CN109879667B - Preparation method of dense oxygen-loss zinc oxide ceramic body - Google Patents
Preparation method of dense oxygen-loss zinc oxide ceramic body Download PDFInfo
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Abstract
The invention provides a preparation method of a compact oxygen-loss zinc oxide ceramic body, which mainly comprises the steps of preparing zinc layer coated zinc oxide granulation powder, preparing a ceramic blank by the zinc layer coated zinc oxide granulation powder and sintering the ceramic blank; the preparation process of the zinc oxide layer coated zinc oxide granulation powder comprises the steps of adding zinc oxide premix into liquid containing a dispersing agent to prepare slurry, carrying out spray granulation on the slurry, and conveying zinc steam to a granulation area to realize zinc layer coating on the surface of the zinc oxide granulation powder, wherein the forming temperature of the zinc steam is 1000-1300 ℃. Compared with the prior art, the preparation method disclosed by the invention has the advantages that the preparation of the compact oxygen-loss zinc oxide ceramic body is realized by adopting a simple method, the used equipment is simple, the cost is low, the compactness is higher, the relative density of the product is more than 95%, the product has lower resistivity, and the resistivity is tested to be less than 1 omega cm, so that the sputtering requirements of DC and MF can be met.
Description
Technical Field
The invention relates to the technical field of photoelectric materials, in particular to a zinc oxide ceramic body oxygen loss rate control method which can realize high compactness and control of the oxygen loss rate of the zinc oxide ceramic body, can be used as a target material for magnetron sputtering and meets the use requirements of downstream photoelectric coating industries.
Background
The zinc oxide is used as an environment-friendly multifunctional wide bandgap oxide material with abundant reserves, can be changed into a Transparent Conductive Oxide (TCO) with higher photoelectric performance after a certain amount of degenerate doping (such as Al, Ga, In and the like), has the advantages of ultraviolet light absorption, visible light transparency, infrared light reflection, adjustable electrical characteristics and the like, is increasingly applied to the field of photoelectric information such as flat panel display, thin-film solar cells, Low-E glass for building energy conservation, intelligent glass and the like, and can be used as a transparent electrode layer, a middle dielectric layer and a back electrode high-reflection layer In the thin-film solar cells, a functional dielectric layer In the energy-saving Low-E glass, a transparent electrode layer of the intelligent glass, an infrared reflection layer of household appliance glass and the like. At present, the technology for depositing zinc oxide based films is various, wherein magnetron sputtering film formation is the most mature, and the zinc oxide based films have the advantages of high film density, good uniformity and repeatability, easy large-area high-speed deposition and the like, and are accepted and widely adopted by the industry. In the magnetron sputtering process, the ceramic target plays a crucial role, and the performance of the ceramic target is closely related to the sputtering stability and the photoelectric characteristic of a final film layer. The basic requirements for high-performance ceramic targets are: high compactness, fine and uniform crystal grains and uniform and consistent components. Recently, new development requirements of the coating industry can realize strict control on oxygen vacancy of the target material, and meet application requirements of a novel zinc oxide functional film: (1) for a CIGS thin film solar cell, a layer of intrinsic i-ZnO needs to be deposited, the traditional intrinsic ZnO ceramic target has poor conductivity, an expensive Radio Frequency (RF) power supply is needed for sputtering, in addition, the sputtering rate is slow, and the requirement of rapid batch production is difficult to meet, so that the conductivity of the target needs to be improved by adjusting oxygen vacancies in ZnO crystals, and Direct Current (DC) or intermediate frequency (MF) can be adopted for realizing high-speed deposition; (2) in the field of multilayer film deposition such as low-E coating, the ZnO target material is required to have a certain oxygen loss rate, so that the deposited film can absorb certain oxygen molecules in a coating cavity, a lower metal layer is further protected, and the metal layer is prevented from being oxidized in the coating process.
