CN112481592A - Hot press molding preparation method of nickel oxide-based ceramic target material - Google Patents

Hot press molding preparation method of nickel oxide-based ceramic target material Download PDF

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CN112481592A
CN112481592A CN202011268698.7A CN202011268698A CN112481592A CN 112481592 A CN112481592 A CN 112481592A CN 202011268698 A CN202011268698 A CN 202011268698A CN 112481592 A CN112481592 A CN 112481592A
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group
mass
nickel oxide
doping source
powder
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高明
张虎
张花蕊
杨本润
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Beijing Orient Co ltd
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Beijing Hangda Micro Technology Co ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/085—Oxides of iron group metals
    • 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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  • Chemical Kinetics & Catalysis (AREA)
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to a hot-press forming preparation method of a nickel oxide-based ceramic target material, which is characterized by comprising the following steps of: preparing raw materials; b, spray drying; c, putting the mixed powder prepared in the step B into a hot-pressing die; d, pre-pressurizing and degassing the die; e, hot-pressing sintering: the pressure is 5-100MPa, the vacuum degree is 0.1-10Pa, the sintering temperature is 600-; d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank; e with or without machining as required. The nickel oxide-based ceramic target material with good conductivity, high purity and fine grain size can be prepared by the method, and the method can realize net size forming and has high efficiency.

Description

Hot press molding preparation method of nickel oxide-based ceramic target material
Technical Field
The invention relates to a preparation method of a ceramic target material, in particular to a hot press molding preparation method of a nickel oxide-based ceramic target material.
Background
Nickel oxide is a P-type transition group wide bandgap semiconductor material with a 3d outermost electronic structure, and has excellent chemical stability and certain special photoelectric properties. At present, the nickel oxide film has great application potential, including a P-type transparent conductive film, an electrochromic film, a catalytic film, a magnetic film and the like.
In order to prepare the film, the nickel oxide-based ceramic target is prepared by a coating method such as magnetron sputtering and the like, so that the method has an application prospect. However, the nickel oxide-based ceramic in the prior art has poor conductivity, so that the conductivity of the prepared nickel oxide film is poor, and the development of the nickel oxide film in the application field needing to utilize the conductivity of the nickel oxide film, such as a P-type transparent conductive film, an electrochromic film and the like, is restricted.
In addition, in terms of coating process performance, the nickel oxide-based ceramic target material in the prior art has low purity, generally below 99.9%, poor conductivity, and only high-cost radio frequency sputtering equipment can be adopted as an insulator; meanwhile, the crystal grain size is too large and uneven, so that the film coating process is unstable, the phenomenon of sparking and reverse sputtering is serious, the thickness of the film is uneven, the electrical property of the film is poor, the dyeing property is unstable, and the film-making cost is too high. The low density of the target material can cause the instability of the coating process and the poor performance of the coating.
Therefore, a nickel oxide-based ceramic target material with good conductivity, high purity and fine grain size is required for the wide application of the nickel oxide thin film. However, the nickel oxide-based ceramic target material cannot be prepared in the prior art.
Disclosure of Invention
The invention aims to solve the technical problem of providing a hot-press forming preparation method for preparing a nickel oxide-based ceramic target material with good conductivity, high purity and fine grain size aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a hot press molding preparation method of a nickel oxide based ceramic target material is characterized by comprising the following steps:
preparing raw materials: the mixed powder comprises nickel oxide powder and doping source powder, wherein the total mass fraction of doping source elements in the mixed powder is not higher than 10%, the doping source elements are selected from one or more of Li, Na, Mg, Al, Si, K, Zn, Zr, Mn, Cu, Cr, V, W and Ti, and the mass fraction range of the selected corresponding elements is as follows: 0-6% by mass of Li element, 0-0.3% by mass of Na element, 0-1.0% by mass of Mg element, 0-0.1% by mass of Al element, 0-0.1% by mass of Si element, 0-0.15% by mass of K element, 0-12% by mass of Zn element, 0-1.5% by mass of Zr element, 0-1.2% by mass of Mn element, 0-10% by mass of Cu element, 0-1.2% by mass of Cr element, 0-0.3% by mass of V element, 0-10% by mass of W element, and 0-2.5% by mass of Ti element; the purity of the nickel oxide powder and the doping source powder is higher than 99.99%, the average grain diameter is 500nm-2 mu m, and the grain diameter of D50 is 50nm-800 nm;
b, spray drying: carrying out spray drying treatment on the mixed powder;
c, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die; preferred pre-pressurization parameters are: 1-2MPa for 1-2 hours.
E, hot-pressing sintering: the pressure is 5-100MPa, the vacuum degree is 0.1-10Pa, the sintering temperature is 600-;
preferably, the doping source elements are at least three elements selected from Li, Na, Mg, Al, Si, K, Zn, Zr, Mn, Cu, Cr, V, W and Ti.
Preferably, the pressure is 10-70MPa, the vacuum degree is 0.5-8Pa, the hot pressing temperature is 650-900 ℃, the heat preservation time is 2.5-4.5, and the temperature rising speed is 1.0-2.5 ℃/min;
further preferably, the pressure is 30MPa, the vacuum degree is 1.0Pa, the hot pressing temperature is 750 ℃, the heat preservation time is 3 hours, and the temperature rising speed is 1.2 ℃/min.
D, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
e with or without machining as required.
Preferably, the step B spray drying comprises the steps of:
(a) adding 0.5-5 times of liquid into the mixed powder to prepare slurry with 15-60% vol, and performing ball milling dispersion; further preferably, 4-5 times of volume of deionized water is added to prepare 17% -20% vol slurry; the liquid in the step is any one of proper liquids such as deionized water, alcohol, acetone, kerosene and the like;
(b) spray drying to obtain secondary powder particles;
(c) and sieving and refining the secondary powder.
For the purposes of the present invention, any number of dopant sources is selected and mixed in any proportion to increase the conductivity of the nickel oxide ceramic produced, in order to obtain better conductivity:
more preferably, the mass fraction of Li element is 0.05-5%, the mass fraction of Na element is 0.05-0.25%, the mass fraction of Mg element is 0.3-0.9%, the mass fraction of Al element is 0.01-0.09%, the mass fraction of Si element is 0.01-0.08%, the mass fraction of K element is 0.03-0.12%, the mass fraction of Zn element is 0.2-10%, the mass fraction of Zr element is 0.3-1.3%, the mass fraction of Mn element is 0.3-1.1%, the mass fraction of Cu element is 0.3-0.8%, the mass fraction of Cr element is 0.3-1.0%, the mass fraction of V element is 0.02-0.25%, the mass fraction of W element is 1.0-9.0%, and the mass fraction of Ti element is 0.05-2.3%.
Further preferred is: 0.05-2% by mass of Li element, 0.1-0.2% by mass of Na element, 0.4-0.8% by mass of Mg element, 0.02-0.08% by mass of Al element, 0.02-0.07% by mass of Si element, 0.05-0.1% by mass of K element, 0.4-8.0% by mass of Zn element, 0.4-1.1% by mass of Zr element, 0.5-1.0% by mass of Mn element, 0.4-0.7% by mass of Cu element, 0.5-0.8% by mass of Cr element, 0.05-0.20% by mass of V element, 2-8.0% by mass of W element, and 0.1-2.0% by mass of Ti element. It is further preferable for the Li element in the above range that the mass fraction of the Li element is 0.2 to 1.8%, and it is further preferable that the mass fraction of the Li element is 0.3 to 1.6%.
Preferably, the doping source element is selected from one of the following groups:
a first group: the doping source element is selected from one or more of Li, Zr, Ti and W elements;
second group: the doping source is selected from one or more of Li, Na, Zn and W;
third group: the doping source is selected from one or more of Li, Zr, Zn and Ti;
and a fourth group: the doping source is selected from one or more of Li, Zn, K, W and V;
and a fifth group: one or more of the doping sources W, Ti and Zr;
a sixth group: the doping source is selected from one or more of Li, Cu, Mn, Cr and Si;
a seventh group: the doping source is selected from one or more of Mg, Al, Zn and Ti;
and an eighth group: one or more of the doping sources Zr, Zn, Al and W;
ninth group: the doping source is selected from one or more of Li, Mg, Zn, Zr and Ti;
the tenth group: the doping source is selected from one or more of W, Zn, Na, K, Mg, Ti and Li.
Further preferably, the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w ═ 0-2: (0-2): (0-1): (0-5);
second group: li: na: zn: w ═ 0-2: (0-1): (0-2);
third group: li: zr: zn: ti ═ 0-2: (0-2): (0-5): (0-2);
and a fourth group: li: zn: k: w: v ═ 0-2, (0-1), (0-2), (0-1);
and a fifth group: w: ti: zr ═ 0-5: (0-2): (0-2);
a sixth group: li: cu: mn: cr: si ═ 0-2: (0-1): (0-1);
a seventh group: mg: al: zn: ti (0-5): 0-0.5): 0-5): 0-2;
and an eighth group: zr: zn: al: w ═ 0-2: (0-5): (0-0.5): (0-5);
ninth group: li: mg: zn: zr: ti (0-2), (0-1), (0-5), (0-0.5) and (0-2).
Further preferably, the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w ═ (0.5-1.8): (0.5-1.8): (0.05-0.9): (0.5-4.5);
second group: li: na: zn: w ═ 0.5-1.5, (0-1), (0.5-1.5);
third group: li: zr: zn: ti ═ 0.5 to 1.8: (0.5-1.8): (0.5-4.5): (0.05-1.8);
and a fourth group: li: zn: k: w: v ═ 0.5-2, (0-1), (0.5-2), (0-1);
and a fifth group: w: ti: zr ═ 0.5 to 4.5: (0.5-1.8): (0.05-1.8);
a sixth group: li: cu: mn: cr: si is (0.5-2), (0-1), (0:0.5), (0-0.5) and (0-0.5);
a seventh group: mg: al: zn: ti (0.5-2.5): 0.05-0.3): 0.5-3.5): 0.5-1.5);
and an eighth group: zr: zn: al: w ═ (0.5-1.8): (0.5-4.5): (0.01-0.45): (0.5-4.5);
ninth group: li: mg: zn: zr: ti (0.5-1.5), (0.2-0.75), (0.5-3.5), (0.05-0.3), (0-2).
