CN100554204C - The preparation method of nanometer grade indium tin oxide composite powder - Google Patents
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Abstract
The present invention is a kind of technology for preparing the nano-scale indium and tin oxides composite granule with coprecipitation method, be characterized in utilizing the inorganic single strong acid or the mixed strong acids aqueous solution dissolution of metals indium, metallic tin respectively, or soluble metal indium salt and metal pink salt are dissolved in the water, two solution of preparation are mixed, under violent stirring mixing solutions condition, add precipitation agent and produce indium tin coprecipitate, through the washing, organic solvent is washed with solid-liquid separation after, add organic solvent and carry out component distillation, the filter cake drying, break up, calcine and make ultra-fine ITO composite granule.The ITO target relative theory density that the tin indium oxide powder of prepared of the present invention is fired through simple technology reaches more than 99%.
Description
Technical field
The present invention is a kind of method for preparing nanometer grade indium tin oxide composite powder (ITO) with coprecipitation method.The ITO composite granule that makes with present method is applicable to that preparation light function shows the ITO target that plated film is used.
Background technology
Ito powder is the raw material of preparation ITO sputtering coating target, wishes to get high-quality, highdensity ITO sputtering target material, then needs to form ultrapure ultra-fine ito powder uniformly.
Traditional method for preparing ito powder: the one, Indium sesquioxide is mixed with mechanical means with the powder of stannic oxide, obtain through calcining again.Because the particulate agglomeration, make that the degree that mixes of different oxide compounds is limited in the ito powder, influence the quality of ITO target, so influence ito thin film electroconductibility, light transmission and with the tack of substrate.The method that another kind is used to prepare the ultra micro composite powder is an aqua-solution method.Blended contained in indium and the tin ion metal salt solution add precipitation agent,, after reaction, can obtain the precipitation of various uniform component phase composites, heat-treat again and obtain ultra-fine ITO particle because dissociated ion is to exist in solution with homogeneous phase.For obtaining to make the ito powder of high density ITO target sintered compact, Chinese patent CN130595A discloses a kind of preparation method of indium tin oxide composite powder, this method is dissolved emulsification respectively with indium metal, tin, through mixing, co-precipitation, washing, filtration, oven dry, calcination, quenching at last grinds, product.This method makes narrow diameter distribution easily, and chemical ingredients evenly and the ultra-fine grain of good fluidity.But this method process complexity, adding additive during emulsification can influence degree of purity of production.CN1412117A has announced a kind of method for preparing the tin indium oxide powder with aqua-solution method, mainly be to dissolve indium compound, tin compound respectively in water, add suitable additives again, produce metal hydroxides, after filtration, after the washing, add suitable additives again and give dispergation, high quality nanometer level tin indium oxide powder is made in drying and calcining.But the particles dispersed that this method makes is not really desirable, and particle diameter generally can reach 96% with the density of the target of this ITO powder preparing more than 100nm, be difficult to satisfy the requirement of high performance thin film plated film.
Summary of the invention
The present invention can overcome aqua-solution method and prepare in the ITO powder process additive to the influence of purity, solve the control and the scattering problem of superfine powder grain graininess, a kind of particle diameter is even, controlled, fluffy, plant-scale nano level high purity ITO composite granule preparation method of good dispersity thereby provide.
Main technical schemes of the present invention: with indium, tin metal or indium, tin metal soluble salt is feedstock production or preparation mixing solutions, through co-precipitation, washing foreign ion, organic solvent wash, adding exists the organic solvent of ternary azeotrope to carry out component distillation with water and ethanol after the solid-liquid separation, drying, break up, calcine and obtain the ITO composite granule.
Above-mentioned is the feedstock production mixing solutions with indium, tin metal, be indium metal, tin to be dissolved in respectively in the acid solution mix then, wherein the purity of indium, tin metal is greater than 99.99%, acid solution is the aqueous solution of purity more than or equal to the pure concentrated nitric acid of top grade, the vitriol oil and/or concentrated hydrochloric acid, preferred concentrated nitric acid, the vitriol oil, concentrated hydrochloric acid any two kinds or three kinds of mixed aqueous solution.