In order to control the content of the oxygen loss rate of the zinc oxide ceramic target material, the related documents give the following preparation technical means. Wandongyun et al, in Chinese Optical Letters (2011, volume 9, page 10, 103102), disclose a method for preparing a pure ZnO target with oxygen defects, in which a ZnO blank formed by dry pressing is sintered at 1350 ℃ for 4h and then taken out, and the sintered ZnO blank is placed in a small crucible, the small crucible is placed in an inverted large crucible, carbon powder is placed between the two crucibles, the carbon powder reacts with residual oxygen in the temperature rise process to form reductive CO gas, the gas reacts with ZnO to reduce and lose oxygen in the inverted ZnO crystal lattice, and a zinc oxide ceramic target with oxygen vacancies is formed. Ming-Wei Wu et al, Journal of Alloys and Compounds (2015, 650, 514) published a method for preparing aluminum doped zinc oxide (AZO) ceramic targets with a certain oxygen loss by hot isostatic pressing, in which AZO bodies are first sintered at 1300 ℃ for 3h under air conditions and then sintered at 1250 ℃ for 3h in a hot isostatic pressing apparatus under argon pressure. In addition, a preparation method for forming the ceramic target with a certain oxygen loss rate by adopting a special atmosphere sintering furnace to perform reduction treatment on the ceramic material is also provided. However, the three methods are still difficult to be applied to the large-scale production of large-size AZO targets, and have the following defects: (1) limited by a crucible and a hot isostatic pressing equipment cavity, the method can be only used for processing small-sized laboratory samples and cannot be applied to sintering large-sized ceramic targets in batches; (2) the operation process is complicated, and the target needs to be sintered into a block and then placed in another device for secondary treatment, so that the preparation cost of the target is indirectly increased; the surface of the first-time sintered ceramic is relatively compact, so that a certain barrier effect is achieved on the reducing atmosphere in the second-time sintering, and the phenomenon of nonuniform oxygen loss inside and on the surface is easy to occur, so that the uniformity of the target material is influenced; (3) equipment for hot isostatic pressing and special atmosphere sintering is high in cost, and the cost for preparing the target material is increased.
Disclosure of Invention
In order to solve the technical problems, the invention starts from the treatment of zinc oxide raw material powder, realizes the coating of a zinc layer on the surface of zinc oxide granulated powder, the blank body molding, and utilizes xZn + (1-x) ZnO → ZnO in the subsequent sintering process1-xThe preparation of the compact oxygen-loss zinc oxide ceramic body is realized through the diffusion reaction.
The technical scheme of the invention is to provide a preparation method of a compact oxygen-loss zinc oxide ceramic body, which mainly comprises the steps of preparing zinc layer coated zinc oxide granulation powder, preparing a ceramic blank by the zinc layer coated zinc oxide granulation powder and then sintering; the preparation process of the zinc oxide layer coated zinc oxide granulation powder comprises the steps of adding zinc oxide premix into liquid containing a dispersing agent to prepare slurry, carrying out spray granulation on the slurry, and conveying zinc steam to a granulation area to realize zinc layer coating on the surface of the zinc oxide granulation powder, wherein the forming temperature of the zinc steam is 1000-1300 ℃.
Further, the zinc oxide premix is prepared by mixing zinc oxide powder and doped oxide powder, wherein the mass of the doped oxide powder/(the mass of the zinc oxide powder + the mass of the doped oxide powder) in the mixture is 0-10 wt%; when the mass fraction of the doped oxide powder is 0, the zinc oxide premix is composed of only zinc oxide powder.
Further, the mass fraction of the dispersing agent in the liquid containing the dispersing agent is 0.1-3 wt%, and the solvent is deionized water; and preparing slurry by ball milling for 8-24 h.
Furthermore, the average particle size of the zinc oxide powder in the zinc oxide premix is 200-500 nm, and the purity is 99.95-99.99%; belongs to high-purity zinc oxide powder; the doped oxide is one or two of aluminum oxide, gallium oxide and indium oxide, the average grain diameter is 100-400 nm, and the purity is 99.95-99.99%;
further, the dispersing agent is one or two of polyvinylpyrrolidone, polyvinyl alcohol and carboxymethyl cellulose;
furthermore, the zinc layer is coated with zinc oxide granulation powder, the average particle size of the zinc layer is 10-100 μm, and the thickness of the zinc layer is 0.5-2 μm;
further, the above zinc layer-coated zinc oxide granulated powder production apparatus includes: the device comprises a slurry container with a liquid nozzle at the bottom, carrier gas units with gas nozzles distributed around the liquid nozzle, at least one gas nozzle, at least one carrier gas unit and a zinc vapor forming pool; wherein the angle alpha between the gas flow sprayed by the gas nozzle and the liquid flow sprayed by the liquid nozzle is 20-90 degrees, so that the liquid particles are crushed and atomized to the expected particle size;
furthermore, the aperture of the liquid nozzle hole is 0.5-2 mm, and the flow rate of the slurry flowing out of the hole is 0.01-5L/min;
furthermore, the gas carried by the carrier gas unit is one of argon or nitrogen, the gas pressure is 0.8-30 MPa, the temperature of the heated carrier gas is 80-120 ℃, the slurry liquid flow is further crushed and atomized through the carrier gas flow, and meanwhile, the carrier gas has a certain temperature to evaporate water in partial liquid particles, so that the subsequent adhesion of zinc vapor on the surfaces of the zinc oxide granulation powder particles is facilitated.