Further preferably, the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w is 1:1:0.4: 3;
second group: li: na: zn: w is 1:0.5:0.8: 1.2;
third group: li: zr: zn: and Ti is 1:1:3: 1;
and a fourth group: li: zn: k: w: v ═ 1.2:0.6:0.2:1: 0.2;
and a fifth group: w: ti: zr ═ 2.5:1: 0.5;
a sixth group: li: cu: mn: cr: si ═ 1.5:0.5:0.1:0.1: 0.01;
a seventh group: mg: al: zn: ti 1.5:0.1:2.5: 1;
and an eighth group: zr: zn: al: w is 1:3:0.1: 3;
ninth group: li: mg: zn: zr: ti is 1:0.5:2.5:0.15: 1.
In order to obtain better conductivity, the nickel oxide powder and the doping source powder both have an average particle size of 700nm-1.5 μm, and the D50 particle size is 350-700 nm. More preferably, the nickel oxide powder and the doping source powder both have an average particle size of 800 μm-1.3 μm, and the D50 particle size is 300-600 nm. More preferably, the nickel oxide powder and the dopant source powder both have an average particle size of 1 μm, and the D50 particle size is 0.4 μm.
Preferably, the mass fraction of the doping source is not higher than 8%. Further preferably, the mass fraction of the doping source is not higher than 5%.
Preferably, each element of the doping source is selected from corresponding simple substance metal, alloy, inorganic salt, organic salt or oxide. However, because some metal elements such as Li, Na, K and the like have high activity, and enter into slurry to perform chemical reaction with water, the danger is high, and if metal simple substances and alloys with low activity are added, the time for oxidation to oxides is long, and the ball milling time needs to be prolonged, therefore, it is further preferable that each element of the doping source is selected from corresponding inorganic salts or oxides. The inorganic salt of each element of the doping source is selected from corresponding nitrate, carbonate, fluoride salt or bicarbonate and the like. The organic salt of each element of the doping source is selected from corresponding acetate, oxalate or citrate.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the conductivity of the prepared nickel oxide-based ceramic is improved by doping a doping source, and the density of holes generated by a p-type semiconductor is obviously improved by adding IA main group elements such as Li, Na, Mg, K and the like, so that the conductivity is improved; transition elements such as Al, Si, Zn, Zr, Mn, Cu, Cr, V, W and the like are added, so that the hole density can be improved, the conductivity is improved, and the ceramic material becomes a sintering aid and is beneficial to improving the density of the ceramic;
the purity of the nickel oxide powder and the doping source powder is higher than 99.99 percent, the average grain diameter is 500nm-2 mu m, the grain diameter of D50 is 50-800nm, the powder has high purity and the grain diameter reaches the nanometer level, so the activity of the powder is improved, the activation energy of powder grains is greatly improved, the sintering temperature is reduced, a ceramic block with smaller grains and higher density can be obtained under the same sintering process, the defect rate in the block is reduced, a cavity is easier to move, and the conductivity of the ceramic prepared by using the powder is improved;
2. the invention adopts the hot-press forming method to prepare the nickel oxide ceramic, the hot-press forming can bring the highest compactness and the finest size combination of nickel oxide grains, meanwhile, the hot-press forming has great advantages for preparing the laboratory size plane target material, can realize the near net size forming, is convenient for accurately controlling the size, can finish all the working procedures within 12 hours, and has higher efficiency. And meanwhile, the hot-press forming die is mostly made of graphite, so that a reducing atmosphere can be provided in the hot-press process, the stroke of the internal cavity of the nickel oxide is facilitated, and the conductivity is improved.
3. The introduction of the spray drying process is beneficial to improving the powder fluidity and the bulk density and improving the sintering performance.
4. The parameters of the hot-pressing sintering in the step E are as follows: the pressure is 5-100MPa, the vacuum degree is 0.1-10Pa, the hot-pressing temperature is 600-.
The pressure intensity is 5-100MPa, and the proper pressure intensity can provide stable plastic deformation and full contact of the powder particles, so that high density is brought. Too low pressure causes low density, and too many air holes in the target affect the sputtering effect.
The hot pressing temperature is 600 ℃ and 950 ℃, the heat preservation time is 2-5, the optimal combination of grain size and density can be realized at a proper hot pressing temperature, the density is too low due to too low hot pressing temperature, the grain growth is insufficient, the density difference of the inner part and the outer part of the target material is too large, too high hot pressing temperature can cause too large grain size and too many oxygen vacancies, the density is not high, and simultaneously, a direct and severe interface reaction between the mold and the ceramic can be caused. The choice of incubation time also has similar effects.
Therefore, the nickel oxide-based ceramic target material finally prepared by the invention comprises the following components in percentage by weight: the purity of the raw material powder is more than 99.99 percent, the average grain size is 1-10 mu m, the doped phase size is 0-800nm, the density is more than 98 percent, and the conductivity is more than 15S/cm. The ceramic target material has good conductivity, so that the film prepared by using the target material also has good conductivity, and industrial application of a P-type transparent conductive film, an electrochromic film and the like which need to use the conductivity of a nickel oxide film becomes possible; in addition, in terms of coating process performance, the target material has high conductivity, low-cost direct current sputtering equipment can be directly adopted, and the film-making cost is reduced; the grain size is reduced, the distribution of the doped phase is uniform, the density of the target material is improved, the coating process is stable, the phenomenon of sparking and back sputtering is prevented, the thickness of the film is more uniform, the strength of the ceramic structure is improved, the target material can bear higher power density during sputtering, and faster deposition rate is obtained.
