CN113321490A - Preparation method of ITO target material - Google Patents
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- CN113321490A CN113321490A CN202110704806.9A CN202110704806A CN113321490A CN 113321490 A CN113321490 A CN 113321490A CN 202110704806 A CN202110704806 A CN 202110704806A CN 113321490 A CN113321490 A CN 113321490A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000013077 target material Substances 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 87
- 239000002131 composite material Substances 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 18
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000003825 pressing Methods 0.000 abstract description 4
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- 238000007493 shaping process Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 8
- 238000004064 recycling Methods 0.000 description 8
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- 239000002699 waste material Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract
The invention relates to a preparation method of an ITO target material, which collects ITO composite powder which is not molded and sintered and has a grain diameter not meeting the production requirement after the powder making step, carries out recovery preparation step, uses specific temperature for calcination, can remove organic impurities in the ITO composite powder under the condition of avoiding crystal orientation shaping, reduces and disperses the ITO composite powder into small-grain indium oxide and tin oxide mixed powder, and then carries out the powder making step again to obtain the ITO composite powder with the grain diameter meeting the production requirement, so that the obtained ITO composite powder is not easy to agglomerate, more air holes can be avoided in the process of molding and pressing green bodies, and the prepared ITO target material has high sintering density. The preparation method of the ITO target material provided by the invention is simple in process, and the recovered preparation steps do not use reagents which pollute the environment, so that the preparation method is more environment-friendly.
Description
Technical Field
The invention relates to the technical field of ITO target production, in particular to a preparation method of an ITO target.
Background
Indium Tin Oxide target material, referred to as ITO target material for short, is a ceramic functional material formed by mixing powders of two metal oxides of Indium Oxide and Tin Oxide, processing the mixture into ITO composite powder, and then pressing and sintering the ITO composite powder at high temperature. After the ITO target material is subjected to vacuum magnetron sputtering coating, an ITO transparent conductive film can be formed on a substrate such as glass, the ITO film has high visible light transmittance, high infrared light region reflectivity and high ultraviolet light region absorptivity, and has good conductivity, substrate adhesion and chemical stability, and the ITO transparent conductive film is widely applied to industry in recent years.
Because indium is a rare metal and is expensive, recycling of the ITO target is particularly important. At present, the common recyclable ITO target material has two main sources, one is a residual waste target of the ITO target material after magnetron sputtering coating, and the other is a target material waste material generated by cutting and polishing a bad target material with a shape and a size which do not reach the standard after sintering. The existing recovery treatment mode is to carry out acid soaking, crushing and other treatments on the waste target or the target material waste to obtain ITO granules.
The continuous grain boundaries can be formed among the grains of the ITO composite powder after sintering, so that the crystal orientation is shaped, the process is usually irreversible, and the grain boundaries formed among the grains after sintering cannot be removed through the existing recovery mode, so that after the ITO target materials from the two sources are recovered, the original mixed powder of indium oxide and tin oxide cannot be directly recovered under the limitation of the grain boundaries, only ITO granules with the shaped crystal orientation can be obtained, the ITO granules are easy to agglomerate in the pressing process, so that more pores exist in a pressed green body, and the pores cannot be completely removed after sintering, so that the ITO target material with high strength and high density cannot be obtained after the green body pressed by the ITO granules is sintered. In addition, the conventional recovery treatment methods have complicated processes and high recovery cost, and reagents including acids used in the treatment process may cause environmental pollution.
Disclosure of Invention
The invention aims to provide a preparation method of an ITO target, which has simple recovery and preparation process and no pollution to the environment.
In order to achieve the above object, the present invention provides a method for preparing an ITO target,
comprises the following main preparation steps:
s1, performing a powder making step by taking indium oxide powder and tin oxide powder as raw materials to obtain ITO composite powder;
s2, taking ITO composite powder with the particle size of 20-80 mu m, and carrying out molding sintering to obtain an ITO target material;
also comprises the following recovery preparation steps:
s3, collecting the ITO composite powder obtained in the step S1, wherein the grain size of the ITO composite powder is not 20-80 microns, and calcining the ITO composite powder so as to disperse and reduce the ITO composite powder into small-grain indium oxide and tin oxide mixed powder, wherein the calcining temperature is lower than the lowest temperature for sintering the ITO composite powder into an ITO target;
s4, performing a powder making step by taking the mixed powder of indium oxide and tin oxide obtained in the step S3 as a raw material to obtain ITO composite powder with the granularity of 20-80 mu m;
s5, molding and sintering the ITO composite powder obtained in the step S4 to obtain an ITO target material;
wherein the powder making step comprises:
a. adding a dispersing agent and water to ball mill the raw materials, and then adding a primary dispersing agent and water to sand;
b. adding a binder and a defoaming agent, and stirring to obtain ITO slurry;
c. and carrying out spray granulation on the ITO slurry.
