain the indium tin oxide (In)2O3+SnO2) More than 99.86 percent, the particle size range of the particle size measured by a laser particle sizer is between 0.58 and 10.2 mu m, the average particle size is 5.18 mu m, wherein, the-5.0 mu m accounts for 63 percent.
Example 3
The raw materials of the indium metal ingot and the tin metal ingot were the same as those in example 1.
The embodiment provides a method for preparing ultrafine ITO powder from metal indium and metal tin, a process flow chart of which is shown in the attached figure 1, and the method comprises the following specific steps:
s1, composition design: taking a metal indium ingot and a metal tin ingot according to the mass ratio of 9.45: 1, accurately weighing 1000 g;
s2, alloying and premelting: pre-melting weighed indium metal ingots and tin metal ingots in a crucible at the temperature of 250 ℃ to form alloy melt with uniform components of indium and tin, and stirring for a plurality of times;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, adding a corresponding number of zirconia balls according to the ball-to-material ratio of 3, and starting electric heating to enable the temperature of the inner cavity of the ball mill to reach 280 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining the rotating speed at 40rpm, simultaneously blowing air into the inner cavity from the air inlet at a linear speed of 0.4m/s, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: after reacting for 3h, stopping heating, ball milling and air blowing, opening a discharge opening to discharge the ITO powder, naturally cooling to a greenhouse, and then placing into a storage bin.
The product ITO composite powder is analyzed and tested for oxygen content to obtain the indium tin oxide (In)2O3+SnO2) More than 92.10 percent, the particle size range of the particle size measured by a laser particle sizer is 1.43-18.27 mu m, the average particle size is 8.06 mu m, wherein the-5.0 mu m accounts for 34 percent.
Example 4
The raw materials of the indium metal ingot and the tin metal ingot were the same as those in example 1.
The embodiment provides a method for preparing ultrafine ITO powder from metal indium and metal tin, a process flow chart of which is shown in the attached figure 1, and the method comprises the following specific steps:
s1, composition design: taking a metal indium ingot and a metal tin ingot according to the mass ratio of 9.45: 1, accurately weighing 1000 g;
s2, alloying and premelting: pre-melting weighed indium metal ingots and tin metal ingots in a crucible at the temperature of 270 ℃ to form alloy melt with uniform components of indium and tin, and stirring for a plurality of times;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, putting a corresponding number of agate balls according to the ball-to-material ratio of 7, and starting electric heating to enable the temperature of the inner cavity of the ball mill to reach 250 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining the rotating speed at 120rpm, simultaneously blowing air into the inner cavity from the air inlet at a linear speed of 1.0m/s, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: after reacting for 2h, stopping heating, ball milling and air blowing, opening a discharge opening to discharge the ITO powder, naturally cooling to a greenhouse, and then placing into a storage bin.
The product ITO composite powder is analyzed and tested for oxygen content to obtain the indium tin oxide (In)2O3+SnO2) More than 99.80 percent, the particle size range of the particle size measured by a laser particle sizer is between 0.02 and 4.6 mu m, the average particle size is 1.37 mu m, wherein 5.0 mu m accounts for 100 percent.
Example 5
The raw materials of the indium metal ingot and the tin metal ingot were the same as those in example 1.
The embodiment provides a method for preparing ultrafine ITO powder from metal indium and metal tin, a process flow chart of which is shown in the attached figure 1, and the method comprises the following specific steps:
s1, composition design: taking a metal indium ingot and a metal tin ingot according to the mass ratio of 9.45: 1, accurately weighing 5000 g;
s2, alloying and premelting: pre-melting weighed indium metal ingots and tin metal ingots in a crucible at the temperature of 300 ℃ to form alloy melt with uniform components of indium and tin, and stirring for a plurality of times;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, putting a corresponding number of zirconia balls according to the ball-to-material ratio of 7, and starting electric heating to enable the temperature of the inner cavity of the ball mill to reach 220 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining the rotating speed at 90rpm, simultaneously blowing air into the inner cavity from the air inlet at a linear speed of 0.7m/s, and starting an oxidation reaction and ball milling; in the hot ball milling oxidation process, the flue gas of the combustion chamber is discharged from a flue gas outlet of the fuel chamber, the flue gas in the reaction inner cavity is discharged through a flue gas filtering outlet arranged in the reaction cavity, and a ceramic filtering plate is arranged at a filtering port, so that the materials in the ball mill can be prevented from being carried out;
s5, cooling and discharging: after reacting for 2.5h, stopping heating, ball milling and air blowing, opening a discharge opening to discharge the ITO powder, naturally cooling to a greenhouse, and then placing into a storage bin.
The product ITO composite powder is analyzed and tested for oxygen content to obtain the indium tin oxide (In)2O3+SnO2) More than 99.20%, the particle size range is 0.35-9.42 μm, the average particle size is 4.72 μm, wherein-5.0 μm accounts for 69%.
