CN112479682A - Preparation method of environment-friendly and efficient ITO target material - Google Patents
Preparation method of environment-friendly and efficient ITO target material Download PDFInfo
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- CN112479682A CN112479682A CN202011477287.9A CN202011477287A CN112479682A CN 112479682 A CN112479682 A CN 112479682A CN 202011477287 A CN202011477287 A CN 202011477287A CN 112479682 A CN112479682 A CN 112479682A
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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
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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
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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
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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
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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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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- 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
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
Abstract
The invention discloses a preparation method of an environment-friendly and efficient ITO target, which comprises the following steps: s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In a gas flow containing 40% vol of oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder; s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing; s3, adding a dispersing agent and continuously mixing; s4, adding a wax-based binder and continuously mixing; s5, injecting the formed pulp into a filter type forming die to manufacture a forming body; s6, drying and degreasing the formed body; and S7, feeding the dried and degreased formed body into a sintering furnace for sintering to obtain the target material. The invention has the advantages of easy demoulding, and can improve the relative density of the target material, thereby increasing the yield of the target material and reducing the production cost.
Description
Technical Field
The invention relates to the technical field of ITO target preparation, in particular to a preparation method of an environment-friendly high-efficiency ITO target.
Background
The ITO target is a mixture of indium oxide and tin dioxide, and is an important raw material for preparing the ITO film. The ITO target is mainly used for manufacturing ITO film transparent conductive glass, which is a main material for manufacturing flat liquid crystal display and has wide and important application in the electronic industry and the information industry. The high-quality finished ITO target material has the relative density of more than or equal to 99 percent, and the target material has lower resistivity, higher thermal conductivity and higher mechanical strength. The high-density target can be sputtered on a glass substrate under the condition of lower temperature to obtain a conductive film with lower resistivity and higher light transmittance, and even an ITO conductive film can be sputtered on an organic material. However, the ITO powder at the present stage is not easy to demould after extrusion forming, and the relative density of the target material is unstable, so that the good product rate of the ITO target material is not ideal, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a preparation method of an environment-friendly and efficient ITO target material, which has the advantages of easiness in demoulding, capability of improving the relative density of the target material, further increase of the yield of the target material and reduction of the production cost, and solves the problems that the ITO powder at the present stage is difficult to demould after extrusion forming, the relative density of the target material is unstable, further the good yield of the ITO target material is not ideal, and the production cost is increased.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of an environment-friendly high-efficiency ITO target comprises the following steps:
s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In a gas flow containing 40% vol oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder, wherein the cooling speed is 106-108K/S;
s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing for 20-24 hours, wherein the average particle size of the raw material powder is 0.03-0.25 mu m;
s3, adding a dispersant, and continuously mixing, wherein the dispersant is a polycarboxylic dispersant, and the mixing time is 1-2 hours;
s4, adding a wax-based binder and continuously mixing;
s5, injecting the formed pulp into a filter type forming die to manufacture a forming body, wherein the raw material of the filter type forming die is a water-insoluble material which is obtained by pulping ceramic raw materials and draining water under reduced pressure to obtain the forming body;
s6, drying and degreasing the formed body;
and S7, feeding the dried and degreased formed body into a sintering furnace for sintering to obtain the target material.
Preferably, the mixing time in S4 is 15 to 20 hours.
Preferably, the drying temperature in S6 is 400 ℃ to 600 ℃.
Preferably, the primary sintering temperature is 1500-1700 ℃, the sintering time is 5-10min, the temperature is reduced to 1400-1600 ℃, the temperature is preserved for 15-20h, and then the temperature is cooled to the room temperature.
Preferably, the average cooling rate from the highest sintering temperature to 400 ℃ is 80-100 ℃/h.
