[go: up one dir, main page]

CN116162908B - Indium zinc oxide target and preparation method thereof - Google Patents

Indium zinc oxide target and preparation method thereof Download PDF

Info

Publication number
CN116162908B
CN116162908B CN202211616872.1A CN202211616872A CN116162908B CN 116162908 B CN116162908 B CN 116162908B CN 202211616872 A CN202211616872 A CN 202211616872A CN 116162908 B CN116162908 B CN 116162908B
Authority
CN
China
Prior art keywords
zinc oxide
slurry
dispersing
indium
grinding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202211616872.1A
Other languages
Chinese (zh)
Other versions
CN116162908A (en
Inventor
顾德盛
邵学亮
王奇峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Vital Thin Film Materials Guangdong Co Ltd
Original Assignee
Vital Thin Film Materials Guangdong Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vital Thin Film Materials Guangdong Co Ltd filed Critical Vital Thin Film Materials Guangdong Co Ltd
Priority to CN202211616872.1A priority Critical patent/CN116162908B/en
Publication of CN116162908A publication Critical patent/CN116162908A/en
Application granted granted Critical
Publication of CN116162908B publication Critical patent/CN116162908B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • C04B2235/02—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
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • 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
    • C04B2235/02—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
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • 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
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention belongs to the technical field of photoelectric material preparation, and discloses an indium zinc oxide target and a preparation method thereof. The indium zinc oxide target material consists of indium oxide and zinc oxide, wherein the atomic ratio of Zn to In the target material is Zn/(Zn+In) =18-50%. The preparation method comprises the following steps: adding a dispersing agent, zinc oxide powder, indium oxide powder and a binder into water, stirring and dispersing uniformly, and then carrying out wet grinding to obtain mixed slurry; and (3) granulating the obtained mixed slurry by spraying to obtain IZO powder, and sintering after dry pressing and cold isostatic pressing to obtain the indium zinc oxide target. The IZO target material has high-proportion ZnO addition, can achieve higher density and conductivity, and can remarkably reduce the use amount of metal indium.