Has the advantages that: the invention recovers ITO composite powder which is not sintered, but has particle size which does not meet the production requirement without molding and sintering, the recovered ITO composite powder is not sintered, continuous crystal boundaries are not formed among crystal grains in the ITO composite powder, the ITO composite powder is calcined at a specific temperature which is lower than the lowest temperature for sintering the ITO composite powder into an ITO target, so that organic impurities in the ITO composite powder can be removed under the condition of avoiding crystal orientation shaping, the ITO composite powder is reduced and dispersed into small-particle indium oxide and tin oxide mixed powder, the powder manufacturing step is executed again to obtain the ITO composite powder with particle size meeting the production requirement, and the ITO composite powder is not easy to agglomerate compared with ITO granules obtained by the existing recovery processing step, and more air holes can be avoided in the process of molding and pressing green bodies, the target material prepared from the ITO composite powder has high sintering density. Compared with the existing recovery processing mode, the recovery preparation steps of the invention have simpler process, and the recovery preparation steps do not use reagents which pollute the environment, thus being more environment-friendly.
Drawings
FIG. 1 is a particle size distribution diagram of an ITO composite powder prepared by the recycling preparation step in example 1 of the present invention;
FIG. 2 is a particle size distribution diagram of the ITO composite powder prepared by the recycling and preparing step in example 4 of the present invention.
Detailed Description
And collecting the ITO composite powder after the powder making step and before the forming step in the preparation process of the ITO target, removing the binder in the ITO powder by dry grinding, and then obtaining the ITO target by the powder making, forming and sintering steps.
The invention is described in further detail below with reference to specific embodiments.
Example 1
A preparation method of an ITO target comprises the following main preparation steps:
s1, performing a powder making step by taking indium oxide powder and tin oxide powder with a mixing ratio of 90:10 as raw materials to obtain ITO composite powder;
s2, taking ITO composite powder with the particle size of 20-80 mu m, and carrying out molding sintering to obtain an ITO target material;
also comprises the following recovery preparation steps:
s3, collecting ITO composite powder with the particle size of 20-80 mu m in the composite powder obtained in the step S1, placing the collected ITO composite powder in a crucible, calcining for 4 hours at 800 ℃, removing organic impurities in the ITO composite powder, and dispersing and reducing the ITO composite powder into indium oxide and tin oxide mixed powder;
s4, performing a powder making step by taking the mixed powder of the indium oxide and the tin oxide obtained in the step S3 as a raw material to obtain ITO composite powder;
s5, molding and sintering the ITO composite powder obtained in the step S6 to obtain an ITO target material;
the powdering step performed in steps S1 and S4 specifically is:
a. adding a dispersing agent and water to ball mill the raw materials, and then adding a primary dispersing agent and water to sand;
b. adding a binder and a defoaming agent, and stirring to obtain ITO slurry;
c. and carrying out spray granulation on the ITO slurry.
Starting from step S3, a recycling preparation step may be performed after step S2, or may be performed together with step S2. In step S3, the organic impurities removed are mainly compounds composed of C, H, O, such as binders added in the powdering step of the main preparation step. In the powdering step of step S1, the addition ratio of the dispersing agent in the ball-milling process was 0.8%, and the addition ratio of the dispersing agent in the sanding process was 0.5%, and in the powdering step of step S4, the addition ratio of the dispersing agent in the ball-milling process was 0.5%, and the addition ratio of the dispersing agent in the sanding process was 0.3%. The grain diameter of the ITO composite powder obtained in the step S4 is 37.09 mu m (as shown in figure 1), and the density of the ITO target obtained by sintering in the step S5 reaches 7.137g/cm 3.
Example 2
A method for producing an ITO target, which comprises the same steps as in example 1, except that in step S1, the mixing ratio of indium oxide powder and tin oxide powder is 93:7, the addition ratio of the dispersant in the ball milling process is 0.7%, and the addition ratio of the dispersant in the sand milling process is 0.4%. The density of the ITO target sintered in the step S5 is 7.126g/cm 3.
Example 3
The preparation method of the ITO target material is basically the same as that of the example 1, except that in the step S1, the mixing ratio of the indium oxide powder and the tin oxide powder is 97:3, the adding ratio of the dispersing agent in the ball milling process is 0.72%, the adding ratio of the dispersing agent in the sand milling process is 0.4%, and the density of the ITO target material obtained by sintering in the step S5 is 7.096g/cm 3.
In the recovery preparation step, even if organic impurities are removed through calcination, the particle size of the obtained indium oxide and tin oxide mixed powder is basically larger than that of raw material indium oxide powder and tin oxide powder used in the powder making step of the main preparation step, and in order to improve the dispersibility of the ITO composite powder and reduce agglomeration, the adding proportion of the dispersing agent in the powder making step of the recovery preparation step is theoretically deduced to be larger than that in the powder making step of the main preparation step. As can be seen from examples 1 to 3, the addition ratio of the dispersing agent in the powdering step of the recycling preparation step is always smaller than the addition ratio of the dispersing agent in the powdering step of the main preparation step, and the results show that by using the method of the present invention, the ITO composite powder after the powdering step in the main preparation step and before the molding step is collected for the recycling preparation step, and in the powdering step of the recycling preparation step, the same effect as the conventional addition ratio of the dispersing agent in the main preparation step can be achieved with only a small amount of the dispersing agent.
