CN113800900A - Method for processing high-density ITO target material powder - Google Patents
Method for processing high-density ITO target material powder Download PDFInfo
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- CN113800900A CN113800900A CN202110940440.5A CN202110940440A CN113800900A CN 113800900 A CN113800900 A CN 113800900A CN 202110940440 A CN202110940440 A CN 202110940440A CN 113800900 A CN113800900 A CN 113800900A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Abstract
The invention provides a method for processing high-density ITO target powder, which comprises the steps of adding tin oxide powder into a sand mill, adding deionized water, a dispersing agent and an additive, pre-milling, adding deionized water, a dispersing agent and an additive into tin oxide slurry and indium oxide powder, and then, sanding, wherein the addition amount of the dispersing agent in the second step/the addition amount of the dispersing agent in the second step and the addition amount of the dispersing agent in the third step is less than or equal to 40 percent, so that the slurry is synthesized by mixing once, the period is short, the density is obviously improved, and the product performance and the use efficiency of a client are improved.
Description
Technical Field
The invention relates to the field of ITO target materials, in particular to a method for processing high-density ITO target material powder.
Background
The ITO target material is an N-type semiconductor material-sintered body of indium tin oxide, and an ITO film obtained by magnetron sputtering has excellent light transmission and electrical conductivity, good processing performance, high hardness and corrosion resistance. The organic electroluminescent material is widely applied to the fields of Thin Film Transistors (TFT), flat Liquid Crystal Displays (LCD), solar cells, functional glass and the like. Among the main indexes of high density, large size, low nodulation and low resistance of the ITO target, the high density is the primary factor and is the key factor for determining whether the ITO target can be normally used or not and obtaining good ITO film performance.
In the current mainstream ITO target production process, a powder treatment process is adopted without exception, and the process is almost decisive for the influence of the high-density ITO target in the whole production line, so that the importance of ensuring the high-density ITO target is self-evident. The prior art patent CN104944964B discloses a method for preparing a high-density ITO target material by reducing sintering conditions, in the preparation of the initial ITO slurry, a first premixed solution is prepared and used in a ball mill, and a baking oven is used in the preparation of a secondary material by low-temperature drying, in the preparation of the ITO slurry, a second premixed solution is prepared and used in the ball mill again, a slip casting method is adopted in the forming processing of the ITO green body, compressed air is used as a pressure transmission medium, the sintering processing of the ITO green body adopts the condition of normal pressure oxygen atmosphere, the ITO slurry with high solid content is one of the necessary conditions for preparing the high-density ITO green body, the relative density of the prepared ITO green body can reach 74-76 percent through mercury discharge method, the solid content of the ITO slurry reaches 89-91% by ball milling of the secondary material, and the high-density ITO target material with the relative density of 99.50-99.67% can be prepared by better viscosity fluidity and lower sintering temperature. The technology adopts twice premixing, twice drying and finally preparing the slurry, has long production period and complicated operation, needs a redesign processing method for the ITO target powder, and adopts once mixing to prepare the slurry to shorten the period, so that the problem is very necessary to be solved.
Disclosure of Invention
In order to solve the problems, the invention provides a method for processing high-density ITO target material powder, wherein tin oxide powder is added into a sand mill to be pre-milled by adding deionized water, a dispersing agent and an additive, and then tin oxide slurry and indium oxide powder are added with deionized water, a dispersing agent and an additive to be milled, wherein the addition amount of the dispersing agent in the second step/the addition amount of the dispersing agent in the second step and the addition amount of the dispersing agent in the third step is less than or equal to 40 percent, so that the slurry is synthesized by mixing once, the period is short, the density is obviously improved, the product performance and the use efficiency of a client are improved, and the problems in the background technology are solved.
The invention aims to provide a method for processing high-density ITO target powder, wherein the ITO target powder comprises indium oxide powder and tin oxide powder; the method comprises the following steps:
the method comprises the following steps: firstly, preparing indium oxide powder and tin oxide powder;
step two: pre-grinding tin oxide powder: pouring tin oxide powder into a sand mill, adding quantitative deionized water, adding a dispersing agent and an additive, pre-stirring and mixing, and pre-milling, wherein the solid content is 20% -55%;
step three: pouring indium oxide powder into a sanding tank to be mixed with the tin oxide slurry prepared in the step two, adding a certain amount of deionized water, a dispersant and an additive, uniformly mixing and stirring, and then starting a sanding machine for sanding until the granularity meets the specified requirement;
the dispersing agent is: the dispersant is an anionic dispersant HS-DISPERSANT 6067M, wherein the addition amount of the dispersant in the second step/the addition amount of the dispersant in the second step and the third step is less than or equal to 40 percent.