Above-mentioned is the preparation of raw material mixing solutions with indium, tin metal salt, is purity is dissolved in back mixing in the deionized water respectively more than or equal to top grade pure solubility indium salt and pink salt.
Above-mentioned co-precipitation is meant that adding purity under the situation of the mixing solutions that stirs preparation or preparation produces indium, tin coprecipitate more than or equal to the pure mixing solutionss such as neutralizing agent yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium hydroxide, potassium hydroxide, hydrated barta, lithium hydroxide or urea of top grade to alkalescence.
Above-mentioned washing is with the deionized water wash of resistance greater than 10M Ω .CM, and it is more than or equal to analytically pure anhydrous methanol or ethanol or acetone with purity that organic solvent is washed.
The organic solvent that above-mentioned distillation adds is: purity is more than or equal to the pure ethyl acetate of top grade, fluoroacetic acid ethyl ester, triethylamine, isopropylcarbinol, Pentyl alcohol, n-hexyl alcohol, n-Heptyl alcohol, hexalin, butanols, tetracol phenixin etc.
Above-mentioned azeotropic distillation process control principle is: the organic solvent that adds when making the component that distills at last be distillation.
Effect of the present invention: by stirring and distilling and to control particulate globule size and dispersiveness effectively, adopt adding and water and ethanol to have the organic solvent azeotropic distillation of ternary azeotrope, water in the co-precipitation of ITO composite granule precursor distills prior to organic solvent, eliminated that agglomeration takes place the existence owing to hydrogen bond between the particle, thereby make the powder granule good dispersity that makes, particle diameter is controlled between 10nm--40nm, BET specific surface area 30～60m
2/ g; The ITO target relative theory density of firing through simple technology with the ITO composite granule of present method preparation reaches more than 99%; And the inventive method dissolution process can not heat, and has reduced emulsifying process, need not add other additives, has simplified technological process and technological process is controlled easily; Reduce cost, adopted common chemical industry equipment, be easy to suitability for industrialized production.
Description of drawings:
Fig. 1 is the transmission electron microscope photo of the powder of present method preparation.
Fig. 2 is the XRD figure of the powder of present method preparation.
Embodiment
The concrete implementation step of method of the present invention:
(1) be feedstock production or preparation mixing solutions with indium, tin metal or indium, tin soluble metal salt: be that indium metal and metallic tin are dissolved in purity respectively more than or equal to back mixing in the aqueous solution of the pure concentrated nitric acid of top grade, the vitriol oil or concentrated hydrochloric acid, or indium metal and metallic tin be dissolved in purity more than or equal to the pure concentrated nitric acid of top grade, the vitriol oil and concentrated hydrochloric acid any two kinds or three kinds of mixed aqueous solution, wherein indium metal, tin purity are greater than 99.99%, and the add-on of indium metal, tin is according to Indium sesquioxide and stannic oxide mass percent In after converting in the mixing solutions
2O
3: SnO
2Add at=90: 10; Or purity is dissolved into respectively in the deionized water of resistance greater than 10M Ω .CM more than or equal to top grade pure soluble metal indium salt and pink salt, thorough mixing, used indium salt and pink salt be In (NO normally
3)
3, In
2(SO
4)
3, InCl
3, Sn (NO
3)
4, Sn (SO
4)
2, SnCl
4Deng, the add-on of indium salt and pink salt is according to Indium sesquioxide and stannic oxide mass percent In after converting in the mixing solutions
2O
3: SnO
2Add at=90: 10.
(2) adding purity under the situation of the mixing solutions that stirs preparation or preparation makes mixing solutions produce indium, tin oxyhydroxide or carbonate coprecipitation to alkalescence more than or equal to top grade pure neutralizing agent yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium hydroxide, potassium hydroxide, hydrated barta, lithium hydroxide or urea etc.; Filter after scouring, washing comprises with resistance washes greater than deionized water washing and the organic solvent of 10M Ω .CM, and the organic solvent washing uses purity commonly used more than or equal to analytically pure methyl alcohol or ethanol or acetone.