Description

Indium zinc oxide target and preparation method thereof
Technical Field
The invention belongs to the technical field of photoelectric material preparation, and particularly relates to an indium zinc oxide target and a preparation method thereof.
Background
Transparent conductive oxide (TRANSPARENT CONDUCTIVE OXIDE, TCO for short) is an important optoelectronic functional material, which has very high transmittance to visible light and very high reflectivity to infrared light, and has excellent conductivity. Therefore, TCOs are widely used in the fields of solar cells, flat panels and liquid crystal displays, light emitting diodes and heat radiation mirrors. Tin doped indium Oxide (Indi μm Tin Oxide, abbreviated as ITO) is the most widely used transparent conductive film at present, and the mass content of indium Oxide in the film is up to 90%. It is known that indium metal is scarce in crust and is a scarce resource and expensive; and ITO is unstable in hydrogen plasma. Therefore, a novel low indium content transparent conductive film must be developed to replace ITO. The zinc oxide raw material has rich sources, low price, no toxicity and good stability in hydrogen plasma; the semiconductor has high transmittance to visible light, is easy to realize n-type doping, and the conductivity of the transparent conductive film after n-type doping is close to that of ITO. Therefore, a transparent conductive film doped with zinc oxide as a matrix has become an important point of current research, and there is a trend to gradually replace ITO in many fields. Currently, a target of indium zinc oxide (In 2O3 -ZnO: commonly referred to as IZO) is widely used for various electronic components such as a transparent conductive film of a liquid crystal display device and a gas sensor.
Patent CN 109837512A discloses an IZO target having the following overall composition: the IZO target contains In, sn and Zn, satisfies Zn/(In+Sn+Zn) =0.030 to 0.250 and Sn/(In+Sn+Zn) =0.002 to 0.080 In terms of atomic ratio, and the balance is composed of O and unavoidable impurities, and has a target structure In which Sn segregation particles having a particle diameter of 200nm or more, which are specified by FE-EPMA and contain In, sn and O, are dispersed. Patent CN 106187100A discloses a sputtering target containing the compound In 2CexZnO4+2x, where x=0.5 to 2. The sputtering target is formed by mixing indium oxide (In 2O3), cerium oxide (CeO 2), and zinc oxide (ZnO) and sintering the mixture.
The above patent technology generally adopts Sn or Ce doping to improve the photoelectric properties of the IZO target, but no solution is proposed for improving the relative density and conductivity of undoped IZO targets.
Disclosure of Invention
In view of the above drawbacks and shortcomings of the prior art, a primary object of the present invention is to provide an indium zinc oxide target.
The invention also aims to provide a preparation method of the indium zinc oxide target.
The invention aims at realizing the following technical scheme:
an indium zinc oxide target material is composed of indium oxide and zinc oxide; the atomic ratio of Zn to In the target is Zn/(Zn+In) =18-50%.
Further, the relative density of the indium zinc oxide target material is more than 98.5%, and the conductivity is more than 1350s/cm.
The preparation method of the indium zinc oxide target material comprises the following preparation steps:
(1) Adding a dispersing agent, zinc oxide powder, indium oxide powder and a binder into water, stirring and dispersing uniformly, and then carrying out wet grinding to obtain mixed slurry;
(2) Granulating the mixed slurry obtained in the step (1) by spraying to obtain IZO powder;
(3) And sintering the IZO powder after dry pressing and cold isostatic pressing to obtain the indium zinc oxide target.
Further, the preparation steps of the indium zinc oxide target material are as follows:
1) Adding zinc oxide powder and a dispersing agent into water, stirring and dispersing uniformly, and then grinding by a wet method to obtain slurry I;
2) Adding a dispersing agent, water and indium oxide powder into the slurry I, stirring and dispersing uniformly, and then grinding by a wet method to obtain a slurry II;
3) Adding a binder into the slurry II, stirring and dispersing uniformly, and then grinding by a wet method to obtain a slurry III;
4) Granulating the slurry III by spraying to obtain IZO powder;
5) And sintering the IZO powder after dry pressing and cold isostatic pressing to obtain the indium zinc oxide target.
Further, the dispersing agent is selected from one or more of polyvinylpyrrolidone (PVP), sodium Dodecyl Benzene Sulfonate (SDBS), sodium hexadecyl benzene sulfonate, polycarboxylic acid compound and polyvinyl acid salt.
Further, the addition amount of the dispersing agent in the step 1) is 1-5% of the mass of the zinc oxide.
Further, the stirring and dispersing uniformly in the step 1) means dispersing for 15-30 min under the condition that the stirring rotating speed is 100-300 rpm; the wet grinding is grinding for 8-12 h under the condition that the rotating speed of a grinding machine is 1000-1500 rpm.
Further, the solid content of the slurry I in the step 1) is 40% -80%, the slurry granularity D50 is 0.1-0.5 μm, and the D90 is 0.1-1.5 μm.
Further, the mass ratio of the indium oxide powder to the zinc oxide powder is 77.5-90:10-22.5.
Further, the addition amount of the dispersing agent in the step 2) is 0.1-5% of the total mass of zinc oxide and indium oxide.
Further, the stirring and dispersing uniformly in the step 2) means dispersing for 15-30 min under the condition that the stirring rotating speed is 100-300 rpm; the wet grinding is grinding for 10-15 h under the condition that the rotating speed of a grinding machine is 1000-1500 rpm.
Further, the solid content of the second slurry in the step 2) is 40-80%, the slurry granularity D50 is less than or equal to 0.2 mu m, and D90 is less than or equal to 0.6 mu m.
Further, the binder in the step 3) is one or more of polyvinyl alcohol (PVA), polyethylene glycol (PEG) and polyvinyl butyral (PVB); the addition amount of the binder is 15-26% of the total mass of the zinc oxide powder, the indium oxide powder and the binder.