The further improvement lies in that: the pre-grinding after the pre-stirring and mixing in the second step is specifically as follows: and (3) after the pre-stirring is carried out for more than or equal to 10 minutes, pre-grinding the tin oxide by adopting a circulation or grinding way quadratic mode, and pumping the pre-ground tin oxide slurry into a sand grinding tank for waiting after the pre-grinding.
The further improvement lies in that: pre-milling until the size of the tin oxide slurry reaches 0.15um < D50<0.3 um.
The further improvement lies in that: and adding a certain amount of additives and deionized water after sanding in the third step.
The further improvement lies in that: the method also comprises the following four steps: and granulating the slurry, and then mixing and grading to obtain ITO target powder.
The further improvement lies in that: and step four, after mixing and grading, forming and sintering the ITO target powder to obtain an ITO target sintered body.
The invention has the beneficial effects that: according to the invention, the tin oxide powder is added into a sand mill to be pre-milled by adding deionized water, a dispersing agent and an additive, then the tin oxide slurry and the indium oxide powder are added with deionized water, a dispersing agent and an additive to be milled, and the addition amount of the dispersing agent in the second step/the addition amount of the dispersing agent in the second step and the addition amount of the dispersing agent in the third step is less than or equal to 40 percent, so that the slurry is synthesized by mixing once, the period is short, the density is obviously improved, and the product performance and the use efficiency of a client are improved; the dispersing agent is an anionic dispersing agent HS-DISPERSANT 6067M, and the agglomerated powder is more easily dispersed in the ball milling process; the pre-grinding of the tin oxide powder needs to reach the granularity of the slurry of 0.15um < D50<0.3um, thus ensuring the pre-grinding effect; the addition amount of the dispersing agent in the second step/the addition amount of the dispersing agent in the second step and the third step is less than or equal to 40%, the addition amount of the dispersing agent is matched with different sanding requirements, and the sanding effect of the second step and the third step is ensured, so that the density of the finally prepared ITO target sintered body is ensured; the density of the ITO target sintered body is obviously improved, the relative density of the ITO target is stabilized to be more than 99.5%, the density is greatly improved, and the performance and the use efficiency of a client product are improved.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
Example one
The embodiment provides a method for processing high-density ITO target powder, which comprises the following steps:
the method comprises the following steps: preparing indium oxide powder and tin oxide powder with the mass percentage of 90: 10;
step two: pre-grinding tin oxide powder: pouring tin oxide powder into a sand mill, adding quantitative deionized water, adding an anionic dispersant HS-DISPERSANT 6067M and an additive accounting for 40% of the total amount, pre-stirring for 12 minutes, pre-milling tin oxide, pre-milling in a circulating mode, wherein the granularity of slurry of sand-milled tin oxide slurry reaches D50 of 0.21, and pumping the pre-milled tin oxide slurry into a sand mill tank for waiting;
step three: pouring indium oxide powder into a sanding tank to be mixed with tin oxide slurry, adding a certain amount of deionized water, the remaining 60% of anionic dispersant HS-DISPERSANT 6067M and additives, uniformly mixing and stirring, and then starting a sanding machine for sanding until the granularity meets the specified requirement; then adding a certain amount of additive and deionized water;
step four: and granulating the slurry, mixing and grading to obtain ITO target powder, and finally molding and sintering the ITO target powder to obtain an ITO target sintered body.
In this embodiment, the tin oxide powder is added into a sand mill, deionized water, a dispersing agent and an additive are added into the sand mill, and pre-milling is performed to obtain tin oxide slurry, then the deionized water, the dispersing agent and the additive are added into the tin oxide slurry and the indium oxide powder, and sand milling is performed to obtain ITO powder slurry, and then granulation and fractional sintering are performed, so that the tin oxide powder is pre-milled, and the ITO target material relative density is detected to be 99.6%.
Example two
The embodiment provides a method for processing high-density ITO target powder, which comprises the following steps:
the method comprises the following steps: preparing 95 mass percent: 5 indium oxide powder and tin oxide powder;
step two: pre-grinding tin oxide powder: pouring tin oxide powder into a sand mill, adding quantitative deionized water, adding 35% of solid content, adding 35% of anionic dispersant HS-DISPERSANT 6067M and additive, pre-stirring for 15 minutes, pre-milling tin oxide, pre-milling by adopting a channel-making quadratic mode, wherein the granularity of the paste of sand-milled tin oxide paste reaches D50 of 0.19, and pumping the pre-milled tin oxide paste into a sand mill tank for waiting;
step three: pouring indium oxide powder into a sanding tank to be mixed with tin oxide slurry, adding quantitative deionized water, remaining 65% of anionic dispersant HS-DISPERSANT 6067M and additive, mixing and stirring uniformly, and then starting a sanding machine for sanding until the granularity meets the specified requirement; then adding a certain amount of additive and deionized water;
step four: and granulating the slurry, mixing and grading to obtain ITO target powder, and finally molding and sintering the ITO target powder to obtain an ITO target sintered body.