(3) add the organic solvent azeotropic distillation; Organic solvent is selected from purity more than or equal to the pure ethyl acetate of top grade, fluoroacetic acid ethyl ester, triethylamine, isopropylcarbinol, Pentyl alcohol, n-hexyl alcohol, n-Heptyl alcohol, hexalin, butanols, tetracol phenixin etc.Distil process control principle is that the component that distills at last is the organic solvent that adds.
(4) under 40 ℃～160 ℃, carried out drying 2～24 hours; Under 350 ℃～1000 ℃, calcined 2～8 hours, make nano level ITO composite granule.
The present invention adopts and stirs and distillation, and make that grain diameter is controlled, solved the agglomeration traits between the particle, the good dispersity of product, particle diameter is controlled in the 10nm--40nm scope; The ITO composite granule electromicroscopic photograph of the present invention preparation as shown in Figure 1, ITO composite granule thing is met each other shown in Figure 2 for single indium trioxide mutually.The target relative theory density of firing with the nano level ITO composite granule of present method preparation reaches more than 99%.
Embodiment 1:
A. get 22.964 gram indium metal (purity 99.99%) and be dissolved in the pure aqueous nitric acid of top grade, get 7.02 gram SnCl
45H
2O (purity 99.99%) is dissolved in proper amount of deionized water.
B. above-mentioned two kinds of solution thorough mixing are stirred, add proper amount of deionized water, indium, tin ion concentration are 0.8M in the mixing solutions at this moment.
C. under violent stirring mixing solutions condition, add the pure sodium bicarbonate of top grade, making the pH value of solution value is 7～11, and at this moment clear soln produces indium tin coprecipitate, continues to stir 2 hours.
D. filter supernatant liquid with the centrifugal settling mode, obtain indium tin coprecipitate filter cake again with deionized water agitator treating again, washing is to there not being NO
3 -, Na
+And Cl
-Ion filters the back the last time and adds analytically pure anhydrous methanol.
E. with after the anhydrous methanol washing three times, add the pure butanols violent stirring of top grade again after, 64 ℃ of beginning component distillations obtain indium tin hydroxide.
F. indium tin hydroxide is placed 10 hours dryings down for 30 ℃～150 ℃ at oven temperature, break up then.
G. the indium tin hydroxide after will breaing up is put into retort furnace, is incubated 4 hours down at 780 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 16nm, BET specific surface area 42m
2/ g
Embodiment 2:
A. get 55.113 gram indium metal (purity 99.99%) and be dissolved in the pure aqueous nitric acid of top grade, get 5.832 gram metallic tins (purity 99.99%) and be dissolved in the pure aqueous sulfuric acid of top grade.
B. above-mentioned two kinds of solution thorough mixing are stirred, add proper amount of deionized water, indium, tin ion concentration are 0.4M in the solution at this moment.
C. under violent stirring mixing solutions condition, add the pure volatile salt of top grade, making the pH value of solution value is 7～11, and at this moment clear soln produces indium tin coprecipitate, continues to stir 2 hours.
D. filter supernatant liquid with the centrifugal settling mode, obtain indium tin coprecipitate filter cake again with deionized water agitator treating again, washing is to there not being NO
3 -, NH
4 +And SO
4 2-Ion filters the back the last time and adds the analytical pure dehydrated alcohol.
E. with behind the absolute ethanol washing, add the pure isopropylcarbinol violent stirring of top grade again after, under 78 ℃ of conditions of temperature, begin component distillation, obtain indium tin coprecipitate.
F. indium tin hydroxide is placed 12 hours down to complete drying 30 ℃～130 ℃ of oven temperatures.Break up then.
G. the indium tin hydroxide after will breaing up is put into retort furnace, and temperature is incubated 5 hours down at 820 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 10nm, BET specific surface area 58m
2/ g.
Embodiment 3:
A. get 55.113 gram indium metal (purity 99.99%) and be dissolved in the pure nitric acid of top grade and the mixed in hydrochloric acid aqueous solution, get 5.832 gram metallic tins (purity 99.99%) and be dissolved in the pure aqueous sulfuric acid of top grade.