Further, in the step 3), the stirring and dispersing are carried out uniformly, namely, dispersing for 15-30 min under the condition that the stirring rotation speed is 100-300 rpm; the wet grinding is grinding for 3-5 h under the condition that the rotating speed of a grinding machine is 1000-1500 rpm.
Further, the spray granulation in the step 4) refers to spray granulation by adopting a flow spray drying tower, wherein the air outlet temperature is 60-70 ℃, and the frequency of an atomizer is 25-30 Hz.
Further, in the step 5), the dry pressing pressure is 90MPa, and the cold isostatic pressing pressure is 360-400 MPa; and (3) after the target embryo is obtained by cold isostatic pressing, heating to 200-500 ℃ for degreasing treatment for 1-3 h, and then cooling to room temperature.
Further, in the step 5), the sintering temperature is 1300-1500 ℃, the heating rate is 0.1-0.5 ℃/min, and the heat preservation time is 10-15 h; sintering is performed under an oxygen atmosphere.
Further preferably, the preparation steps of the indium zinc oxide target material are as follows:
a) Adding zinc oxide powder and a dispersing agent into water, stirring and dispersing uniformly, and then grinding by a wet method to obtain small-particle-size slurry with the slurry granularity D50 less than or equal to 0.2 mu m and the slurry granularity D90 less than or equal to 0.6 mu m;
b) Adding indium oxide powder and a dispersing agent into water, stirring and dispersing uniformly, and then grinding by a wet method to obtain large-particle-size slurry with the granularity D50 being more than 0.2 mu m and less than or equal to 0.5 mu m and the granularity D90 being more than 0.6 mu m and less than or equal to 1 mu m;
c) Mixing the small-particle-size slurry in the step a) with the large-particle-size slurry in the step b), adding a binder, and uniformly stirring and dispersing to obtain mixed slurry;
d) Granulating the mixed slurry obtained in the step c) by spraying to obtain IZO powder;
e) And sintering the IZO powder after dry pressing and cold isostatic pressing to obtain the indium zinc oxide target.
Compared with the prior art, the invention has the beneficial effects that:
(1) The IZO target material has high-proportion ZnO addition, can achieve higher density and conductivity, and can remarkably reduce the use amount of metal indium.
(2) The invention further adopts the preparation process of mixing and granulating the slurry with large and small particle sizes, and the particles with large and small particle sizes can be more tightly contacted with each other after being mixed by the slurry, and the density and the conductivity of the target material can be obviously improved through verification.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
(1) 8000G of indium oxide powder and 2000g of zinc oxide powder were weighed, wherein the average grain size of the indium oxide powder was 2. Mu.m, and the average grain size of the zinc oxide powder was 3. Mu.m.
(2) 1800G of pure water and 50g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel, and the mixture is stirred uniformly to be fully dissolved. Wherein, the polyvinylpyrrolidone dispersing agent accounts for 2.5 percent of the mass of the zinc oxide powder.
(3) And (3) adding the zinc oxide powder weighed in the step (1) into the solution in the step (2) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. And (3) pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding, wherein the grinding speed is 1300rpm, and the grinding time is 8 hours, so as to obtain slurry I. Malvern assay slurry particle size d50=0.361 μm, d90=0.687 μm.
(4) Weighing 500g of polyvinylpyrrolidone dispersing agent and 3500g of pure water, adding into the slurry I, stirring for pre-dispersing for 15min, adding the indium oxide powder weighed in the step (1) into the slurry after uniform dispersing, and dispersing for 30min. Wherein, the mass of the polyvinylpyrrolidone dispersing agent accounts for 5% of the total mass of the indium oxide and zinc oxide powder; the dispersion speed was 300rpm and the dispersion time was 30min. And (3) pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding, wherein the grinding speed is 1300rpm, and the grinding time is 10 hours, so as to obtain slurry II. Malvern assay slurry particle size d50=0.175 μm, d90=0.591 μm.
(5) Adding a mixture of a binder PVA and PEG into the slurry II obtained in the step (4) for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing rotating speed is 500rpm; pumping the dispersed slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry III. Wherein the grinding time is 5 hours, the grinding rotating speed is 1300rpm, and the binder accounts for 15% of the total mass of the added powder and the binder.
(6) And (3) carrying out spray granulation on the slurry III obtained in the step (5) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein, the air outlet temperature is 68 ℃, and the atomizer frequency is 25Hz.
(7) And (3) dry-pressing the IZO target precursor obtained in the step (6) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained target blank, degreasing at 500 ℃ (keeping the temperature for 2 hours, and then cooling to room temperature, introducing oxygen (40L/min) to raise the temperature for sintering, wherein the sintering temperature is 1400 ℃, the heating rate is 0.3 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the target material obtained by testing is 98.57%, and the conductivity of the target material is 1502s/cm.
Example 2
(1) 7750G of indium oxide powder and 2250g of zinc oxide powder were weighed for use, wherein the average grain size of the indium oxide powder was 2 μm and the average grain size of the zinc oxide powder was 3. Mu.m.
(2) 2500G of pure water and 150g of polyvinylpyrrolidone dispersing agent were added to the slurry tank and stirred well. Wherein the dispersing time is 30min, the dispersing rotating speed is 300rpm, and the polyvinylpyrrolidone dispersing agent accounts for 6.67 percent of the mass of the zinc oxide powder.
(3) And (3) adding the zinc oxide powder weighed in the step (1) into the solution in the step (2) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. The slurry obtained was pumped into a sand mill using a pneumatic diaphragm pump at a grinding speed of 1400rpm for 8 hours to obtain slurry one. Malvern assay slurry particle size d50=0.398 μm, d90=0.648 μm.