Compared with the prior art, the invention has the beneficial effects that:
the powder prepared by melt oxidation has small specific surface area, the average grain diameter of 0.03-0.25 mu m, is approximately spherical, has low resistivity, and is suitable for preparing ITO target material with low resistivity, thereby being capable of obtaining high sputtering coating rate;
the wax-based binder can effectively reduce internal and external friction, reduce the loss of pressing pressure, improve the density of a pressed blank, reduce the demolding force in the demolding process, prolong the service life of a mold and enable parts to have better surface finish;
since the pressure during the pressure-reducing drainage of the filter type press mold is applied only between the filter and the lower molding die, a material having a low strength can be used as the lower molding die, and the material cost can be kept low even if the molding size is increased.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The invention provides a technical scheme of a preparation method of an environment-friendly high-efficiency ITO target material
Example 1:
a preparation method of an environment-friendly high-efficiency ITO target comprises the following steps:
s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In a gas flow containing 40% vol of oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder, wherein the cooling speed is 106K/S, and the average particle size of the raw material powder is 0.25 mu m;
s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing for 20 hours;
s3, adding a dispersant which is a polycarboxylic dispersant and mixing for 2 hours;
s4, adding a wax-based binder and continuously mixing for 20 hours;
s5, injecting the formed pulp into a filter type forming die to manufacture a forming body, wherein the raw material of the filter type forming die is a water-insoluble material which is obtained by pulping the ceramic raw material and draining water under reduced pressure to obtain the forming body;
s6, drying and degreasing the formed body, wherein the drying temperature is 500 ℃;
and S7, conveying the dried and degreased formed body into a sintering furnace for sintering to obtain the target material, wherein the primary sintering temperature is 1700 ℃, the sintering time is 10min, the temperature is reduced to 1600 ℃, the temperature is kept for 20h, then the temperature is cooled to room temperature, and the average cooling speed is reduced to 400 ℃ from the highest sintering temperature by 80 ℃/h.
Example 2:
a preparation method of an environment-friendly high-efficiency ITO target comprises the following steps:
s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In gas 6D41 containing 40% vol of oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder, wherein the cooling speed is 108K/S, and the average particle size of the raw material powder is 0.03 mu m;
s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing for 24 hours;
s3, adding a dispersant which is a polycarboxylic dispersant and continuously mixing for 1 hour;
s4, adding a wax-based binder and continuously mixing for 15 hours;
s5, injecting the formed pulp into a filter type forming die to manufacture a forming body, wherein the raw material of the filter type forming die is a water-insoluble material which is obtained by pulping the ceramic raw material and draining water under reduced pressure to obtain the forming body;
s6, drying and degreasing the formed body, wherein the drying temperature is 600 ℃;
and S7, conveying the dried and degreased formed body into a sintering furnace for sintering to obtain the target material, wherein the primary sintering temperature is 1600 ℃, the sintering time is 8min, the temperature is reduced to 1400 ℃, the temperature is kept for 15 ℃, then the temperature is cooled to room temperature, and the average cooling speed is reduced to 400 ℃ from the highest sintering temperature at 100 ℃/h.
Example 3:
a preparation method of an environment-friendly high-efficiency ITO target comprises the following steps:
s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In a gas flow containing 40% vol of oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder, wherein the cooling speed is 107K/S, and the average particle size of the raw material powder is 0.2 mu m;
s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing for 20 hours;
s3, adding a dispersant which is a polycarboxylic dispersant and continuously mixing for 1.5 hours;
s4, adding a wax-based binder and continuously mixing for 20 hours;
s5, injecting the formed pulp into a filter type forming die to manufacture a forming body, wherein the raw material of the filter type forming die is a water-insoluble material which is obtained by pulping the ceramic raw material and draining water under reduced pressure to obtain the forming body;
s6, drying and degreasing the formed body, wherein the drying temperature is 600 ℃;
and S7, conveying the dried and degreased formed body into a sintering furnace for sintering to obtain the target material, wherein the primary sintering temperature is 1600 ℃, the sintering time is 10min, the temperature is reduced to 1600 ℃, the temperature is kept for 15h, then the temperature is cooled to room temperature, and the average cooling speed is reduced to 400 ℃ from the highest sintering temperature at 90 ℃/h.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (5)
1. The preparation method of the environment-friendly high-efficiency ITO target is characterized by comprising the following steps:
s1, melting the In-Sn alloy by plasma arc, oxidizing the molten metal In a gas flow containing 40% vol oxygen In a plasma generating chamber, and intensively cooling the obtained reaction product In the gas flow to obtain raw material powder, wherein the cooling speed is 106-108K/S;
s2, putting the raw material powder, ion exchange water and zirconia into a ball milling tank, and carrying out ball milling and mixing for 20-24 hours, wherein the average particle size of the raw material powder is 0.03-0.25 mu m;
s3, adding a dispersant, and continuously mixing, wherein the dispersant is a polycarboxylic dispersant, and the mixing time is 1-2 hours;
s4, adding a wax-based binder and continuously mixing;
s5, injecting the formed pulp into a filter type forming die to manufacture a forming body, wherein the raw material of the filter type forming die is a water-insoluble material which is obtained by pulping ceramic raw materials and draining water under reduced pressure to obtain the forming body;
s6, drying and degreasing the formed body;
and S7, feeding the dried and degreased formed body into a sintering furnace for sintering to obtain the target material.