Further, the relative density of a ceramic blank body made of zinc oxide granulation powder coated by a zinc layer is 60-75%, the sintering process is that the temperature is increased to the first set temperature of 1000-1250 ℃ at the heating rate of 0.5-10 ℃/min, and the temperature is kept for 30-90 min; and then raising the temperature to 1300-1450 ℃ at a heating rate of 10-100 ℃/min, preserving the temperature for 120-480 min, and finally lowering the temperature to room temperature at a cooling rate of 0.5-10 ℃/min, wherein the sintering atmosphere is one or a mixture of air, nitrogen and argon.
Further, the blank forming method is cold isostatic pressing, the pressure is 120-300 MPa, and the pressure maintaining time is 60-600 s.
The prepared compact oxygen-loss zinc oxide ceramic body can be subjected to post-treatment such as cutting, polishing and the like according to actual requirements, and the color of the post-treated product is black.
The invention has the advantages and beneficial effects that: the preparation of the compact oxygen-loss zinc oxide ceramic body is realized by adopting a simple method, the used equipment is simple, the cost is low, the compactness is higher, the relative density of the product is more than 95%, and the product has lower resistivity, and the resistivity of the product is tested to be less than 1 omega cm, so that the sputtering requirements of DC and MF can be met.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing zinc-coated zinc oxide granulated powder according to the present invention.
In the figure, 1-slurry container, 2-slurry, 3-carrier gas, 4-gas nozzle, 5-heating coil, 61-zinc oxide granulation powder, 62-zinc layer coated zinc oxide granulation powder, 7-zinc steam and 8-zinc steam forming pool
Detailed Description
The present invention will be further described with reference to the following embodiments.
The invention provides a preparation method of a compact oxygen-loss zinc oxide ceramic body, which mainly comprises the steps of preparing zinc layer coated zinc oxide granulation powder, preparing a ceramic blank by the zinc layer coated zinc oxide granulation powder and then sintering. The preparation process of the zinc oxide layer coated zinc oxide granulation powder comprises the steps of adding a zinc oxide premix into a liquid containing a dispersing agent to prepare a slurry 2, carrying out spray granulation on the slurry 2, and then conveying zinc steam 7 to a granulation area to realize zinc layer coating on the surface of the zinc oxide granulation powder, wherein the forming temperature of the zinc steam 7 is 1000-1300 ℃; the preparation device of zinc oxide granulation powder coated by a zinc layer adopted by the invention is shown in figure 1 and comprises the following components: a slurry container 1 with a liquid nozzle at the bottom, at least one carrier gas unit with a gas nozzle 4 distributed around the liquid nozzle, two gas nozzles 4 are shown in fig. 1, and a zinc vapor formation tank 8; wherein the angle alpha between the gas flow sprayed by the gas nozzle 4 and the liquid flow sprayed by the liquid nozzle is 20-90 degrees, so that the liquid particles of the slurry 2 are crushed and atomized to the expected particle size; the carrier gas 3 and the zinc vapor 7 are heated by the heating coil 5.
As a further improvement, the aperture of the liquid nozzle hole is 0.5-2 mm, and the flow rate of the slurry 2 flowing out of the hole is 0.01-5L/min;
as a further improvement, the carrier gas 3 of the carrier gas unit is one of argon or nitrogen, the gas pressure is 0.8-30 MPa, the temperature for heating the carrier gas 3 is 80-120 ℃, the slurry liquid flow is further crushed and atomized by the carrier gas 3, and meanwhile, the carrier gas 3 has a certain temperature which can evaporate water in part of liquid particles, so that the subsequent zinc vapor 7 can be attached to the surfaces of zinc oxide granulation powder particles.