(4) And (3) adding 500g of the indium oxide powder weighed in the step (1) and 2500g of polyvinylpyrrolidone dispersing agent and pure water into the slurry I, and stirring for pre-dispersing. Wherein, the mass of the polyvinylpyrrolidone dispersing agent accounts for 5% of the total mass of the indium oxide and the zinc oxide powder; the dispersion speed was 300rpm and the dispersion time was 30min. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding, wherein the grinding speed is 1500rpm, and the grinding time is 8 hours, so as to obtain slurry II; malvern assay slurry particle size d50=0.156 μm, d90=0.512 μm.
(5) Adding a mixture of a binder PVA and PEG into the slurry II obtained in the step (4) for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing rotating speed is 300rpm; pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry III. Wherein the grinding time is 2.5 hours, the grinding rotating speed is 1500rpm, and the binder accounts for 12% of the total mass of the added powder and the binder.
(6) And (3) carrying out spray granulation on the slurry III obtained in the step (5) by using a parallel-flow spray drying tower to obtain an IZO target precursor. Wherein the air outlet temperature is 70 ℃, and the frequency of the atomizer is 25Hz.
(7) And (3) dry-pressing the IZO target precursor obtained in the step (6) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained IZO target blank, degreasing at the temperature of 450 ℃ (keeping the temperature for 2.5 hours, and heating the material at the rate of 0.5 ℃/min), cooling the material to room temperature, introducing oxygen (40L/min), raising the sintering temperature to sinter the material, wherein the sintering temperature is 1410 ℃, the heating rate is 0.5 ℃/min, and the keeping the temperature for 10 hours to obtain the IZO target material. The relative density of the target material obtained by testing is 98.89%, and the conductivity of the target material is 1356s/cm.
Example 3
(1) 8300G of indium oxide powder, 1700g of zinc oxide powder, in which the average grain size of the indium oxide powder was 2 μm and the average grain size of the zinc oxide powder was 3 μm, were weighed.
(2) 2000G of pure water and 60g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel and stirred uniformly to be fully dissolved. Wherein, the polyvinylpyrrolidone dispersing agent accounts for 3.5 percent of the mass of the zinc oxide powder.
(3) And (3) adding the zinc oxide powder weighed in the step (1) into the solution in the step (2) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry I. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 8 hours; malvern assay slurry particle size d50=0.298 μm, d90=0.701 μm.
(4) And (3) weighing 540g of polyvinylpyrrolidone dispersing agent and 3600g of pure water, adding into the slurry I, stirring for pre-dispersing for 30min, and adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing. Wherein, the mass of the polyvinylpyrrolidone dispersing agent accounts for 5.4 percent of the total mass of the indium oxide and zinc oxide powder; the dispersion speed was 300rpm and the dispersion time was 30min. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain a slurry II. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 12 hours; malvern assay slurry particle size d50=0.137 μm, d90=0.598 μm.
(5) Adding a mixture of a binder PVA and PEG into the slurry II obtained in the step (4) for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing rotating speed is 300rpm; pumping the dispersed slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry III. Wherein the grinding time is 8 hours, the grinding rotating speed is 1300rpm, and the binder accounts for 18% of the total mass of the added powder and the binder.
(6) And (3) carrying out spray granulation on the slurry III obtained in the step (5) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein, the air outlet temperature is 68 ℃, and the atomizer frequency is 25Hz.
(7) And (3) dry-pressing the IZO target precursor obtained in the step (6) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained IZO target blank, degreasing at 500 ℃ (keeping the temperature for 2 hours, and then cooling to room temperature, introducing oxygen (40L/min) to raise the temperature for sintering, wherein the sintering temperature is 1425 ℃, the heating rate is 0.4 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the target material obtained by testing is 98.74%, and the conductivity of the target material is 1621s/cm.
Example 4
(1) 8500G of indium oxide powder and 1500g of zinc oxide powder were weighed, wherein the average grain size of the indium oxide powder was 2 μm and the average grain size of the zinc oxide powder was 3 μm.
(2) 2200G of pure water and 66g of polyvinylpyrrolidone dispersing agent were added to the slurry tank and stirred uniformly to be sufficiently dissolved. Wherein, the polyvinylpyrrolidone dispersing agent accounts for 4.4 percent of the mass of the zinc oxide powder.
(3) And (3) adding the zinc oxide powder weighed in the step (1) into the solution in the step (2) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry I. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 8 hours; malvern assay slurry particle size d50=0.271 μm, d90=0.654 μm.
(4) Adding 580g of polyvinylpyrrolidone dispersing agent and 4100g of pure water into the slurry I, stirring for pre-dispersing for 30min, and adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing. Wherein, the mass of the polyvinylpyrrolidone dispersing agent accounts for 5.8 percent of the total mass of the indium oxide and zinc oxide powder; the dispersion speed was 500rpm and the dispersion time was 30min. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain a slurry II. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 12 hours; malvern assay slurry particle size d50=0.124 μm, d90=0.601 μm.
(5) Adding a mixture of a binder PVA and PEG into the slurry II obtained in the step (4) for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing rotating speed is 300rpm; pumping the dispersed slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry III. Wherein the grinding time is 8 hours, the grinding rotating speed is 1300rpm, and the binder accounts for 21% of the total mass of the added powder and the binder.