Drawings
FIG. 1 is a photomicrograph of a nickel oxide powder of example 1 of the present invention;
FIG. 2 is an XRD spectrum of nickel oxide powder of example 1 of the present invention;
FIG. 3 is a PSD chart of nickel oxide powder according to example 1 of the present invention;
FIG. 4 is an electron micrograph of a nickel oxide-based target material according to example 1 of the present invention;
FIG. 5 is a photomicrograph of a nickel oxide powder of example 3 of the present invention;
FIG. 6 is a PSD chart of nickel oxide powder according to example 3 of the present invention;
FIG. 7 is a photomicrograph of nickel oxide powder of example 8 of the present invention;
FIG. 8 is a PSD chart of nickel oxide powder in example 8 of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The nickel oxide powders of the following examples were prepared by the following method:
(a) introducing oxygen into the high-purity nickel steam at 1600-1800 ℃ to form high nickel oxide;
(b) mixing high nickel oxide with a reducing agent, and roasting at the temperature of 500-1000 ℃ to obtain a nickel oxide block, wherein the reducing agent is high-purity graphite or reducing atmosphere such as carbon monoxide, hydrogen and the like;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder, wherein the specific process parameters are as follows: the ball-material ratio is 2: 1-4: 1, the average diameter of the grinding balls is 0.3mm-10mm, the volume of the grinding balls and the slurry accounts for 1/4-2/3 of the volume of the grinding chamber, and the ball-milling time is 10-20 hours to obtain the nickel oxide powder; the solvent selected by the wet ball milling is any one of proper conventional solvents such as deionized water, alcohol, acetone, kerosene and the like, and the material of the grinding ball is any one of proper conventional grinding ball materials such as zirconia, corundum, agate and the like.
The doping source powder of the following examples is commercially available, and each element is selected from corresponding elementary metal, alloy, inorganic salt, organic salt or oxide. However, because some metal elements such as Li, Na, K and the like have high activity, and enter into slurry to perform chemical reaction with water, the danger is high, and if metal simple substances and alloys with low activity are added, the time for oxidation to oxides is long, and the ball milling time needs to be prolonged, therefore, it is further preferable that each element of the doping source is selected from corresponding inorganic salts or oxides. The inorganic salt of each element of the doping source is selected from corresponding nitrate, carbonate, fluoride salt or bicarbonate and the like. The organic salt of each element of the doping source is selected from corresponding acetate, oxalate or citrate.
Example 1:
firstly, preparing nickel oxide powder:
(a) introducing oxygen into the high-purity nickel steam at 1650 ℃ to form high nickel oxide;
(b) mixing high nickel oxide with a high-purity graphite reducing agent, and roasting at 700 ℃ to obtain a nickel oxide block;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder: the ball-material ratio is 3:1, the average diameter of the grinding ball is 5mm, the volume of the grinding ball and the slurry accounts for 50% of the volume of the grinding chamber, the nickel oxide powder is obtained after ball milling for 15 hours, the purity of the obtained nickel oxide powder is 99.99%, a micrograph of the nickel oxide powder is shown in figure 1, an XRD (X-ray diffraction) spectrum of the nickel oxide powder is shown in figure 2, a PSD (phase-sensitive Detector) diagram of the nickel oxide powder is shown in figure 3, and the nickel oxide powder prepared in the embodiment has the average particle size of 1.0 mu m and the D50 particle size. The solvent used in the wet ball milling in this embodiment is any one of suitable conventional solvents such as deionized water, alcohol, acetone, kerosene, etc., and the material of the grinding ball is any one of the materials of conventional grinding balls such as zirconia, corundum, agate, etc.
Secondly, obtaining doping source powder: the doping source powder is purchased from commercial inorganic salt powder of corresponding elements, the purity is 99.99 percent, the average grain diameter is 1.0 mu m, and the grain diameter of D50 is 400 nm; the doping source powder can purchase other simple substance metals, alloy inorganic salts, organic salts and oxides of corresponding elements, and the effect is similar.
Thirdly, preparing nickel oxide-based ceramic:
preparing raw materials:
weighing nickel oxide powder and doping source powder with corresponding mass by using a digital electronic balance, uniformly mixing by wet ball milling to obtain nickel oxide-based mixed powder, wherein the mass fraction of the nickel oxide powder in the mixed powder is 95%, the mass fraction of the doping source is 5%, and the doping source comprises the following components in molar ratio of Li: zr: ti: w is 1:1:0.4: 3;
b, spray drying:
(a) adding deionized water with the volume being 4.5 times that of the mixed powder of nickel oxide powder and doping source powder with corresponding weight into the mixed powder to prepare slurry with the solid phase fraction being 18 percent vol, and performing ball milling for 18 hours for dispersion;
(b) spray drying the slurry at an inlet temperature of 300 ℃ and an outlet temperature of 100 ℃ to obtain secondary powder;
(c) the powder was sieved through a 80 mesh sieve.