Example 1
The invention provides a preparation method of a dense oxygen-loss zinc oxide ceramic body, which comprises the following steps:
the method comprises the following steps: preparation of zinc layer coated zinc oxide granulation powder
1. Weighing a certain amount of high-purity zinc oxide powder and mixing with doped oxide powder, wherein the mass of the doped oxide powder/(the mass of the zinc oxide powder + the mass of the doped oxide powder) in the mixture is 5 wt%; wherein the average grain diameter of the high-purity zinc oxide powder is 200nm, the purity is 99.95-99.99%, the doped oxide powder is alumina, the average grain diameter is 100nm, and the purity is 99.95-99.99%;
2. mixing the powder, pouring the mixture into deionized water containing 1 wt% of dispersant, and performing ball milling for 8 hours to form slurry 2; wherein the dispersant is polyvinylpyrrolidone;
3. placing the slurry 2 in a granulating device shown in fig. 1, spraying the slurry 2 through a liquid nozzle, spraying a carrier gas 3 through a gas nozzle 4, dispersing liquid particles by using gas, evaporating water of the liquid particles due to certain temperature of the gas to complete granulation, and obtaining zinc oxide granulating powder 61, and then conveying zinc steam 7 from a zinc steam forming pool 8 (keeping the temperature at 1000-1300 ℃, so as to facilitate continuous formation of the zinc steam 7) to a powder granulating area to realize zinc layer coating on the surface of the zinc oxide granulating powder 61, so as to form zinc layer coated zinc oxide granulating powder 62; the obtained zinc layer coated zinc oxide granulation powder 62 has an average particle size of 10 to 100 μm and a zinc layer thickness of 0.5 to 2 μm;
step two, preparing a blank body and sintering the blank body
1. Putting the zinc layer coated zinc oxide granulation powder 62 obtained in the step one into a mould, and carrying out cold isostatic pressing at 120-300 MPa for 60-600 s to form a ceramic blank with the relative density of 60-75%;
2. and (3) placing the ceramic blank into an atmosphere (air is adopted as the sintering atmosphere in the embodiment) sintering furnace, raising the temperature of the electric furnace from room temperature to the set temperature of 1000-1250 ℃ in the first step at the heating rate of 0.5-10 ℃/min, and preserving the heat for 30-90 min. Then, the temperature is increased to 1300-1450 ℃ at the temperature increasing rate of 10-100 ℃/min, the temperature is kept for 120-480 min, and finally the temperature is reduced to the room temperature at the temperature reducing rate of 0.5-10 ℃/min;
3. cutting and polishing a sample into a specified size to obtain a compact oxygen-loss zinc oxide ceramic body; after polishing, the ceramic body appears dark black in color.
Example 2
The invention provides a preparation method of a dense oxygen-loss zinc oxide ceramic body, which comprises the following steps:
the method comprises the following steps: preparation of zinc layer coated zinc oxide granulation powder
1. Weighing a certain amount of high-purity zinc oxide powder and mixing with doped oxide powder, wherein the mass of the doped oxide powder/(the mass of the zinc oxide powder + the mass of the doped oxide powder) in the mixture is 10 wt%; wherein the average grain diameter of the high-purity zinc oxide powder is 500nm, the purity is 99.95-99.99%, the doped oxide powder is aluminum oxide and gallium oxide, the average grain diameter is 400nm, and the purity is 99.95-99.99%;
2. mixing the powder, pouring the mixture into deionized water containing 2 wt% of a dispersing agent, and performing ball milling for 16 hours to form slurry 2; wherein the dispersant is polyvinyl alcohol;
3. placing the slurry 2 in a granulating device shown in fig. 1, spraying the slurry 2 through a liquid nozzle, spraying a carrier gas 3 through a gas nozzle 4, dispersing liquid particles by using gas, evaporating water of the liquid particles due to certain temperature of the gas to complete granulation, and obtaining zinc oxide granulating powder 61, and then conveying zinc steam 7 from a zinc steam forming pool 8 (keeping the temperature at 1000-1300 ℃, so as to facilitate continuous formation of the zinc steam 7) to a powder granulating area to realize zinc layer coating on the surface of the zinc oxide granulating powder 61, so as to form zinc layer coated zinc oxide granulating powder 62; the obtained zinc layer coated zinc oxide granulation powder 62 has an average particle size of 10-100 μm and a zinc layer thickness of 0.5-2 μm;
step two, preparing a blank body and sintering the blank body
1. Putting the zinc layer coated zinc oxide granulation powder 62 obtained in the step one into a mould, and carrying out cold isostatic pressing at 120-300 MPa for 60-600 s to form a ceramic blank with the relative density of 60-75%;
2. and (3) placing the ceramic blank into an atmosphere (air is adopted as the sintering atmosphere in the embodiment) sintering furnace, raising the temperature of the electric furnace from room temperature to the set temperature of 1000-1250 ℃ in the first step at the heating rate of 0.5-10 ℃/min, and preserving the heat for 30-90 min. Then, the temperature is increased to 1300-1450 ℃ at the temperature increasing rate of 10-100 ℃/min, the temperature is kept for 120-480 min, and finally the temperature is reduced to the room temperature at the temperature reducing rate of 0.5-10 ℃/min;
3. cutting and polishing a sample into a specified size to obtain a compact oxygen-loss zinc oxide ceramic body; after polishing, the ceramic body appears dark black in color.