(6) And (3) carrying out spray granulation on the slurry III obtained in the step (5) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein the air outlet temperature is 70 ℃, and the frequency of the atomizer is 25Hz.
(7) And (3) dry-pressing the IZO target precursor obtained in the step (6) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained IZO target blank, degreasing at 500 ℃ (the heat preservation time is 2.5 hours, the heating rate is 0.5 ℃/min), cooling to room temperature, introducing oxygen (40L/min), increasing the temperature, sintering at 1435 ℃, the heating rate is 0.5 ℃/min, and the heat preservation time is 8 hours, so as to obtain the IZO target material. The relative density of the target material is 98.61%, and the conductivity of the target material is 1397s/cm.
Example 5
(1) 9000G of indium oxide powder, 1000g of zinc oxide powder, wherein the average grain size of the indium oxide powder was 2 μm and the average grain size of the zinc oxide powder was 3 μm, were weighed.
(2) 2350G of pure water and 70g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel, and the mixture is stirred uniformly to be fully dissolved. Wherein, the polyvinylpyrrolidone dispersing agent accounts for 7 percent of the mass of the zinc oxide powder.
(3) And (3) adding the zinc oxide powder weighed in the step (1) into the solution in the step (2) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry I. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 8 hours; malvern assay slurry particle size d50=0.264 μm, d90=0.703 μm.
(4) And (3) weighing 520g of polyvinylpyrrolidone dispersing agent and 3850g of pure water, adding into the slurry I, stirring for pre-dispersing for 30min, and adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing. Wherein, the mass of the polyvinylpyrrolidone dispersing agent accounts for 5.2 percent of the total mass of the indium oxide and zinc oxide powder; the dispersion speed was 300rpm and the dispersion time was 30min. Pumping the obtained slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain a slurry II. Wherein the grinding rotation speed is 1300rpm, and the grinding time is 12 hours; malvern assay slurry particle size d50=0.161 μm, d90=0.612 μm.
(5) Adding a mixture of a binder PVA and PEG into the slurry II obtained in the step (4) for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing rotating speed is 300rpm; pumping the dispersed slurry into a sand mill by using a pneumatic diaphragm pump for grinding to obtain slurry III. Wherein the grinding time is 8 hours, the grinding rotating speed is 1300rpm, and the binder accounts for 26% of the total mass of the added powder and the binder.
(6) And (3) carrying out spray granulation on the slurry III obtained in the step (5) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein the air outlet temperature is 70 ℃, and the frequency of the atomizer is 25Hz.
(7) And (3) dry-pressing the IZO target precursor obtained in the step (6) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained IZO target blank, degreasing at 500 ℃ (keeping the temperature for 3 hours, and then cooling to room temperature, introducing oxygen to raise the temperature for sintering, wherein the sintering temperature is 1450 ℃, the heating rate is 0.4 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the tested target is 98.54%, and the conductivity of the target is 1580s/cm.
Example 6
Compared with the embodiment 1, the composition of the components is the same, and the preparation is carried out by adopting a process of mixing and granulating slurry with large and small particle diameters, and the specific steps are as follows:
(1) 8000g of indium oxide powder and 2000g of zinc oxide powder were weighed, wherein the average grain size of the indium oxide powder was 2. Mu.m, and the average grain size of the zinc oxide powder was 3. Mu.m.
(2) 1800G of pure water and 50g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel, and the mixture is stirred uniformly to be fully dissolved. Then adding the zinc oxide powder weighed in the step (1) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1500rpm for 12 hours to obtain a small particle size slurry having a slurry particle size d50=0.165 μm and d90=0.572 μm.
(3) Weighing 500g of polyvinylpyrrolidone dispersing agent and 3500g of pure water, stirring for pre-dispersing for 15min, adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing, wherein the dispersing speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1300rpm for 6 hours to obtain a large particle size slurry having a slurry particle size d50=0.384 μm and d90=0.740 μm.
(4) Mixing the small-particle-size slurry obtained in the step (2) with the large-particle-size slurry obtained in the step (3), and then adding a mixture of the binder PVA and PEG for pre-dispersion, wherein the pre-dispersion time is 30min, and the dispersion rotating speed is 500rpm, so as to obtain the mixed slurry. Wherein the binder comprises 15% of the total mass of the added powder and binder.
(5) And (3) carrying out spray granulation on the mixed slurry obtained in the step (4) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein, the air outlet temperature is 68 ℃, and the atomizer frequency is 25Hz.
(6) And (3) dry-pressing the IZO target precursor obtained in the step (5) by using a die with the thickness of 120mm, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained target blank, degreasing at 500 ℃ (keeping the temperature for 2 hours, and then cooling to room temperature, introducing oxygen (40L/min) to raise the temperature for sintering, wherein the sintering temperature is 1400 ℃, the heating rate is 0.3 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the target material obtained by testing is 99.52%, and the conductivity of the target material is 2230s/cm.
As can be seen from the comparison result of the embodiment and the embodiment 1, the compactness and the conductivity of the IZO target can be obviously improved through the preparation process of mixing and granulating the slurry with large and small particle sizes.
Comparative example 1