Claims (12)
1. A method for preparing ultrafine ITO powder from metal indium and metal tin is characterized in that metal indium ingots and metal tin ingots are used as raw materials, composition design and alloying premelting are firstly carried out, hot ball milling oxidation is carried out in a hot ball mill at the temperature of 100-300 ℃ under the condition of introducing oxidizing gas, so that the metal indium and the metal tin are oxidized in a liquid state, ball milling is carried out simultaneously, and the ultrafine ITO powder is obtained after the hot ball milling oxidation is completed;
wherein the temperature of the alloying premelting is 250-300 ℃.
2. The method for preparing ultrafine ITO powder from metallic indium and metallic tin according to claim 1, wherein the mass ratio of metallic indium ingot to metallic tin ingot in the composition design is 9.45: 1.
3. the method for preparing ultrafine ITO powder of claim 1, wherein the oxidizing gas is air or oxygen.
4. The method for preparing ultrafine ITO powder of claim 1, wherein the blowing linear velocity of the oxidizing gas is 0.1 to 2 m/s.
5. The method for preparing ultrafine ITO powder according to claim 4, wherein the blowing linear velocity of the oxidizing gas is 0.5 to 1.5 m/s.
6. The method for preparing ultrafine ITO powder from metal indium and metal tin according to claim 1, wherein the ball milling strength in the hot ball milling process is 30-120 rpm, the filling rate is 10-50%, and the mass ratio of the ball material is 3-9.
7. The method for preparing ultrafine ITO powder from metallic indium and metallic tin according to claim 6, wherein the filling rate is 20 to 40% and the mass ratio of the ball material is 5 to 8.
8. The method for preparing ultrafine ITO powder according to claim 1, wherein the ball material medium used for ball milling is one of zirconia balls, corundum balls and agate balls.
9. The method for preparing ultrafine ITO powder of claim 8, wherein the ball-milling medium is zirconium oxide.
10. The method for preparing ultrafine ITO powder from metallic indium and metallic tin according to claim 1, wherein the time of the hot ball milling reaction process is 1-5 hours.
11. The method for preparing ultrafine ITO powder from indium metal and tin metal according to claim 10, wherein the time of the hot ball milling reaction process is 1 to 3 hours.
12. The method for preparing ultrafine ITO powder from indium metal and tin metal according to any one of claims 1 to 11, comprising the following steps:
s1, composition design: accurately weighing indium metal ingots and tin metal ingots according to a certain mass proportion;
s2, alloying and premelting: pre-melting the weighed indium metal ingots and tin metal ingots at the temperature of 250-300 ℃ to form alloy melt with uniform components from indium and tin;
s3, alloy melting: adding the alloy melt obtained in the step S2 into a hot ball mill, and starting electric heating to enable the temperature of an inner cavity of the ball mill to reach 100-300 ℃;
s4, hot ball milling oxidation: starting a rotating device, starting a hot ball milling reaction, maintaining a certain rotating speed, simultaneously blowing oxidizing gas into the inner cavity from the gas inlet, and starting an oxidation reaction and ball milling;
s5, cooling and discharging: and after reacting for a certain time, stopping heating, ball milling and blowing oxidizing gas, opening a discharge opening to discharge the ITO powder, completely cooling to a greenhouse, then placing into a storage bin, and grading to obtain ITO powder with different particle sizes.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6018737B2 (en) * | 1979-04-06 | 1985-05-11 | 松下電器産業株式会社 | electrical contact materials |
| CN103590072A (en) * | 2013-10-17 | 2014-02-19 | 清远先导材料有限公司 | Preparation method of high-purity indium |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN108002428A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | It is a kind of that the preparation method with ITO particles and the ITO particles by this method preparation is deposited |
| CN108557770A (en) * | 2018-06-21 | 2018-09-21 | 常熟理工学院 | A method of preparing nanometer metal oxide powder |
-
2018
- 2018-10-09 CN CN201811187676.0A patent/CN109231259B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6018737B2 (en) * | 1979-04-06 | 1985-05-11 | 松下電器産業株式会社 | electrical contact materials |
| CN103590072A (en) * | 2013-10-17 | 2014-02-19 | 清远先导材料有限公司 | Preparation method of high-purity indium |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN107794389A (en) * | 2017-10-20 | 2018-03-13 | 温州宏丰电工合金股份有限公司 | A kind of silver-tin oxide or indium oxide contact material and preparation method thereof |
| CN108002428A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | It is a kind of that the preparation method with ITO particles and the ITO particles by this method preparation is deposited |
| CN108557770A (en) * | 2018-06-21 | 2018-09-21 | 常熟理工学院 | A method of preparing nanometer metal oxide powder |
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