Example 3
The invention provides a preparation method of a dense oxygen-loss zinc oxide ceramic body, which comprises the following steps:
the method comprises the following steps: preparation of zinc layer coated zinc oxide granulation powder
1. Weighing a certain amount of high-purity zinc oxide powder, wherein the average grain diameter of the high-purity zinc oxide powder is 300nm, the purity of the high-purity zinc oxide powder is 99.95-99.99%, the doped oxide powder is aluminum oxide and indium oxide, the average grain diameter of the doped oxide powder is 200nm, and the purity of the doped oxide powder is 99.95-99.99%;
2. mixing the powder, pouring the mixture into deionized water containing 0.5 wt% of dispersant, and performing ball milling for 24 hours to form slurry 2; wherein the dispersant is carboxymethyl cellulose;
3. placing the slurry 2 in a granulating device shown in fig. 1, spraying the slurry 2 through a liquid nozzle, spraying a carrier gas 3 through a gas nozzle 4, dispersing liquid particles by using gas, evaporating water of the liquid particles due to certain temperature of the gas to complete granulation, and obtaining zinc oxide granulating powder 61, and then conveying zinc steam 7 from a zinc steam forming pool 8 (keeping the temperature at 1000-1300 ℃, so as to facilitate continuous formation of the zinc steam 7) to a powder granulating area to realize zinc layer coating on the surface of the zinc oxide granulating powder 61, so as to form zinc layer coated zinc oxide granulating powder 62; the obtained zinc layer coated zinc oxide granulation powder 62 has an average particle size of 10-100 μm and a zinc layer thickness of 0.5-2 μm;
step two, preparing a blank body and sintering the blank body
1. Putting the zinc layer coated zinc oxide granulation powder 62 obtained in the step one into a mould, and carrying out cold isostatic pressing at 120-300 MPa for 60-600 s to form a ceramic blank with the relative density of 60-75%;
2. and (3) placing the ceramic blank in a sintering furnace with an atmosphere (air is adopted in the sintering atmosphere in the embodiment), raising the temperature of the electric furnace from room temperature to the set temperature of 1000-1250 ℃ in the first step at the heating rate of 0.5-10 ℃/min, and preserving the heat for 30-90 min. Then, the temperature is increased to 1300-1450 ℃ at the temperature increasing rate of 10-100 ℃/min, the temperature is kept for 120-480 min, and finally the temperature is reduced to the room temperature at the temperature reducing rate of 0.5-10 ℃/min;
3. cutting and polishing a sample into a specified size to obtain a compact oxygen-loss zinc oxide ceramic body; after polishing, the color of the ceramic body is dark black.
The density was measured using the Archimedes method and the relative density of the target was calculated as a percentage of the measured density to the theoretical density, the relative density of the target being greater than 95%, e.g., for the ceramic target of example 1, the ceramic body was determined to have a density of 5.553g/cm3The theoretical density of the powder is 5.58g/cm3Thus the relative density is 99.5% and the relative density results for the other examples are similar and all greater than 95%. For a compact zinc oxide ceramic body with a certain doping content, the resistivity change of the compact zinc oxide ceramic body comes from the formation of oxygen vacancies, so the number of the oxygen vacancies can be represented by the resistivity of the material, and the resistivity of the ceramic target material is tested<1 omega cm, and further meets the sputtering requirements of DC and MF.