In this comparative example, as compared with example 6, a large particle size slurry was prepared using zinc oxide powder, and a small particle size slurry was prepared using indium oxide powder, specifically as follows:
(1) 8000g of indium oxide powder and 2000g of zinc oxide powder were weighed, wherein the average grain size of the indium oxide powder was 2. Mu.m, and the average grain size of the zinc oxide powder was 3. Mu.m.
(2) 1800G of pure water and 50g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel, and the mixture is stirred uniformly to be fully dissolved. Then adding the zinc oxide powder weighed in the step (1) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1300rpm for 8 hours to obtain a large particle size slurry having a slurry particle size d50=0.361 μm and d90=0.687 μm.
(3) Weighing 500g of polyvinylpyrrolidone dispersing agent and 3500g of pure water, stirring for pre-dispersing for 15min, adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing, wherein the dispersing speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1500rpm for 12 hours to obtain a small particle size slurry having a slurry particle size d50=0.168 μm and d90=0.559 μm.
(4) Mixing the large-particle-size slurry obtained in the step (2) with the small-particle-size slurry obtained in the step (3), and then adding a mixture of the binder PVA and PEG for pre-dispersion, wherein the pre-dispersion time is 30min, and the dispersion rotating speed is 500rpm, so as to obtain the mixed slurry. Wherein the binder comprises 15% of the total mass of the added powder and binder.
(5) And (3) carrying out spray granulation on the mixed slurry obtained in the step (4) by using a parallel-flow spray drying tower to obtain a precursor of the IZO target. Wherein, the air outlet temperature is 68 ℃, and the atomizer frequency is 25Hz.
(6) And (3) dry-pressing the IZO target precursor obtained in the step (5) by using a die with the thickness of 120mm, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained target blank, degreasing at 500 ℃ (keeping the temperature for 2 hours, and then cooling to room temperature, introducing oxygen (40L/min) to raise the temperature for sintering, wherein the sintering temperature is 1400 ℃, the heating rate is 0.3 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the target material obtained by testing is 98.86%, and the conductivity of the target material is 1752s/cm.
As can be seen from the comparison of the present comparative example with examples 1 and 6, the process of preparing the pellets by mixing the zinc oxide slurry with a large particle size in a low proportion and the indium oxide slurry with a small particle size in a high proportion has a limited effect of improving the compactness and conductivity of the IZO target.
Comparative example 2
In this comparative example, compared with example 6, the large particle size slurry and the small particle size slurry were spray granulated and then mixed, pressed and sintered, and the specific steps were as follows:
(1) 8000g of indium oxide powder and 2000g of zinc oxide powder were weighed, wherein the average grain size of the indium oxide powder was 2. Mu.m, and the average grain size of the zinc oxide powder was 3. Mu.m.
(2) 1800G of pure water and 50g of polyvinylpyrrolidone dispersing agent are added into the slurry barrel, and the mixture is stirred uniformly to be fully dissolved. Then adding the zinc oxide powder weighed in the step (1) to perform pre-dispersion. Wherein the pre-dispersion time is 30min and the pre-dispersion rotating speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1500rpm for 12 hours to obtain a small particle size slurry having a slurry particle size d50=0.165 μm and d90=0.572 μm.
(3) Weighing 500g of polyvinylpyrrolidone dispersing agent and 3500g of pure water, stirring for pre-dispersing for 15min, adding the indium oxide powder weighed in the step (1) into the slurry for dispersing for 30min after uniform dispersing, wherein the dispersing speed is 300rpm. The obtained slurry was pumped into a sand mill by a pneumatic diaphragm pump at a grinding speed of 1300rpm for 6 hours to obtain a large particle size slurry having a slurry particle size d50=0.384 μm and d90=0.740 μm.
(4) And (3) adding the mixture of the binder PVA and the PEG into the small-particle-size slurry obtained in the step (2) and the large-particle-size slurry obtained in the step (3) respectively for pre-dispersing, wherein the pre-dispersing time is 30min, and the dispersing speed is 500rpm. Wherein the binder comprises 15% of the total mass of the added powder and binder. And (3) respectively carrying out spray granulation on the small-particle-size slurry and the large-particle-size slurry obtained in the step, wherein the air outlet temperature is 68 ℃, and the frequency of an atomizer is 25Hz, so as to obtain large-particle-size granulated powder and small-particle-size granulated powder. And then mixing the large-particle-size granulated powder and the small-particle-size granulated powder to obtain the precursor of the IZO target.
(5) And (3) dry-pressing the IZO target precursor obtained in the step (4) by using a 120mm die, wherein the pressure is 90MPa. And then carrying out cold isostatic pressing, wherein the pressure is 360-400 MPa, and obtaining the target embryo. And (3) performing heat treatment on the obtained target blank, degreasing at 500 ℃ (keeping the temperature for 2 hours, and then cooling to room temperature, introducing oxygen (40L/min) to raise the temperature for sintering, wherein the sintering temperature is 1400 ℃, the heating rate is 0.3 ℃/min, and the keeping the temperature for 8 hours to obtain the IZO target. The relative density of the target material obtained by testing is 98.90%, and the conductivity of the target material is 1825s/cm.
As can be seen from the comparison result of the comparative example and the example 6, the preparation process of the invention can remarkably improve the compactness and the conductivity of the IZO target by adopting the mode of mixing large-grain size and small-grain size powder compared with the mode of mixing large-grain size and small-grain size slurry.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (7)

