CN115650701B - Preparation method and application of nickel oxide-based target - Google Patents
Preparation method and application of nickel oxide-based target Download PDFInfo
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- CN115650701B CN115650701B CN202211396319.1A CN202211396319A CN115650701B CN 115650701 B CN115650701 B CN 115650701B CN 202211396319 A CN202211396319 A CN 202211396319A CN 115650701 B CN115650701 B CN 115650701B
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 248
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 248
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 131
- 238000005245 sintering Methods 0.000 claims abstract description 85
- 239000013077 target material Substances 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 238000000748 compression moulding Methods 0.000 claims abstract description 7
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 23
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 23
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 21
- 229910052760 oxygen Inorganic materials 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000395 magnesium oxide Substances 0.000 claims description 13
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000005751 Copper oxide Substances 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- 239000012798 spherical particle Substances 0.000 claims 3
- 239000008187 granular material Substances 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 239000007921 spray Substances 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 description 59
- 238000007088 Archimedes method Methods 0.000 description 41
- 230000000052 comparative effect Effects 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 4
- 230000005525 hole transport Effects 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention discloses a preparation method and application of a nickel oxide-based target, comprising the following preparation steps: s1, preparing a nickel oxide-based powder material, a dispersing agent, a binder and water into slurry, and performing spray granulation to obtain spherical nickel oxide-based particles; step S2, performing compression molding and cold isostatic pressing on the spherical nickel oxide-based particles to obtain a blank target; and step S3, degumming the blank target, and cooling after sectional sintering. The nickel oxide-based target material prepared by the method has high relative density, is not easy to crack, and can be widely applied to the preparation of solar cells.
Description
Technical Field
The invention relates to the technical field of oxide targets, in particular to a preparation method and application of a nickel oxide-based target.
Background
In the related art, in order to rapidly improve the photoelectric conversion efficiency of the organic-inorganic hybrid perovskite solar cell, most high-performance devices need a high-quality electron transport layer and a high-quality hole transport layer to effectively transport electrons and holes generated by the perovskite of the light absorption layer respectively. The inorganic transport layer material is widely concerned due to the advantages of high carrier mobility, high stability and the like, and the nickel oxide material serving as the inorganic hole transport layer material has the advantages of high carrier mobility, good stability, high optical transmittance, relatively matched work function and perovskite energy level, simple preparation method and the like. The nickel oxide hole transport layer is mostly used in p-i-n type planar perovskite solar cells, but the photoelectric conversion efficiency of the nickel oxide based perovskite solar cells is still lower than that of PEDOT (polymer electrolyte coated) PSS (perovskite solar cells), and the main reason is that the nickel oxide film is not high in conductivity, and meanwhile, the interface contact between the nickel oxide substrate and the perovskite film is poor and the crystallinity and quality of the perovskite film grown on the nickel oxide substrate are poor by adopting a spin coating or sol-gel and other low-temperature film forming modes.
Aiming at the problem of low open-circuit voltage and short-circuit current of a p-i-n perovskite solar cell based on a nickel oxide hole transport layer, the method of ion doping or regulating the nickel/oxygen ratio in NiO is generally adopted in the related technology to improve the electrical performance of NiO, and the change of oxygen content can change the nickel/oxygen ratio in NiO, namely one Ni 2+ Vacancies can produce two Ni 3+ Ion, ni 3+ The p-type characteristic of NiO is determined by the formation of ions, a nickel oxide film with good crystallinity and good interface contact with a perovskite film can be obtained by Physical Vapor Deposition (PVD) low-temperature film forming, and the adjustment of oxygen content in the annealing process has important significance for improving the efficiency of the inverted perovskite solar cell. However, since nickel oxide has various molecular formulas, oxygen content of different molecular formulas is different, and densities of various components are different, if there is a component change in the sintering process, the sintered target is cracked, so that the requirement of the magnetron sputtering target cannot be met.
Therefore, there is a need for a nickel oxide-based target that has a good sintering density and is less prone to cracking after sintering.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a preparation method and application of a nickel oxide-based target, which can solve the problem that the target is easy to crack after cooling.
The invention also provides a nickel oxide-based target.
The invention also provides application of the nickel oxide-based target material in preparing perovskite solar cells.
In a first aspect of the present invention, there is provided a method for preparing a nickel oxide-based target, comprising the steps of:
s1, preparing a nickel oxide-based powder material, a dispersing agent, a binder and water into slurry, and performing spray granulation to obtain spherical nickel oxide-based particles;
step S2, performing compression molding and cold isostatic pressing on the spherical nickel oxide-based particles to obtain a blank target;
and step S3, degumming the blank target, and cooling after sectional sintering.