B. above-mentioned two kinds of solution thorough mixing are stirred, add proper amount of deionized water, indium, tin ion concentration are 0.5M in the solution at this moment.
C. under violent stirring mixing solutions condition, adding the pure bicarbonate of ammonia of top grade, making the pH value of solution value is 7～11, and at this moment clear soln produces indium tin coprecipitate, continues to stir 2 hours.
D. filter supernatant liquid with the centrifugal settling mode, the indium tin coprecipitate filter cake that obtains white is again with deionized water agitator treating again, and repeated washing is to there not being NO
3 -, NH
4 +And SO
4 2-Ion filters the back the last time and adds analytically pure acetone.
E. after using washing with acetone five times, add analytically pure n-Heptyl alcohol violent stirring again after, at 56 ℃ of beginnings of temperature component distillation, obtain indium tin coprecipitate.
F. indium tin coprecipitate was placed 10 hours down for 50 ℃～120 ℃ at oven temperature.Break up then.
G. the indium tin coprecipitate after will breaing up is put into retort furnace, and temperature is incubated 4 hours down at 900 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 14nm, BET specific surface area 50m
2/ g.
Embodiment 4:
A. get 55.113 gram indium metal (purity 99.99%) and be dissolved in the pure aqueous nitric acid of top grade, get 5.832 gram metallic tins (purity 99.99%) and be dissolved in the pure sulfuric acid of top grade and the mixed in hydrochloric acid aqueous solution.
B. above-mentioned two kinds of solution thorough mixing are stirred, add proper amount of deionized water, indium, tin ion concentration are 2.3M in the solution at this moment.
C. under violent stirring mixing solutions condition, add the pure urea of top grade, making the pH value of solution value is 7～11, and at this moment clear soln produces white indium tin coprecipitate, continues to stir 2 hours.
D. the centrifugal settling mode is filtered supernatant liquid, and the indium tin coprecipitate filter cake that obtains white is again with deionized water agitator treating again, and repeated washing filters the back the last time and adds the analytical pure anhydrous methanol to there not being other ion.
E. with after the anhydrous methanol washing three times, add the pure Pentyl alcohol violent stirring of top grade again after, at 64 ℃ of beginnings of temperature component distillation, obtain indium tin coprecipitate.
F. indium tin coprecipitate was placed 8 o'clock down for 40 ℃～80 ℃ at oven temperature.Break up then.
G. indium tin coprecipitate is put into retort furnace, temperature is incubated 6 hours down at 470 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 20nm, BET specific surface area 38m
2/ g.
Embodiment 5:
A. get 551.13 gram indium metal (purity 99.99%) and be dissolved in the pure aqueous nitric acid of top grade, get 58.32g metallic tin (purity 99.99%) and be dissolved in the pure aqueous hydrochloric acid of top grade.
B. will dissolve two kinds of good solution and mix, and add appropriate amount of deionized water, indium, tin ion concentration are the mixing solutions of 1.2M in the wiring solution-forming.
C. under violent stirring mixing solutions condition, add the pure sodium hydroxide of top grade, make pH value reach 7～11, produce indium tin coprecipitate, continue to stir 2 hours.
D. cross cleaner liquid, obtain indium tin coprecipitate filter cake again with deionized water agitator treating again, repeated washing filters the back the last time and adds the analytical pure anhydrous methanol to there not being other ion.
E. with after the anhydrous methanol washing three times, add the pure n-hexyl alcohol violent stirring of top grade again after, at 64 ℃ of beginnings of temperature component distillation, obtain indium tin indium tin coprecipitate.
F. indium tin indium tin coprecipitate was placed 10 hours down for 40 ℃～140 ℃ at oven temperature.Break up then.
G. indium tin indium tin coprecipitate is put into retort furnace, temperature is incubated 5 hours down at 450 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 25nm, BET specific surface area 32m
2/ g.
Embodiment 6:
A. get 1.435 kilograms of indium metal (purity 99.99%) and be dissolved in the pure concentrated nitric acid aqueous solution of top grade, get 0.451 kilogram of SnCl that top grade is pure
45H
2O is dissolved in the deionized water.