To obtain a pileThe density was 1.52g cm-3The mixed powder of (1).
C, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing the die: degassing under the pressure of 1MPa for-2 hours;
e, hot-pressing sintering: the pressure is 10MPa, the vacuum degree is 7Pa, the sintering temperature is 700 ℃, the heat preservation time is 2h, and the temperature rise speed is 1 ℃/min;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
and E, machining according to the requirement to obtain a ceramic finished product.
The electron micrograph of the nickel oxide-based target material is shown in FIG. 4, the average grain size is 5 μm, the doped phase size is 120nm, the bulk conductivity is 35S/cm, and the relative density is 99.6% as measured by a drainage method.
Example 2:
this example differs from example 1 in that the dopant source components of the a feedstock preparation step are, in terms of mole ratios, Li: na: zn: w is 1:0.5:0.8: 1.2.
The average grain size of the obtained ceramic target finished product is 4 mu m, the doped phase size is 190nm, the bulk conductivity is 25S/cm, and the relative density is measured to be 99.1% by a drainage method.
Example 3:
firstly, preparing nickel oxide powder:
(a) introducing oxygen into the high-purity nickel steam at 1600 ℃ to form high nickel oxide;
(b) roasting the nickel oxide in hydrogen atmosphere at 1000 ℃ to obtain a nickel oxide block;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder: the ball-material ratio is 2:1, the average diameter of the grinding ball is 0.3mm, the volume of the grinding ball and the slurry accounts for 2/3 of the volume of the grinding chamber, and the nickel oxide powder is obtained after ball milling for 20 hours; the purity of the obtained nickel oxide powder was 99.995%, the photomicrograph of the nickel oxide powder prepared in this example is shown in fig. 5, the PSD chart is shown in fig. 6, the average particle size of the nickel oxide powder prepared in this example is 500nm, and the particle size of D50 is 50 nm. In the embodiment, deionized water is used as a solvent for wet ball milling, and zirconia or corundum is used as a grinding ball; besides, the materials of the conventional solvent and the grinding ball can be properly selected.
Second, obtaining of doping source powder the commercially available inorganic salt powder of the corresponding element was purchased, purity 99.995%, average particle size 500nm, and D50 particle size 50 nm. The doping source powder can purchase other simple substance metals, alloys, inorganic salts, organic salts and oxides of corresponding elements, and the effect is similar.
Thirdly, preparing nickel oxide-based ceramic:
preparing raw materials:
weighing nickel oxide powder and doping source powder with corresponding mass by using a digital electronic balance, mixing three-dimensionally to obtain nickel oxide-based mixed powder, wherein the mass fraction of the nickel oxide powder in the mixed powder is 97%, the mass fraction of the doping source is 3%, and the doping source comprises the following components in molar ratio of Li: zr: zn: ti 1:1:3: 1;
b, spray drying:
(a) adding deionized water with the volume 0.8 times that of the mixed powder of nickel oxide powder and doping source powder with corresponding weight into the mixed powder to prepare slurry with 56% vol solid phase fraction, and performing ball milling for 10 hours for dispersion;
(b) spray drying the slurry at an inlet temperature of 300 ℃ and an outlet temperature of 110 ℃ to obtain secondary powder;
(c) sieving the powder with a 60-mesh sieve;
obtaining a bulk density with a flowability parameter of 1.45g cm-3The mixed powder of (1).
C, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die;
e, hot-pressing sintering: the pressure is 30MPa, the vacuum degree is 3Pa, the sintering temperature is 750 ℃, the heat preservation time is 4h, and the temperature rise speed is 2 ℃/min;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
and E, machining according to the requirement to obtain a ceramic finished product.
The average grain size of the obtained ceramic target finished product is 3 mu m, the doped phase size is 70nm, the bulk conductivity is 18S/cm, and the relative density is measured to be 99.2% by a drainage method.
Example 4:
this example differs from example 3 in that the dopant source components of the a feedstock preparation step are, in terms of mole ratios, Li: zn: k: w: v ═ 1.2:0.6:0.2:1: 0.2;
the average grain size of the obtained ceramic target finished product is 2.5 mu m, the doped phase size is 130nm, the bulk conductivity is 22S/cm, and the relative density is measured to be 99.0% by a drainage method.
Example 5:
firstly, preparing nickel oxide powder:
(a) introducing oxygen into high-purity nickel steam at 1800 ℃ to form high nickel oxide;
(b) mixing nickel oxide with a reducing agent, and roasting at 500 ℃ in a carbon monoxide reducing atmosphere to obtain a nickel oxide block;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder: the ball-material ratio is 4:1, the average diameter of the grinding ball is 7mm, the volume of the grinding ball and the slurry accounts for 1/4 of the volume of the grinding chamber, and the nickel oxide coarse powder is subjected to ball milling for 20 hours to obtain nickel oxide powder; the purity of the obtained nickel oxide powder was 99.99%, the average particle size of the nickel oxide powder prepared in this example was 0.8 μm, and the particle size of D50 was 0.5 μm;
secondly, obtaining doping source powder: the dopant source powder was obtained by purchasing a commercially available inorganic salt or oxide powder of the corresponding element, the purity of which was 99.99%, the average particle size was 0.8 μm, and the particle size of D50 was 0.5 μm. And each element of the doping source can be selected from corresponding organic salt, simple substance metal and alloy, and the effect is similar.