2. The method for preparing the environment-friendly high-efficiency ITO target material according to claim 1, wherein the method comprises the following steps: the mixing time in S4 is 15-20 hours.
3. The method for preparing the environment-friendly high-efficiency ITO target material according to claim 1, wherein the method comprises the following steps: the drying temperature in S6 is 400-600 ℃.
4. The method for preparing the environment-friendly high-efficiency ITO target material according to claim 1, wherein the method comprises the following steps: the primary sintering temperature is 1500-1700 ℃, the sintering time is 5-10min, the temperature is reduced to 1400-1600 ℃, the temperature is preserved for 15-20h, and then the temperature is cooled to the room temperature.
5. The method for preparing the environment-friendly high-efficiency ITO target material according to claim 8, wherein the method comprises the following steps: the average cooling speed from the highest sintering temperature to 400 ℃ is 80-100 ℃/h.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1149084A (en) * | 1995-08-18 | 1997-05-07 | W·C·赫罗伊斯有限公司 | Manufacturing method of cathode sputtering target or the similar targets |
| CN1208018A (en) * | 1997-05-23 | 1999-02-17 | W·C·赫罗伊斯有限公司 | Process for making crystalline solid-solution powder with low electrical resistance |
| CN1891663A (en) * | 2005-06-29 | 2007-01-10 | 三井金属矿业株式会社 | Indium oxide-tin oxide powder and sputtering target using the same and method for producing the indium oxide-tin oxide powder |
| CN1906130A (en) * | 2003-12-25 | 2007-01-31 | 三井金属矿业株式会社 | Indium oxide-tin oxide powder and sputtering target using the same |
| CN101269834A (en) * | 2008-05-19 | 2008-09-24 | 昆明理工大学 | Method for producing nano-ITO powder with plasma electrical arc one-step method |
| CN101392362A (en) * | 2008-10-30 | 2009-03-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ITO target from nano homogeneous ITO powder |
-
2020
- 2020-12-15 CN CN202011477287.9A patent/CN112479682A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1149084A (en) * | 1995-08-18 | 1997-05-07 | W·C·赫罗伊斯有限公司 | Manufacturing method of cathode sputtering target or the similar targets |
| CN1208018A (en) * | 1997-05-23 | 1999-02-17 | W·C·赫罗伊斯有限公司 | Process for making crystalline solid-solution powder with low electrical resistance |
| CN1906130A (en) * | 2003-12-25 | 2007-01-31 | 三井金属矿业株式会社 | Indium oxide-tin oxide powder and sputtering target using the same |
| CN1891663A (en) * | 2005-06-29 | 2007-01-10 | 三井金属矿业株式会社 | Indium oxide-tin oxide powder and sputtering target using the same and method for producing the indium oxide-tin oxide powder |
| CN101269834A (en) * | 2008-05-19 | 2008-09-24 | 昆明理工大学 | Method for producing nano-ITO powder with plasma electrical arc one-step method |
| CN101392362A (en) * | 2008-10-30 | 2009-03-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ITO target from nano homogeneous ITO powder |
Non-Patent Citations (1)
| Title |
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| 陈宏: "《压电陶瓷及其应用》", 31 May 2019, 陕西师范大学出版总社 * |
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Application publication date: 20210312 |