In this embodiment, the tin oxide powder is added into a sand mill, deionized water, a dispersing agent and an additive are added into the sand mill, and pre-milling is performed to obtain tin oxide slurry, then the deionized water, the dispersing agent and the additive are added into the tin oxide slurry and the indium oxide powder, and sand milling is performed to obtain ITO powder slurry, and then granulation and fractional sintering are performed, so that the tin oxide powder is pre-milled, and the ITO target material relative density is detected to be 99.57%.
In the conventional ITO powder treatment, indium oxide and tin oxide are directly mixed before sand grinding (or ball milling), and then are treated together, so that the relative density of the final ITO target is less than 99 percent, which is lower than that of the ITO target in the first embodiment and the second embodiment.
Claims (6)
1. A method for processing high-density ITO target material powder comprises the steps of preparing indium oxide powder and tin oxide powder; the method is characterized in that: the method comprises the following steps:
the method comprises the following steps: firstly, preparing indium oxide powder and tin oxide powder;
step two: pre-grinding tin oxide powder: pouring tin oxide powder into a sand mill, adding quantitative deionized water, adding a dispersing agent and an additive, pre-stirring and mixing, and pre-milling, wherein the solid content is 20% -55%;
step three: pouring indium oxide powder into a sanding tank to be mixed with the tin oxide slurry prepared in the step two, adding a certain amount of deionized water, a dispersant and an additive, uniformly mixing and stirring, and then starting a sanding machine for sanding until the granularity meets the specified requirement;
the dispersing agent is: the dispersant is an anionic dispersant HS-DISPERSANT 6067M, wherein the addition amount of the dispersant in the second step/the addition amount of the dispersant in the second step and the third step is less than or equal to 40 percent.
2. The method for processing high-density ITO target powder according to claim 1, wherein: the pre-grinding after the pre-stirring and mixing in the second step is specifically as follows: and (3) after the pre-stirring is carried out for more than or equal to 10 minutes, pre-grinding the tin oxide by adopting a circulation or grinding way quadratic mode, and pumping the pre-ground tin oxide slurry into a sand grinding tank for waiting after the pre-grinding.
3. The method for processing high-density ITO target powder according to claim 2, wherein: pre-milling until the size of the tin oxide slurry reaches 0.15um < D50<0.3 um.
4. The method for processing high-density ITO target powder according to claim 1, wherein: and adding a certain amount of additives and deionized water after sanding in the third step.
5. The method for processing high-density ITO target powder according to claim 1, wherein: the method also comprises the following four steps: and granulating the slurry, and then mixing and grading to obtain ITO target powder.
6. The method for processing high-density ITO target powder according to claim 5, wherein: and step four, after mixing and grading, forming and sintering the ITO target powder to obtain an ITO target sintered body.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115893989A (en) * | 2022-12-29 | 2023-04-04 | 芜湖映日科技股份有限公司 | Process method for refining ITO target material micro grain structure and enhancing mechanical strength |
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| CN108911707A (en) * | 2018-07-30 | 2018-11-30 | 常州苏晶电子材料有限公司 | The preparation method of high-density ITO targe material |
| CN110256049A (en) * | 2019-08-05 | 2019-09-20 | 先导薄膜材料有限公司 | A kind of preparation method of ito powder |
| CN110818404A (en) * | 2018-08-09 | 2020-02-21 | 株洲火炬安泰新材料有限公司 | Novel preparation method of high-density ITO target |
| CN111138202A (en) * | 2020-01-16 | 2020-05-12 | 洛阳晶联光电材料有限责任公司 | Method for preparing ITO (indium tin oxide) granulation powder by mixing method |
| CN111807845A (en) * | 2020-06-23 | 2020-10-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of solid spherical ITO granulation powder |
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2021
- 2021-08-17 CN CN202110940440.5A patent/CN113800900A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106082993A (en) * | 2016-06-08 | 2016-11-09 | 中国船舶重工集团公司第七二五研究所 | A kind of method preparing high-performance ITO pelletizing |
| CN108911707A (en) * | 2018-07-30 | 2018-11-30 | 常州苏晶电子材料有限公司 | The preparation method of high-density ITO targe material |
| CN110818404A (en) * | 2018-08-09 | 2020-02-21 | 株洲火炬安泰新材料有限公司 | Novel preparation method of high-density ITO target |
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| CN111138202A (en) * | 2020-01-16 | 2020-05-12 | 洛阳晶联光电材料有限责任公司 | Method for preparing ITO (indium tin oxide) granulation powder by mixing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115893989A (en) * | 2022-12-29 | 2023-04-04 | 芜湖映日科技股份有限公司 | Process method for refining ITO target material micro grain structure and enhancing mechanical strength |
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