1. The preparation method of the indium zinc oxide target material is characterized In that the indium zinc oxide target material consists of indium oxide and zinc oxide, and the atomic ratio of Zn to In the target material is Zn/(Zn+In) =18-50%;
The preparation method comprises the following preparation steps:
a) Adding zinc oxide powder and a dispersing agent into water, stirring and dispersing uniformly, and then grinding by a wet method to obtain small-particle-size slurry with the slurry granularity D50 less than or equal to 0.2 mu m and the slurry granularity D90 less than or equal to 0.6 mu m;
b) Adding indium oxide powder and a dispersing agent into water, stirring and dispersing uniformly, and then grinding by a wet method to obtain large-particle-size slurry with the granularity D50 being more than 0.2 mu m and less than or equal to 0.5 mu m and the granularity D90 being more than 0.6 mu m and less than or equal to 1 mu m;
c) Mixing the small-particle-size slurry in the step a) with the large-particle-size slurry in the step b), adding a binder, and uniformly stirring and dispersing to obtain mixed slurry;
d) Granulating the mixed slurry obtained in the step c) by spraying to obtain IZO powder;
e) And sintering the IZO powder after dry pressing and cold isostatic pressing to obtain the indium zinc oxide target.
2. The method for preparing the indium zinc oxide target according to claim 1, wherein the dispersing agent is one or more selected from polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium hexadecyl benzene sulfonate, polycarboxylic acid compound and polyvinyl acid salt; the mass ratio of the indium oxide powder to the zinc oxide powder is 77.5-90:10-22.5.
3. The method for preparing the indium zinc oxide target according to claim 1, wherein the adding amount of the dispersing agent in the step a) is 1% -5% of the mass of the zinc oxide; the stirring and dispersing are carried out uniformly, namely, dispersing for 15-30 min under the condition that the stirring rotation speed is 100-300 rpm; the wet grinding is carried out for 8-12 hours under the condition that the rotating speed of a grinding machine is 1000-1500 rpm.
4. The method for preparing an indium zinc oxide target according to claim 1, wherein the addition amount of the dispersing agent in the step b) is 0.1% -5% of the total mass of zinc oxide and indium oxide; the stirring and dispersing are carried out uniformly, namely, dispersing for 15-30 min under the condition that the stirring rotation speed is 100-300 rpm; the wet grinding is carried out for 10-15 hours under the condition that the rotating speed of a grinding machine is 1000-1500 rpm.
5. The method for preparing an indium zinc oxide target according to claim 1, wherein the binder in step c) is one or more of polyvinyl alcohol, polyethylene glycol, and polyvinyl butyral; the addition amount of the binder is 15% -26% of the total mass of the zinc oxide powder, the indium oxide powder and the binder; the stirring and dispersing uniformly means dispersing for 15-30 min under the condition that the stirring rotation speed is 100-300 rpm.
6. The method for preparing an indium zinc oxide target according to claim 1, wherein in the step d), the spray granulation is performed by a flow type spray drying tower, wherein the air outlet temperature is 60-70 ℃, and the frequency of an atomizer is 25-30 Hz; in the step e), the dry pressing pressure is 90MPa, and the cold isostatic pressing pressure is 360-400 MPa; after the target blank is obtained by cold isostatic pressing, heating to 200-500 ℃ for degreasing treatment for 1-3 hours, and then cooling to room temperature; in the step e), the sintering temperature is 1300-1500 ℃, the heating rate is 0.1-0.5 ℃/min, and the heat preservation time is 10-15 h; sintering is performed under an oxygen atmosphere.
7. The method for preparing an indium zinc oxide target according to claim 1, wherein the relative density of the indium zinc oxide target is more than 98.5%, and the conductivity is more than 1350s/cm.
CN202211616872.1A 2022-12-15 2022-12-15 Indium zinc oxide target and preparation method thereof Active CN116162908B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211616872.1A CN116162908B (en) 2022-12-15 2022-12-15 Indium zinc oxide target and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211616872.1A CN116162908B (en) 2022-12-15 2022-12-15 Indium zinc oxide target and preparation method thereof