B. will dissolve two kinds of good solution and mix, and add appropriate amount of deionized water, indium, tin ion concentration are the mixing solutions of 1.4M in the wiring solution-forming, fully stir.
C. under violent stirring mixing solutions condition, add the pure ammoniacal liquor of top grade, make pH value reach 7～11, produce indium tin coprecipitate, continue to stir 4 hours.
D. obtain indium tin coprecipitate filter cake again with deionized water agitator treating again after filtering, repeated washing filters the back the last time and adds analytically pure anhydrous propanone to there not being other ion.
E. with after the anhydrous propanone washing three times, add the pure triethylamine violent stirring of top grade again after, at 56 ℃ of beginnings of temperature component distillation, obtain indium tin coprecipitate.
F. indium tin coprecipitate was placed 10 hours down for 50 ℃～150 ℃ at oven temperature.Break up then.
G. indium tin indium tin coprecipitate is put into retort furnace, temperature is incubated 3 hours down at 520 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 25nm, BET specific surface area 32m
2/ g.
Embodiment 7:
A. get 5.5113 kilograms of indium metal (purity 99.99%) and be dissolved in the pure concentrated nitric acid aqueous solution of top grade, get 0.5832 kilogram of metallic tin (purity 99.99%) and be dissolved in the pure concentrated sulfuric acid aqueous solution of top grade.
B. will dissolve two kinds of good solution and mix, and add appropriate amount of deionized water, indium, tin ion concentration are the mixing solutions of 1.4M in the wiring solution-forming, fully stir.
C. under violent stirring mixing solutions condition, add the pure yellow soda ash of top grade, make pH value reach 7～11, produce indium tin coprecipitate, continue to stir 2 hours.
D. obtain indium tin coprecipitate filter cake again with deionized water agitator treating again after filtering, repeated washing filters the back the last time and adds analytically pure dehydrated alcohol to there not being other ion.
E. after using absolute ethanol washing three times, add the pure ethyl acetate violent stirring of top grade again after, at 56 ℃ of beginnings of temperature component distillation, obtain indium tin coprecipitate.
F. indium tin coprecipitate was placed 10 hours down for 40 ℃～150 ℃ at oven temperature.Break up then.
G. indium tin indium tin coprecipitate is put into retort furnace, temperature is incubated 4 hours down at 860 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 27nm, BET specific surface area 30m
2/ g.
Embodiment 8:
A. get 2.87 kilograms of indium metal (purity 99.99%) and be dissolved in the pure concentrated nitric acid aqueous solution of top grade, get 0.902 kilogram of SnCl that top grade is pure
45H
2O is dissolved in the deionized water.
B. will dissolve two kinds of good solution and mix, and add appropriate amount of deionized water, indium, tin ion concentration are the mixing solutions of 1.1M in the wiring solution-forming, fully stir.
C. under violent stirring mixing solutions condition, add the pure urea of top grade, make pH value reach 7～11, produce indium tin coprecipitate, continue to stir 2 hours.
D. obtain indium tin coprecipitate filter cake again with deionized water agitator treating again after filtering, repeated washing filters the back the last time and adds analytically pure dehydrated alcohol to there not being other ion.
E. after using absolute ethanol washing three times, add the pure butanols violent stirring of top grade again after, at 78 ℃ of beginnings of temperature component distillation, obtain indium tin coprecipitate.
F. indium tin coprecipitate was placed 10 hours down for 40 ℃～130 ℃ at oven temperature.Break up then.
G. indium tin indium tin coprecipitate is put into retort furnace, temperature is incubated 6 hours down at 420 ℃, promptly obtains yellowish green ITO composite granule.The powder granule particle diameter is measured through TEM, and its median size is 18nm, BET specific surface area 40m
2/ g.
The target relative theory density of firing with the ITO composite granule of this prepared reaches more than 99%.