Example 4
The preparation method of the ITO target material basically comprises the same steps as the example 1, except that the calcining temperature is 750 ℃, and the calcining time is 5 hours. The grain diameter of the finally obtained ITO composite powder is 35.54 mu m (as shown in figure 2), and the sintering density of the prepared ITO target is 7.137g/cm 3.
Comparative example 1
A method for preparing an ITO target, which comprises the steps substantially the same as those of example 1, except that step S4 includes: and (4) cutting and polishing the ITO target material, and collecting ITO waste as the raw material of the step S5. The grain diameter of the finally obtained ITO composite powder is 89 mu m, and the sintering density of the prepared ITO target material is 7.101g/cm 3.
From the results of example 1 and comparative example 1, it can be seen that, in the present example, the ITO composite powder that does not enter the sintering step is collected for recycling, and compared with the ITO scrap that is generated after the sintering step, the particle size of the powder prepared in the present example is smaller under the same conditions, and the obtained target material has a higher sintering density.
The above description is only the embodiments of the present invention, and the scope of protection is not limited thereto. The insubstantial changes or substitutions will now be made by those skilled in the art based on the teachings of the present invention, which fall within the scope of the claims.
Claims (5)
- The preparation method of the ITO target comprises the following main preparation steps:s1, performing a powder making step by taking indium oxide powder and tin oxide powder as raw materials to obtain ITO composite powder;s2, taking ITO composite powder with the particle size of 20-80 mu m, and carrying out molding sintering to obtain an ITO target material;the method is characterized by also comprising the following recovery preparation steps:s3, collecting the ITO composite powder obtained in the step S1, wherein the grain size of the ITO composite powder is not 20-80 microns, and calcining the ITO composite powder so as to disperse and reduce the ITO composite powder into small-grain indium oxide and tin oxide mixed powder, wherein the calcining temperature is lower than the lowest temperature for sintering the ITO composite powder into an ITO target;s4, performing a powder making step by taking the mixed powder of indium oxide and tin oxide obtained in the step S3 as a raw material to obtain ITO composite powder with the granularity of 20-80 mu m;s5, molding and sintering the ITO composite powder obtained in the step S4 to obtain an ITO target material;wherein the powder making step comprises:a. adding a dispersing agent and water to ball mill the raw materials, and then adding a primary dispersing agent and water to sand;b. adding a binder and a defoaming agent, and stirring to obtain ITO slurry;c. and carrying out spray granulation on the ITO slurry.
- 2. The method for preparing an ITO target according to claim 1, wherein the proportion of dispersant added in the ball-milling process in the powder-making step of step S4 is smaller than the proportion of dispersant added in the ball-milling process in the powder-making step of step S1, and the proportion of dispersant added in the sand-milling process in step S4 is smaller than the proportion of dispersant added in the sand-milling process in step S1.
- 3. The method for preparing an ITO target according to claim 2, wherein in step S1, the addition ratio of the dispersing agent in the ball milling process is 0.3-0.9%, the addition ratio of the dispersing agent in the sanding process is 0.3-0.7%, in step S4, the addition ratio of the dispersing agent in the ball milling process is 0.2-0.8%, and the addition ratio of the dispersing agent in the sanding process is 0.2-0.5%.
- 4. The method for preparing the ITO target of claim 1, wherein in step S3, the calcination is performed at 400-800 ℃ for 1-5 h.
- 5. The method for preparing an ITO target according to claim 1, wherein in step S1, the mixing ratio of the indium oxide powder to the tin oxide powder is 90:10, 95:5, 93:7, or 97: 3.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11100253A (en) * | 1997-09-25 | 1999-04-13 | Tosoh Corp | Method for regenerating ito sintered body and application thereof |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
| CN109320231A (en) * | 2018-09-13 | 2019-02-12 | 江苏比昂电子材料有限公司 | The recovery and treatment method of ITO target |
| CN109956746A (en) * | 2017-12-25 | 2019-07-02 | 株洲冶炼集团股份有限公司 | A kind of process of the useless target of recycling and reusing ITO |
-
2021
- 2021-06-24 CN CN202110704806.9A patent/CN113321490A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11100253A (en) * | 1997-09-25 | 1999-04-13 | Tosoh Corp | Method for regenerating ito sintered body and application thereof |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
| CN109956746A (en) * | 2017-12-25 | 2019-07-02 | 株洲冶炼集团股份有限公司 | A kind of process of the useless target of recycling and reusing ITO |
| CN109320231A (en) * | 2018-09-13 | 2019-02-12 | 江苏比昂电子材料有限公司 | The recovery and treatment method of ITO target |
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