Materials, reagents and experimental equipment related to the embodiment of the invention are all commercial products in the field of photoelectric materials unless otherwise specified.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, modifications and decorations can be made without departing from the core technology of the present invention, and these modifications and decorations shall also fall within the protection scope of the present invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (10)
1. The preparation method of the compact oxygen-loss zinc oxide ceramic body is characterized by mainly comprising the steps of preparing zinc layer coated zinc oxide granulation powder, preparing a ceramic blank by the zinc layer coated zinc oxide granulation powder and sintering; the preparation process of the zinc layer coated zinc oxide granulation powder comprises the steps of adding a zinc oxide premix into a liquid containing a dispersing agent to prepare a slurry, carrying out spray granulation on the slurry, and conveying zinc steam to a granulation area to realize zinc layer coating on the surface of the zinc oxide granulation powder, wherein the forming temperature of the zinc steam is 1000-1300 ℃, the average particle size of the zinc layer coated zinc oxide granulation powder is 10-100 mu m, and the thickness of a zinc layer is 0.5-2 mu m.
2. The method for preparing a dense oxygen-depleted zinc oxide ceramic body according to claim 1, wherein the zinc oxide premix is prepared by mixing zinc oxide powder and doped oxide powder, and the mass of the doped oxide powder/(the mass of the zinc oxide powder + the mass of the doped oxide powder) = 0-10 wt% in the mixture.
3. The method for preparing the dense oxygen-depleted zinc oxide ceramic body according to claim 1, wherein the dispersant is present in the dispersant-containing liquid in an amount of 0.1 to 3wt% and the solvent is deionized water; and preparing slurry by ball milling for 8-24 h.
4. The method for preparing a dense oxygen-loss zinc oxide ceramic body according to claim 2, wherein the average particle size of zinc oxide powder in the zinc oxide premix is 200-500 nm, and the purity is 99.95-99.99%; the doped oxide is one or two of aluminum oxide, gallium oxide and indium oxide, the average grain diameter is 100-400 nm, and the purity is 99.95-99.99%.
5. The method of making a dense, oxygen-depleted zinc oxide ceramic body of claim 1, wherein the dispersant is one or both of polyvinylpyrrolidone, polyvinyl alcohol, and carboxymethylcellulose.
6. The method of preparing a dense, oxygen-depleted zinc oxide ceramic body of claim 1, wherein the zinc layer coated zinc oxide granulated powder preparation apparatus comprises: the device comprises a slurry container with a liquid nozzle at the bottom, carrier gas units with gas nozzles distributed around the liquid nozzle, at least one gas nozzle, at least one carrier gas unit and a zinc vapor forming pool, wherein the carrier gas units are distributed around the liquid nozzle; wherein an angle alpha between the gas flow jetted by the gas nozzle and the liquid flow jetted by the liquid nozzle is 20-90 degrees.
7. The method of making a dense, oxygen-depleted zinc oxide ceramic body of claim 6, wherein the liquid nozzle has pores with a diameter of 0.5 to 2mm and the slurry flows out of the pores at a rate of 0.01 to 5L/min.
8. The method for preparing the dense oxygen-loss zinc oxide ceramic body according to claim 6 or 7, wherein the gas carried by the carrier gas unit is one of argon gas or nitrogen gas, the gas pressure is 0.8-30 MPa, and the temperature of the heating carrier gas is 80-120 ℃.
9. The method for preparing the dense oxygen-loss zinc oxide ceramic body according to claim 1, wherein the relative density of the ceramic body is 60-75%, the sintering process is carried out by raising the temperature to the first-step set temperature of 1000-1250 ℃ at a heating rate of 0.5-10 ℃/min, and keeping the temperature for 30-90 min; and then raising the temperature to 1300-1450 ℃ at a heating rate of 10-100 ℃/min, preserving the temperature for 120-480 min, and finally lowering the temperature to room temperature at a cooling rate of 0.5-10 ℃/min, wherein the sintering atmosphere is one or a mixture of air, nitrogen and argon.
10. The method for preparing a dense oxygen-depleted zinc oxide ceramic body according to claim 1, wherein the ceramic body forming method is cold isostatic pressing, the pressure is 120-300 MPa, and the pressure holding time is 60-600 s.
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