Claims (7)
1. nanometer grade indium tin oxide composite powder preparation method, with indium, tin metal or indium, the tin metal soluble salt is feedstock production or preparation mixing solutions, through co-precipitation, washing, solid-liquid separation, dry, calcining step, it is characterized in that: mixing solutions is after co-precipitation, washing process comprise the washing and organic solvent wash, there are the organic solvent of ternary azeotrope in adding and water and ethanol again after the solid-liquid separation, carry out component distillation, drying, break up, calcining obtains the ITO composite granule, it is to adopt methyl alcohol that described organic solvent is washed, the organic solvent that adds when ethanol or washing with acetone, described component distillation is an ethyl acetate, isopropylcarbinol, Pentyl alcohol, n-hexyl alcohol, n-Heptyl alcohol, hexalin or butanols.
2. preparation method according to claim 1, it is characterized in that: described is the feedstock production mixing solutions with indium, tin metal, be indium metal, tin to be dissolved in respectively in the acid solution fully mix then, wherein the purity of indium, tin metal is greater than 99.99%, acid solution be purity more than or equal to the pure concentrated nitric acid of top grade, the vitriol oil or concentrated hydrochloric acid aqueous solution, or purity is more than or equal to the pure concentrated nitric acid of top grade, the vitriol oil and concentrated hydrochloric acid any two kinds or three kinds of mixed aqueous solution.
3, preparation method according to claim 1 is characterized in that: described is that the preparation of raw material mixing solutions is that purity is dissolved in back mixing in the deionized water respectively more than or equal to top grade pure solubility indium salt and pink salt with indium, tin metal soluble salt.
4. according to the described preparation method of claim 1, it is characterized in that: described co-precipitation is meant under the situation of the mixing solutions that stirs preparation or preparation and adds purity more than or equal to the pure yellow soda ash of top grade, sodium bicarbonate, salt of wormwood, saleratus, volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium hydroxide, potassium hydroxide, hydrated barta, lithium hydroxide or urea neutralizing agent, makes mixing solutions produce indium, tin coprecipitate to alkalescence.
5. according to the described preparation method of claim 1, it is characterized in that: washing is that organic solvent is washed with purity more than or equal to analytically pure dehydrated alcohol with the deionized water wash of resistance greater than 10M Ω .CM.
6. method according to claim 1 is characterized in that: azeotropic distillation process control principle is: the organic solvent that adds when making the component that distills at last be distillation.
7, method according to claim 1 is characterized in that: calcining is to be incubated 2-15 hour down at 350 ℃ to 1200 ℃.
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| CN101812665B (en) * | 2010-03-26 | 2012-05-23 | 北京化工大学 | Method for preparing indium tin oxide (ITO) target material with single-phase structure and high density |
| CN104692452B (en) * | 2013-12-10 | 2016-04-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method that a kind of tin indium oxide is nanocrystalline |
| CN103771498A (en) * | 2013-12-27 | 2014-05-07 | 柳州百韧特先进材料有限公司 | Process for preparing nano ITO (Indium Titanium Oxide) powder by using reducing atmosphere |
| CN107324778A (en) * | 2017-06-12 | 2017-11-07 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of high density, high conductivity ITO target |
| CN112174193A (en) * | 2020-10-21 | 2021-01-05 | 武汉工程大学 | Preparation method of monodisperse nano ITO |
| CN112457025B (en) * | 2020-12-11 | 2022-08-30 | 广西晶联光电材料有限责任公司 | Preparation method of nano ITO powder with large specific surface area |
| CN112811896A (en) * | 2021-01-20 | 2021-05-18 | 北京化工大学 | Method for preparing indium tin oxide target material based on particle grading accumulation model |
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Non-Patent Citations (4)
| Title |
|---|
| 制备工艺对纳米级铟锡氧化物( ITO) 形貌和电性能的影响. 刘建玲等.功能材料，第36卷第4期. 2005 |
| 制备工艺对纳米级铟锡氧化物(ITO)形貌和电性能的影响. 刘建玲等.功能材料，第36卷第4期. 2005 * |
| 热处理对制备纳米氧化铟锡( ITO) 粉末的影响. 张永红，陈明飞.金属热处理，第28卷第2期. 2003 |
| 热处理对制备纳米氧化铟锡(ITO)粉末的影响. 张永红，陈明飞.金属热处理，第28卷第2期. 2003 * |
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