Publications (2)

Publication Number Publication Date
CN116162908A CN116162908A (en) 2023-05-26
CN116162908B true CN116162908B (en) 2024-08-30

Family

ID=86415423

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211616872.1A Active CN116162908B (en) 2022-12-15 2022-12-15 Indium zinc oxide target and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116162908B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116639956B (en) * 2023-06-09 2024-08-30 先导薄膜材料（广东）有限公司 High-mobility indium titanium cerium tantalum oxide target and preparation method thereof
CN117049870A (en) * 2023-08-11 2023-11-14 先导薄膜材料（广东）有限公司 Indium zinc oxide evaporation target material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101198565A (en) * 2005-07-01 2008-06-11 出光兴产株式会社 Manufacturing method of IZO sputtering target
KR20090052008A (en) * 2007-11-20 2009-05-25 삼성코닝정밀유리 주식회사 Zinc oxide target and its manufacturing method
CN103531638A (en) * 2012-06-29 2014-01-22 三星康宁精密素材株式会社 Thin-film transistor and zinc oxide-based sputtering target for the same
CN107267936A (en) * 2016-03-31 2017-10-20 捷客斯金属株式会社 Indium oxide is Zinc-oxide-based（IZO）Sputtering target and its manufacture method
CN107614741A (en) * 2016-03-31 2018-01-19 捷客斯金属株式会社 IZO sintered body sputtering target and manufacturing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101198565A (en) * 2005-07-01 2008-06-11 出光兴产株式会社 Manufacturing method of IZO sputtering target
KR20090052008A (en) * 2007-11-20 2009-05-25 삼성코닝정밀유리 주식회사 Zinc oxide target and its manufacturing method
CN103531638A (en) * 2012-06-29 2014-01-22 三星康宁精密素材株式会社 Thin-film transistor and zinc oxide-based sputtering target for the same
CN107267936A (en) * 2016-03-31 2017-10-20 捷客斯金属株式会社 Indium oxide is Zinc-oxide-based（IZO）Sputtering target and its manufacture method
CN107614741A (en) * 2016-03-31 2018-01-19 捷客斯金属株式会社 IZO sintered body sputtering target and manufacturing method thereof

Also Published As

Publication number Publication date
CN116162908A (en) 2023-05-26

Similar Documents

Publication Publication Date Title
CN116162908B (en) Indium zinc oxide target and preparation method thereof
CN116199496B (en) Indium zinc oxide doped rare earth metal target material and preparation method thereof
CN101580384B (en) Yttrium-doped AZO target and preparation method thereof
CN114524664B (en) A kind of ceramic target material for solar cell and preparation method thereof
CN115650701B (en) Preparation method and application of nickel oxide-based target
CN104376894A (en) Solar cell conductive positive silver pulp
CN103739282A (en) Preparation method of trace element composite doping modified tin antimony oxide (ATO) ceramic target
CN116219375B (en) Indium zinc oxide target and preparation method thereof
CN102181826B (en) Gallium-molybdenum-codoped indium tin oxide ceramic target, gallium-molybdenum-codoped indium tin oxide transparent conductive film and preparation method
KR101404404B1 (en) Method for manufacturing zinc oxide target and zinc oxide target by using the same
CN117185781A (en) Indium gallium aluminum oxide powder, target material, powder and preparation method of target material
CN114436641B (en) Magnetron sputtering ceramic target material and preparation method thereof
CN114277334B (en) Indium tin tantalum ytterbium oxide powder and preparation method and application thereof
CN104561914A (en) Method for preparing molybdenum target
KR101264078B1 (en) Sintered zinc oxide and method of manufacturing the same
CN103193475A (en) Study of preparation technology of AZO composite target material with high performance and low cost
CN113087519A (en) Conductive zinc-tin oxide target material and preparation method and application thereof
CN117049870A (en) Indium zinc oxide evaporation target material and preparation method thereof
CN105924150A (en) Low-temperature sintered conductive ceramic material and preparation method thereof
CN118547253B (en) Zinc oxide-based target material for RPD coating and preparation method thereof
CN117362006B (en) Preparation method of rare earth ion doped ITO target
CN117486599A (en) Tin oxide target for heterojunction battery and preparation method thereof
CN117229051B (en) LaTb co-doped ITO target material and preparation method and application thereof
CN108538434A (en) A kind of low migration electrode slurry of silver and preparation method of organically-modified solar cell
CN105801107A (en) High-performance conductive ceramic material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant