CN101392362A - Method for preparing ITO target from nano homogeneous ITO powder - Google Patents
Method for preparing ITO target from nano homogeneous ITO powder Download PDFInfo
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- CN101392362A CN101392362A CNA2008102307790A CN200810230779A CN101392362A CN 101392362 A CN101392362 A CN 101392362A CN A2008102307790 A CNA2008102307790 A CN A2008102307790A CN 200810230779 A CN200810230779 A CN 200810230779A CN 101392362 A CN101392362 A CN 101392362A
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Abstract
The invention discloses a method for preparing an ITO target by the use of nano-homogeneous ITO powder. Metal indium or tin with the purity of 4N to 5N is prepared; In2O3 and SnO2 with the proportion of 9 to 1 are added into a melter to be melted at the temperature of 250 DEG C to 500 DEG C through electric heating; In2O3 and SnO2 are then compressed into a reactor with the voltage of 50V to 1000V and the current of 50A to 1000A; the mixture of nitrogen and oxygen or pure oxygen is pumped into the reactor and followed by fast cooling with cooling air or liquid nitrogen to form single-phase nano-ITO powder to which tin oxide is fully soluble into indium oxide lattice. Dry pressing and blanking are carried out under the pressure of 20MPa; the cold isostatic compaction is followed under the pressure of 200MPa to 300MPa to obtain an ITO mold which is then put into a high temperature oxygen-atmosphere sintering furnace in which pure oxygen is pumped; and the ITO mold is sintered for 6h to 40h under the pressure of 0.1MPa to 1.0MPa and the high temperature of 1450 DEG C to 1650 DEG C to form the ITO target. The prepared ITO target has high purity and crystallinity, good dispersity and strong liquidity.
Description
Technical field
The invention belongs to technical field of nano material, in particular for the method for a kind of preparing ITO target from nano homogeneous ITO powder of indicating meter transparent conductive film and special glass ITO sputtering target.
Background technology
So-called ITO (Indium-Tin-Oxide) is meant the composite oxides of Indium (indium) and Tin (tin).Having good transmittance, electroconductibility and high infrared reflection rate etc. by the ITO target through the ito thin film of magnetron sputtering preparation, is very important electron functional materials of information industry.Be mainly used in following three big fields:
1) display industry is as LCD liquid-crystal display, PDP plasma display, inorganic EL and OLED display.
2) solar cell;
3) features glass is as infrared reflection glass, uvioresistant glass, light shield and glass disk etc.
The ITO target preparation method who extensively adopts mainly contains two kinds at present:
A kind of is to adopt indium oxide powder and stannic oxide powder to carry out the ball milling mechanically mixing according to a certain percentage, mixes aftershaping, carries out sintering then and makes the ITO target.
Another kind is to adopt chemical precipitation method to prepare biphase ITO powder mix, and through high-temperature calcination, the secondary ball milling fragmentation makes the ITO powder, and moulding is then carried out sintering and made the ITO target.
Patent of invention CN1412342A " sputtering target " joins the stannic oxide powder of the indium oxide powder of 90 weight % and 10 weight % and dispersion agent, tackiness agent and ion exchanged water to carry out ball milling in the nylon spherical tank unshakable in one's determination and mix, and makes base substrate by isostatic cool pressing (CIP) then.Then, the sintering oven that this base substrate is placed on pure oxygen atmosphere carries out sintering and makes the ITO target.This method may there are the following problems:
1) ITO target general requirement is high-purity, reaches 4N (99.99%).This invention will make Indium sesquioxide and stannic oxide thorough mixing, needs to add dispersion agent, tackiness agent, and mixes through long ball milling, and this may cause sneaking into of impurity, thereby reduces the quality of ITO target.
2) in order to make the ITO target have excellent conductivity, final ITO target requires to be the single-phase crystalline structure of body-centred cubic Indium sesquioxide that promptly stannic oxide must be solidly soluted in the Indium sesquioxide body-centered cubic crystal structure fully.Indium sesquioxide and two kinds of mechanical mixturies that mix of stannic oxide are adopted in this invention, can cause solid solution diffusion difficulty in the sintering process.
Patent of invention CN03118371.9 " indium-tin oxide target material preparation method " has explained the method that chemical coprecipitation prepares the ITO powder, be the high pure metal indium is dissolved in hydrochloric acid and mixes with a certain proportion of tin chloride, add additive citric acid, urea etc., obtain the ITO presoma through homogeneous coprecipitation, with unwanted other ions of the pure water flush away overwhelming majority, elimination moisture under vacuum, and use pure water drip washing, use ethanol drip washing at last, oven dry makes throw out remain dispersity particle preferably, by calcining in 600 ℃ of tunnel furnace, and in 500 ℃ of nitrogen atmosphere reduction furnaces, reduce deoxidation, then this powder is carried out the pressed compact sintering and make the ITO target.There are the following problems for this method:
Production process is long, the Cl in the finished product
-Be not easy to get rid of in negative ion, foreign matter content is difficult to control; Be difficult to form monophasic ito powder, product is the mechanical mixture of Indium sesquioxide and stannic oxide, can cause solid solution diffusion difficulty in the sintering process, influences the conductivity of final ITO target.
Summary of the invention
For the two-phase structure that overcomes present ITO powder is difficult to solid solution in sintering process, cause that electroconductibility is not high, shortcomings such as impurity are sneaked in chemical method powder process easily, the invention provides a kind of method of preparing ITO target from nano homogeneous ITO powder, the nanometer homogeneous phase ITO powder prepared according to this method has the single-phase indium oxide crystal structure of the complete solid solution of stannic oxide, has high purity, high crystalline, good dispersity, mobile characteristics such as strong, after making base substrate with nanometer homogeneous phase ITO powder again, under oxygen atmosphere, carry out sintering, the ITO target that obtained performance is good.
For achieving the above object, the present invention adopts following technical scheme:
The method of described preparing ITO target from nano homogeneous ITO powder comprises batching, preparation nanometer homogeneous phase ITO powder, three steps of preparation ITO target, and three step divisions are as follows:
I, batching
Get the indium metal or the metallic tin of purity 4～5N (purity is 99.99～99.999%), press In
2O
3: SnO
2=9: 1 batching proportion is prepared burden, and batching is joined in the melting tank, and energising is heated to about 250～500 ℃ melts;
II, preparation nanometer homogeneous phase ITO powder
The indium stannum alloy of fusing is pressed into reactor, add 50～1000V voltage, 50-1000A electric current to reactor, and in reactor, feed nitrogen oxygen atmosphere or pure oxygen make its become gasiform indium, tin atom and and the Sauerstoffatom reaction, under resistance heat and strong magnetic field action, the indium stannum alloy of fusing is atomized, gasification, oxidation, cool off fast through cold wind or liquid nitrogen again, formation has the single phase nano ITO powder that stannic oxide is solidly soluted into the Indium sesquioxide lattice fully, open and receive powder system, make nanometer homogeneous phase ITO powder, the nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure;
III, preparation ITO target
With above-mentioned nanometer homogeneous phase ITO powder is that raw material is at dry-pressing base under the 20MPa pressure and carry out cold isostatic compaction and make the ITO base substrate under 200～300MPa pressure; The high temperature oxygen atmosphere sintering oven of again the ITO base substrate being packed into feeds pure oxygen then, under the air pressure of pressure 0.1～1.0MPa and the ITO target that sintering 6～40h obtains being fired under 1450～1650 ℃ of high temperature.
Because adopt aforesaid technical scheme, the present invention has following superiority:
1, nanometer homogeneous phase ITO powder of the present invention has single body centred cubic crystal In through X-ray diffraction analysis
2O
3Structure, having omitted conventional Indium sesquioxide and stannic oxide needs long-time ball milling to mix, the problem that is not easy to mix and be easy to generate problem such as contaminating impurity.
2, nanometer homogeneous phase ITO powder of the present invention is based on the preparation of physical vapor method, has high purity, and high crystalline, polymolecularity, mobile strong do not contain acid radical anion in the powder.
3, nanometer homogeneous phase ITO powder of the present invention has quickened the solid solution diffusion in the ITO target sintering process, makes sintering process be more prone to control.
4, nanometer homogeneous phase ITO powder of the present invention is through granularity Detection, and specific surface area is 8～40m
2/ g (GB/T19587 gas adsorption BET method is measured the solid matter specific surface area), median size≤100nm.
5, the present invention utilizes the performance of the ITO target that homogeneous phase ITO powder fires to be: purity 99.99%, and relative density 〉=99%, resistivity is 1.5～1.7 * 10
-4Ω cm, grain fineness number 2～10 μ m.
Embodiment
Embodiment 1:
1, batching
Get high pure metal indium and the high pure metal tin of 4N, press In
2O
3: SnO
2=9: 1 ratio of components refetches indium metal 80.43% and metallic tin 9.57% is prepared burden, and batching is joined in the melting tank, and energising is heated to about 400 ℃ melts.
2, preparation nanometer homogeneous phase ITO powder
The indium stannum alloy of fusing is pressed into reactor, add 100V voltage, 500A electric current to reactor, and in reactor, feed nitrogen oxygen atmosphere, indium, the tin that gasifies is carried out cold wind to be cooled off fast, open and receive powder system, make nanometer homogeneous phase ITO powder, the nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure.
3, preparation ITO target
With above-mentioned homogeneous phase ITO powder is that raw material carries out dry-pressing base under the 20MPa pressure, carries out cold isostatic compaction and make the ITO base substrate under 200MPa pressure.With the ITO base substrate high temperature oxygen atmosphere sintering oven of packing into, feed pure oxygen, under the air pressure of absolute pressure 0.1MPa and 1550 ℃ of high temperature sintering 20h be fired into the ITO target.
The performance of prepared nanometer homogeneous phase ITO powder sees Table 1.
The performance of table 1 nanometer homogeneous phase ITO powder
| The name of an article | In 2O 3： SnO 2 | Median size nm | Specific surface area m 2/g | Purity | Dispersed |
| ITO | 9：1 | 30 | 20 | > 99.99％ | Hard aggregation-free |
The performance of prepared ITO target is: purity is 99.99%, and relative density 99.5%, resistivity are 1.6 * 10
-4Ω cm, grain fineness number 5～8 μ m.Embodiment 2:
1, batching
Get high pure metal indium and the 5N high pure metal tin of 4N, press In
2O
3: SnO
2=9: 1 ratio of components refetches indium metal 80.43% and metallic tin 9.57% is prepared burden, and indium and the tin for preparing material is joined in the melting tank, and energising is heated to about 500 ℃ melts.
2, preparation nanometer homogeneous phase ITO powder
The indium stannum alloy of fusing is pressed into reactor, add 500V voltage, 200A electric current to reactor, and in reactor, feed nitrogen oxygen atmosphere, indium, the tin that gasifies is carried out cold wind to be cooled off fast, open and receive powder system, make nanometer homogeneous phase ITO powder, the nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure.
3, preparation ITO target
With above-mentioned homogeneous phase ITO alloy powder is that raw material carries out dry-pressing base under the 20MPa pressure, carries out cold isostatic compaction under the 200MPa pressure, makes the ITO base substrate.With the ITO base substrate high temperature oxygen atmosphere sintering oven of packing into, feed pure oxygen, 1600 ℃ of high temperature sintering 6h are fired into the ITO target under the air pressure of absolute pressure 0.1MPa.
The performance of prepared nanometer homogeneous phase ITO powder sees Table 2.
The performance of table 2 nanometer homogeneous phase ITO powder
| The name of an article | In 2O 3： SnO 2 | Median size nm | Specific surface area m 2/g | Purity | Dispersed |
| ITO | 9：1 | 35 | 22 | > 99.99％ | Hard aggregation-free |
The performance of prepared ITO target is: purity is 99.99%, and relative density 99.5%, resistivity are 1.62 * 10
-4Ω cm, grain fineness number 5～8 μ m.
Embodiment 3:
1, batching
Get high pure metal indium and the high pure metal tin of 5N, press In
2O
3: SnO
2=9: 1 ratio of components refetches indium metal 80.43% and metallic tin 9.57% is prepared burden, and indium and the tin for preparing material is joined in the melting tank, and energising is heated to about 400 ℃ melts.
2, preparation nanometer homogeneous phase ITO powder
The indium stannum alloy of fusing is pressed into reactor, add 800V voltage, 50A electric current to reactor, and in reactor, feed nitrogen oxygen atmosphere, indium, the tin that gasifies is carried out cold wind to be cooled off fast, open and receive powder system, make nanometer homogeneous phase ITO powder, the nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure.
3, preparation ITO target
With above-mentioned homogeneous phase ITO alloy powder is that raw material carries out dry-pressing base under the 20MPa pressure, carries out cold isostatic compaction under the 200MPa pressure, makes the ITO base substrate.With the ITO base substrate high temperature oxygen atmosphere sintering oven of packing into, feed pure oxygen, 1550 ℃ of high temperature sintering 20h are fired into the ITO target under the air pressure of absolute pressure 0.5MPa.
The performance of prepared nanometer homogeneous phase ITO powder sees Table 3.
The performance of table 3 nanometer homogeneous phase ITO powder
| The name of an article | In 2O 3： SnO 2 | Median size nm | Specific surface area m 2/g | Purity | Dispersed |
| ITO | 9：1 | 40 | 25 | > 99.999％ | Hard aggregation-free |
The performance of prepared ITO target is: purity is 99.99%, and relative density 99.5%, resistivity are 1.59 * 10
-4Ω cm, grain fineness number 3～6 μ m.
Claims (1)
1, a kind of method of preparing ITO target from nano homogeneous ITO powder is characterized in that: this method comprises batching, preparation nanometer homogeneous phase ITO powder, three steps of preparation ITO target, and three step divisions are as follows:
I, batching
Get the indium metal or the metallic tin of purity 4～5N (purity is 99.99～99.999%), press In
2O
3: SnO
2=9: 1 batching proportion is prepared burden, and batching is joined in the melting tank, and energising is heated to about 250～500 ℃ melts;
II, preparation nanometer homogeneous phase ITO powder
The indium stannum alloy of fusing is pressed into reactor, add 50～1000V voltage, 50-1000A electric current to reactor, and in reactor, feed nitrogen oxygen atmosphere or pure oxygen make its become gasiform indium, tin atom and and the Sauerstoffatom reaction, under resistance heat and strong magnetic field action, the indium stannum alloy of fusing is atomized, gasification, oxidation, cool off fast through cold wind or liquid nitrogen again, formation has the single phase nano ITO powder that stannic oxide is solidly soluted into the Indium sesquioxide lattice fully, open and receive powder system, make nanometer homogeneous phase ITO powder, the nano-ITO powder has single In through the X-ray diffraction facies analysis
2O
3Body-centered cubic crystal structure;
III, preparation ITO target
With above-mentioned nanometer homogeneous phase ITO powder is that raw material is at dry-pressing base under the 20MPa pressure and carry out cold isostatic compaction and make the ITO base substrate under 200～300MPa pressure; The high temperature oxygen atmosphere sintering oven of again the ITO base substrate being packed into feeds pure oxygen then, under the air pressure of pressure 0.1～1.0MPa and the ITO target that sintering 6～40h obtains being fired under 1450～1650 ℃ of high temperature.
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|---|---|---|---|
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812665A (en) * | 2010-03-26 | 2010-08-25 | 北京化工大学 | Method for preparing indium tin oxide (ITO) target material with single-phase structure and high density |
| CN102173817A (en) * | 2011-01-30 | 2011-09-07 | 河北鹏达新材料科技有限公司 | Method for preparing indium tin oxide (ITO) target |
| CN101786885B (en) * | 2009-12-24 | 2012-09-26 | 中国船舶重工集团公司第七二五研究所 | Method for controlling grain size to produce ITO target |
| CN106676488A (en) * | 2016-12-27 | 2017-05-17 | 深圳市三鑫精美特玻璃有限公司 | Magnetron sputtering based production technology of NiO electrochromic film and glass |
| JP2018006685A (en) * | 2016-07-07 | 2018-01-11 | Ｊｘ金属株式会社 | Indium target member and method of manufacturing the same |
| CN109267009A (en) * | 2018-08-31 | 2019-01-25 | 株洲火炬安泰新材料有限公司 | A kind of low-temperature resistance high resistivity ITO conduction membrane preparation method |
| CN112479682A (en) * | 2020-12-15 | 2021-03-12 | 株洲火炬安泰新材料有限公司 | Preparation method of environment-friendly and efficient ITO target material |
| CN113321238A (en) * | 2021-06-04 | 2021-08-31 | 昆明理工大学 | Preparation method of nano ITO powder |
| CN114436642A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of indium tin oxide alloy target material |
| CN114457314A (en) * | 2021-09-29 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tantalum target material |
| CN114457319A (en) * | 2021-09-30 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tungsten target material |
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2008
- 2008-10-30 CN CNA2008102307790A patent/CN101392362A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786885B (en) * | 2009-12-24 | 2012-09-26 | 中国船舶重工集团公司第七二五研究所 | Method for controlling grain size to produce ITO target |
| CN101812665A (en) * | 2010-03-26 | 2010-08-25 | 北京化工大学 | Method for preparing indium tin oxide (ITO) target material with single-phase structure and high density |
| CN102173817A (en) * | 2011-01-30 | 2011-09-07 | 河北鹏达新材料科技有限公司 | Method for preparing indium tin oxide (ITO) target |
| JP2018006685A (en) * | 2016-07-07 | 2018-01-11 | Ｊｘ金属株式会社 | Indium target member and method of manufacturing the same |
| CN106676488A (en) * | 2016-12-27 | 2017-05-17 | 深圳市三鑫精美特玻璃有限公司 | Magnetron sputtering based production technology of NiO electrochromic film and glass |
| CN109267009A (en) * | 2018-08-31 | 2019-01-25 | 株洲火炬安泰新材料有限公司 | A kind of low-temperature resistance high resistivity ITO conduction membrane preparation method |
| CN114436642A (en) * | 2020-11-06 | 2022-05-06 | 湖南七点钟文化科技有限公司 | Preparation method of indium tin oxide alloy target material |
| CN112479682A (en) * | 2020-12-15 | 2021-03-12 | 株洲火炬安泰新材料有限公司 | Preparation method of environment-friendly and efficient ITO target material |
| CN113321238A (en) * | 2021-06-04 | 2021-08-31 | 昆明理工大学 | Preparation method of nano ITO powder |
| CN114457314A (en) * | 2021-09-29 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tantalum target material |
| CN114457319A (en) * | 2021-09-30 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tungsten target material |
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