Thirdly, preparing nickel oxide-based ceramic:
preparing raw materials:
weighing nickel oxide powder and doping source powder with corresponding mass by using a digital electronic balance, mixing three-dimensionally to obtain nickel oxide-based mixed powder, wherein the mass fraction of the nickel oxide powder in the mixed powder is 92%, the mass fraction of the doping source is 8%, and the doping source comprises the following components in molar ratio of W: ti: zr is 2.5:1: 0.5;
b, spray drying:
(a) adding deionized water with the volume 0.7 times that of the mixed powder of nickel oxide powder and doping source powder with corresponding weight into the mixed powder to prepare slurry with 59% vol solid phase fraction, and performing ball milling for 8 hours for dispersion;
(b) spray drying the slurry at an inlet temperature of 300 ℃ and an outlet temperature of 105 ℃ to obtain secondary powder;
(c) the powder was sieved through a 60 mesh sieve.
A bulk density of 1.48 g.cm was obtained-3The mixed powder of (1).
C, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die;
e, hot-pressing sintering: the pressure is 50MPa, the vacuum degree is 2Pa, the sintering temperature is 800 ℃, the heat preservation time is 1h, and the heating speed is 1.5 ℃/min;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
and E, machining according to the requirement to obtain a ceramic finished product.
The average grain size of the obtained ceramic target finished product is 3 mu m, the doped phase size is 350nm, the bulk conductivity is 16S/cm, and the relative density is measured to be 98.4% by a drainage method.
Example 6:
this example differs from example 5 in that the dopant source components of the a feedstock preparation step are, in terms of mole ratios, Li: cu: mn: cr: si ═ 1.5:0.5:0.1:0.1: 0.01;
the average grain size of the obtained ceramic target finished product is 3.5 mu m, the doped phase size is 400nm, the bulk conductivity is 16S/cm, and the relative density is measured to be 98.4% by a drainage method.
Example 7:
firstly, preparing nickel oxide powder:
(a) introducing oxygen into high-purity nickel steam at 1700 ℃ to form high nickel oxide;
(b) mixing high nickel oxide with high-purity graphite, and roasting at 850 ℃ to obtain a nickel oxide block;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder: the ball-material ratio is 3:1, the average diameter of the grinding ball is 10mm, the volume of the grinding ball and the slurry accounts for 1/3 of the volume of the grinding chamber, and the nickel oxide powder is obtained after ball milling for 15 hours; the purity of the obtained nickel oxide powder was 99.993%, the average particle size of the nickel oxide powder prepared in this example was 1.2 μm, and the particle size of D50 was 0.8 μm;
secondly, obtaining doping source powder: the dopant source powder was obtained by purchasing a commercially available inorganic salt or oxide powder of the corresponding element, having a purity of 99.993%, an average particle diameter of 1.2 μm, and a D50 particle diameter of 0.8 μm. And each element of the doping source can be selected from corresponding organic salt, simple substance metal and alloy, and the effect is similar.
Thirdly, preparing nickel oxide-based ceramic:
preparing raw materials:
weighing nickel oxide powder and doping source powder with corresponding mass by using a digital electronic balance, mixing three-dimensionally to obtain nickel oxide-based mixed powder, wherein the mass fraction of the nickel oxide powder in the mixed powder is 95%, the mass fraction of the doping source is 5%, and the doping source comprises the following components in molar ratio: al: zn: ti 1.5:0.1:2.5: 1;
b, spray drying:
(a) adding deionized water with the volume 0.85 times that of the mixed powder of nickel oxide powder and doping source powder with corresponding weight into the mixed powder to prepare slurry with 54% vol solid phase fraction, and performing ball milling for 10 hours for dispersion;
(b) spray drying the slurry at an inlet temperature of 300 ℃ and an outlet temperature of 100 ℃ to obtain secondary powder;
(c) the powder was sieved through a 60 mesh sieve.
The bulk density obtained was 1.58 g.cm-3The mixed powder of (1).
C, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die;
e, hot-pressing sintering: the pressure is 100MPa, the vacuum degree is 0.1Pa, the sintering temperature is 950 ℃, the heat preservation time is 1.5h, and the heating speed is 0.5 ℃/min;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
and E, machining according to the requirement to obtain a ceramic finished product.
The average grain size of the obtained ceramic target finished product is 6 mu m, the doped phase size is 130nm, the bulk conductivity is 28S/cm, and the relative density is measured to be 98.8% by a drainage method.
Example 8:
firstly, preparing nickel oxide powder:
(a) introducing oxygen into the high-purity nickel steam at 1550 ℃ to form high nickel oxide;
(b) mixing high nickel oxide with high-purity graphite, and roasting at 700 ℃ to obtain a nickel oxide block;
(c) airflow crushing to obtain coarse nickel oxide powder;
(d) carrying out wet ball milling on the nickel oxide coarse powder: the ball-material ratio is 2:1, the average diameter of the grinding ball is 2mm, the volume of the grinding ball and the slurry accounts for 1/2 of the volume of the grinding chamber, and the nickel oxide powder is obtained after ball milling for 20 hours; the purity of the obtained nickel oxide powder was 99.991%, and the micrograph of the nickel oxide powder prepared in this example is fig. 7, and the PSD chart is fig. 8, and the average particle size was 2 μm and the D50 particle size was 800 nm.
Secondly, obtaining doping source powder: the dopant source powder was obtained by purchasing a commercially available inorganic salt or oxide powder of the corresponding element, having a purity of 99.991%, an average particle diameter of 2 μm, and a D50 particle diameter of 800 nm. And each element of the doping source can be selected from corresponding organic salt, simple substance metal and alloy, and the effect is similar.
Thirdly, preparing nickel oxide-based ceramic:
preparing raw materials:
weighing nickel oxide powder and doping source powder with corresponding mass by using a digital electronic balance, mixing three-dimensionally to obtain nickel oxide-based mixed powder, wherein the mass fraction of the nickel oxide powder in the mixed powder is 90%, the mass fraction of the doping source is 10%, and the doping source components are all Zr: zn: al: w is 1:3:0.1: 3;
b, spray drying:
(a) adding deionized water with the volume 0.85 times that of the mixed powder of nickel oxide powder and doping source powder with corresponding weight into the mixed powder to prepare slurry with 54% vol solid phase fraction, and performing ball milling for 8 hours for dispersion;
(b) spray drying the slurry at an inlet temperature of 300 ℃ and an outlet temperature of 105 ℃ to obtain secondary powder;
(c) the powder was sieved through a 60 mesh sieve.
A bulk density of 1.65 g.cm was obtained-3The mixed powder of (1).
C, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die;
e, hot-pressing sintering: the pressure is 5MPa, the vacuum degree is 10Pa, the sintering temperature is 600 ℃, the heat preservation time is 5h, and the heating speed is 0.5 ℃/min;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
and E, machining according to the requirement to obtain a ceramic finished product.
The average grain size of the obtained ceramic target finished product is 8 mu m, the doped phase size is 800nm, the bulk conductivity is 30S/cm, and the relative density is measured to be 99.4% by a drainage method.
Example 9
This example differs from example 8 in that the dopant source components of the a feedstock preparation step are, in terms of mole ratios, Li: mg: zn: zr: ti is 1:0.5:2.5:0.15: 1.
The average grain size of the obtained ceramic target finished product is 9 mu m, the doped phase size is 730nm, the bulk conductivity is 27S/cm, and the relative density is measured to be 99.2% by a drainage method.
Example 10
This example is different from example 7 in that the doping sources in the a raw material preparation step are all Li.
The average grain size of the obtained ceramic target finished product is 6 mu m, the doped phase size is 200nm, the bulk conductivity is 32S/cm, and the relative density is measured to be 99.2% by a drainage method.
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.

Claims (10)

1. A hot press molding preparation method of a nickel oxide based ceramic target material is characterized by comprising the following steps:
preparing raw materials: the mixed powder comprises nickel oxide powder and doping source powder, wherein the total mass fraction of doping source elements in the mixed powder is not higher than 10%, the doping source elements are selected from one or more of Li, Na, Mg, Al, Si, K, Zn, Zr, Mn, Cu, Cr, V, W and Ti, and the mass fraction range of the selected corresponding elements is as follows: 0-6% by mass of Li element, 0-0.3% by mass of Na element, 0-1.0% by mass of Mg element, 0-0.1% by mass of Al element, 0-0.1% by mass of Si element, 0-0.15% by mass of K element, 0-12% by mass of Zn element, 0-1.5% by mass of Zr element, 0-1.2% by mass of Mn element, 0-10% by mass of Cu element, 0-1.2% by mass of Cr element, 0-0.3% by mass of V element, 0-10% by mass of W element, and 0-2.5% by mass of Ti element; the purity of the nickel oxide powder and the doping source powder is higher than 99.99%, the average grain diameter is 500nm-2 mu m, and the grain diameter of D50 is 50nm-800 nm;
b, spray drying: carrying out spray drying treatment on the mixed powder;
c, putting the mixed powder prepared in the step B into a hot-pressing die;
d, pre-pressurizing and degassing the die;
e, hot-pressing sintering: the pressure is 5-100MPa, the vacuum degree is 0.1-10Pa, the sintering temperature is 600-;
d, after the heat preservation is finished, removing the pressure, and taking out the sintered blank;
e with or without machining as required.
2. The hot press forming preparation method of the nickel oxide-based ceramic target material according to claim 1, wherein the spray drying in the step B comprises the following steps:
(a) adding 0.5-5 times of liquid into the mixed powder to prepare slurry with 15-60% vol, and performing ball milling dispersion;
(b) spray drying to obtain secondary powder particles;
(c) this step is carried out or not as required: and sieving and refining the secondary powder.
3. The hot press forming preparation method of the nickel oxide-based ceramic target material according to any one of claims 1 to 2, wherein the mass fraction ranges of the corresponding elements are selected as follows: 0.05-5% by mass of Li element, 0.05-0.25% by mass of Na element, 0.3-0.9% by mass of Mg element, 0.01-0.09% by mass of Al element, 0.01-0.08% by mass of Si element, 0.03-0.12% by mass of K element, 0.2-10% by mass of Zn element, 0.3-1.3% by mass of Zr element, 0.3-1.1% by mass of Mn element, 0.3-0.8% by mass of Cu element, 0.3-1.0% by mass of Cr element, 0.02-0.25% by mass of V element, 1.0-9.0% by mass of W element, and 0.05-2.3% by mass of Ti element.
4. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 3, characterized in that: the doping source component is selected from one of the following groups according to a molar ratio:
a first group: the doping source element is selected from one or more of Li, Zr, Ti and W elements;
second group: the doping source is selected from one or more of Li, Na, Zn and W;
third group: the doping source is selected from one or more of Li, Zr, Zn and Ti;
and a fourth group: the doping source is selected from one or more of Li, Zn, K, W and V;
and a fifth group: one or more of the doping sources W, Ti and Zr;
a sixth group: the doping source is selected from one or more of Li, Cu, Mn, Cr and Si;
a seventh group: the doping source is selected from one or more of Mg, Al, Zn and Ti;
and an eighth group: one or more of the doping sources Zr, Zn, Al and W;
ninth group: the doping source is selected from one or more of Li, Mg, Zn, Zr and Ti;
the tenth group: the doping source is selected from one or more of W, Zn, Na, K, Mg, Ti and Li.
5. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 4, characterized in that: the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w ═ 0-2: (0-2): (0-1): (0-5);
second group: li: na: zn: w ═ 0-2: (0-1): (0-2);
third group: li: zr: zn: ti ═ 0-2: (0-2): (0-5): (0-2);
and a fourth group: li: zn: k: w: v ═ 0-2, (0-1), (0-2), (0-1);
and a fifth group: w: ti: zr ═ 0-5: (0-2): (0-2);
a sixth group: li: cu: mn: cr: si ═ 0-2: (0-1): (0-1);
a seventh group: mg: al: zn: ti (0-5): 0-0.5): 0-5): 0-2;
and an eighth group: zr: zn: al: w ═ 0-2: (0-5): (0-0.5): (0-5);
ninth group: li: mg: zn: zr: ti (0-2), (0-1), (0-5), (0-0.5) and (0-2).
6. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 5, characterized in that: the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w ═ (0.5-1.8): (0.5-1.8): (0.05-0.9): (0.5-4.5);
second group: li: na: zn: w ═ 0.5-1.5, (0-1), (0.5-1.5);
third group: li: zr: zn: ti ═ 0.5 to 1.8: (0.5-1.8): (0.5-4.5): (0.05-1.8);
and a fourth group: li: zn: k: w: v ═ 0.5-2, (0-1), (0.5-2), (0-1);
and a fifth group: w: ti: zr ═ 0.5 to 4.5: (0.5-1.8): (0.05-1.8);
a sixth group: li: cu: mn: cr: si is (0.5-2), (0-1), (0:0.5), (0-0.5) and (0-0.5);
a seventh group: mg: al: zn: ti (0.5-2.5): 0.05-0.3): 0.5-3.5): 0.5-1.5);
and an eighth group: zr: zn: al: w ═ (0.5-1.8): (0.5-4.5): (0.01-0.45): (0.5-4.5);
ninth group: li: mg: zn: zr: ti (0.5-1.5), (0.2-0.75), (0.5-3.5), (0.05-0.3), (0-2).
7. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 6, characterized in that: the doping source component is selected from one of the following groups according to a molar ratio:
a first group: li: zr: ti: w is 1:1:0.4: 3;
second group: li: na: zn: w is 1:0.5:0.8: 1.2;
third group: li: zr: zn: and Ti is 1:1:3: 1;
and a fourth group: li: zn: k: w: v ═ 1.2:0.6:0.2:1: 0.2;
and a fifth group: w: ti: zr ═ 2.5:1: 0.5;
a sixth group: li: cu: mn: cr: si ═ 1.5:0.5:0.1:0.1: 0.01;
a seventh group: mg: al: zn: ti 1.5:0.1:2.5: 1;
and an eighth group: zr: zn: al: w is 1:3:0.1: 3;
ninth group: li: mg: zn: zr: ti is 1:0.5:2.5:0.15: 1.
8. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 1, characterized in that: the nickel oxide powder and the doping source powder have the average grain diameter of 800nm-1.3 mu m, and the grain diameter of D50 is 300-600 nm.
9. The hot press molding preparation method of the nickel oxide-based ceramic target material according to claim 1, characterized in that: the mass fraction of the doping source is not higher than 8%.
10. The hot isostatic pressing preparation method of the nickel oxide-based ceramic target material according to claim 1, characterized in that: and each element of the doping source is selected from corresponding simple substance metal, alloy, inorganic salt, organic salt or oxide.
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Publication number Priority date Publication date Assignee Title
WO2023097583A1 (en) * 2021-12-01 2023-06-08 宁德时代新能源科技股份有限公司 Doped nickel oxide target material, and preparation method therefor and use thereof
CN115180962A (en) * 2022-05-27 2022-10-14 先导薄膜材料（广东）有限公司 High-density high-mobility oxide target material and preparation method thereof

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