The preparation method of the nickel oxide-based target for the perovskite solar cell has at least the following beneficial effects: the invention solves the technical problem that the nickel oxide-based target is easy to crack in the cooling process after sintering by adopting a sectional sintering method, and the preparation method of the nickel oxide-based target is simple and easy to realize industrial production.
In some embodiments of the invention, in step S1, D of the slurry 50 Less than 250nm.
In some embodiments of the invention, in step S1, D of the slurry 90 Less than 500nm.
In some embodiments of the invention, in step S1, D of the spherical nickel oxide-based particles 50 Less than 25 μm.
In some embodiments of the invention, in step S1, D of the spherical nickel oxide-based particles 90 Less than 48 μm.
In some embodiments of the invention, in step S1, D of the spherical nickel oxide-based particles 50 Less than 25 μm.
In some embodiments of the invention, in step S1, D of the spherical nickel oxide-based particles 90 Less than 48 μm.
In some embodiments of the present invention, in step S1, the nickel oxide-based powder material is further doped with at least one oxide of magnesium oxide, copper oxide, and niobium oxide.
In some embodiments of the present invention, in step S1, the mass fraction of nickel oxide in the nickel oxide-based powder material is not less than 90%.
In some embodiments of the invention, in step S1, the dispersant is Celaster oil CELLNA D-305.
In some embodiments of the invention, in step S1, the mass percentage of the dispersant in the slurry is 0.5% to 1%.
In some embodiments of the invention, in step S1, the binder is polyvinyl acetate.
In some embodiments of the present invention, in step S1, the mass percentage of the binder in the slurry is 1.5% to 3%.
In some embodiments of the invention, in step S2, the pressure of the compression molding is 0.1Mpa to 0.8Mpa.
In some embodiments of the invention, in step S2, the cold isostatic pressure is between 250Mpa and 300Mpa.
In some embodiments of the invention, in step S3, the degumming temperature is 400 ℃ to 500 ℃.
In some embodiments of the invention, in step S3, the staged sintering comprises a first stage sintering and a second stage sintering, wherein:
the sintering temperature of the first-stage sintering is 700-900 ℃, the heat preservation time is 5-10 h, and the vacuum degree is 0.08-0.1 Mpa;
the sintering temperature of the second-stage sintering is 1300-1500 ℃, the sintering time is 5-12 h, and oxygen or nitrogen-hydrogen mixture is introduced after reaching the sintering temperature of the second stage for 0.8-1.2 h.
In the invention, the time of introducing oxygen or nitrogen-hydrogen mixed gas is delayed, which is beneficial to improving sintering quality.
In some embodiments of the invention, the sintering pressure of the second stage sintering is between 0.05Mpa and 0.1Mpa.
In some embodiments of the invention, the temperature increase rate when the sintering temperature of the first stage sintering is increased to the sintering temperature of the second stage is 0.5 ℃/min to 1.5 ℃/min.
In the invention, too high a heating rate when the sintering temperature in the first stage is raised to the sintering temperature in the second stage also affects the quality of the target, and there is a risk of cracking the target.
In some embodiments of the present invention, the volume ratio of nitrogen to hydrogen in the nitrogen-hydrogen mixture is 98-100: 2.
preferably, the volume ratio of nitrogen to hydrogen in the nitrogen-hydrogen mixture is 98:2.
the purpose of introducing oxygen or nitrogen-hydrogen mixture during sintering is to control the components not to change, when oxygen is introduced, the target components can maintain the oxygen-enriched state, namely, all Ni 2 O 3 The components of the target material cannot generate anoxic components, namely the density difference of different components of the target material cannot be caused, and the cracking condition cannot be generated; when the mixed gas of nitrogen and hydrogen (N) 2 /H 2 When the target component is in an anoxic state, the component is NiO, i.e., the oxygen-enriched component is not present, so that the density difference of different components of the target is not caused, and cracking is not caused.
In some embodiments of the present invention, in step S3, the pressure during the cooling process is 0.1Mpa to 0.5Mpa.
In some embodiments of the present invention, in step S3, the atmosphere in the cooling process is oxygen or a nitrogen-hydrogen mixture;
preferably, the volume ratio of nitrogen to hydrogen in the nitrogen-hydrogen mixture is 98:2.
the oxygen or the nitrogen-hydrogen mixed gas can be used as a protective gas in the cooling process, which is beneficial to reducing target cracking.
In a second aspect of the present invention, there is provided a nickel oxide-based target material, which is prepared by the above preparation method.
The nickel oxide-based target material provided by the embodiment of the invention has at least the following beneficial effects: the nickel oxide-based target material obtained by the preparation method provided by the invention has high relative density (more than 95%), is not easy to crack, and can be widely applied to the preparation of solar cells.
In a third aspect of the invention, there is provided the use of a nickel oxide-based target in the manufacture of a perovskite solar cell.
The nickel oxide-based target material prepared by the method is applied to perovskite solar cells, and is beneficial to improving photoelectric conversion effect.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
In the embodiment of the invention, the dispersing agent is Zhongjing grease CELLNAD-305, the content of the effective component is 40wt%, and the viscosity (25 ℃) is 50cps.
The binder is analytically pure PVA produced by national pharmaceutical sector chemical reagent Co.
The specific conditions are not noted in the embodiments of the present invention and are performed according to conventional conditions or conditions suggested by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The preparation method of the nickel oxide-based target for the perovskite solar cell in the embodiment of the invention comprises the following steps:
(1) Weighing oxidized powder material, deionized water, dispersing agent, binder and zirconia balls for ball milling according to the proportion, grinding for 6-10 h, and grinding to obtain slurry D 50 Less than 250nm, D 90 Less than 500nm, and then performing spray granulation on the obtained slurry to obtain D 50 Less than 25 μm, D 90 Spherical nickel oxide-based particles smaller than 48 μm.
(2) And (3) carrying out compression molding on the spherical nickel oxide-based particles under the pressure of 0.1-0.8 Mpa, and carrying out cold isostatic pressing on the spherical nickel oxide-based particles under the pressure of 250-300 Mpa to obtain the blank target.
(3) Degumming the blank target material at 400-500 ℃ and then carrying out sectional sintering, wherein the sintering temperature in the first stage is 700-900 ℃, the heat preservation time is 5-10 h, and the vacuum degree is 0.08-0.1 Mpa; the sintering temperature of the second stage is 1300-1500 ℃, the sintering time is 5-12 h, and the sintering atmosphere is oxygen or nitrogen-hydrogen mixed gas;
the intermediate heating rate of the sintering temperature in the first stage and the sintering temperature in the second stage is 0.5 ℃/min-1.5 ℃/min, and the atmosphere pressure is kept to be reduced to room temperature after the sintering is completed, so that the nickel oxide-based target material for the perovskite solar cell is obtained.
Example 1
The preparation method of the nickel oxide-based target material comprises the following steps:
(1) Preparation of nickel oxide-based particles: weighing nickel oxide-based powder material (surface area of 7m 2 /g～10m 2 Carrying out ball milling treatment on deionized water, a dispersing agent, a binder and zirconia balls for ball milling, wherein the nickel oxide-based powder material is nickel oxide powder, and the proportion is 20%; zirconia balls (particle size of 0.5 mm) for ball milling account for 50%, deionized water accounts for 28%, dispersing agent accounts for 0.5%, and binder accounts for 1.5%. Grinding in a sand mill for 8 hours until the slurry D 50 Less than 250nm, D 90 Spraying the obtained slurry in a spray tower to obtain D 50 Less than 25 μm, D 90 Spherical nickel oxide particles smaller than 48 μm.
(2) Preparing a blank target: carrying out compression molding on the spherical nickel oxide particles under the pressure of 0.1-0.8 Mpa, and carrying out cold isostatic pressing on the spherical nickel oxide particles under the pressure of 300Mpa to obtain blank targets;
(3) Degumming and sintering: degumming the blank target material at 450 ℃, and then performing sectional sintering, wherein the sintering temperature of the first-stage sintering is 800 ℃, the heat preservation time is 5 hours, and the vacuum degree is 0.09mpa; after the sintering of the first stage is finished, the temperature is increased to 1300 ℃ of the sintering temperature of the second stage at a heating rate of 1 ℃/min, oxygen is introduced after the sintering temperature of the second stage is reached for 1h, the sintering pressure is maintained to be between 0.05Mpa and 0.1Mpa, the sintering is continued, the total sintering time of the second stage is 10h, the atmosphere pressure (oxygen, 0-0.5 Mpa) is maintained after the sintering is finished, and the temperature is reduced to room temperature, so that the nickel oxide-based target material is obtained.
The relative density of the nickel oxide-based target material is measured by adopting an Archimedes method, and the result shows that the relative density is 96 percent and the appearance is free from cracking.
Example 2
The difference between this example and example 1 is that a nickel oxide-based target was prepared: the sintering temperature of the second stage in the step (3) is 1350 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 96.5%, and the appearance is free from cracking.
Example 3
The difference between this example and example 1 is that a nickel oxide-based target was prepared: the sintering temperature of the second stage in the step (3) is 1400 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 97%, and the appearance is free from cracking.
Example 4
The difference between this example and example 1 is that a nickel oxide-based target was prepared: the sintering temperature of the second stage in the step (3) is 1450 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98%, and the appearance is free from cracking.
Example 5
The difference between this example and example 1 is that a nickel oxide-based target was prepared: the sintering temperature of the second stage in the step (3) is 1500 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.1 percent and the appearance is free from cracking.
Example 6
The difference between this example and example 1 is that a nickel oxide-based target was prepared: the sintering temperature in the second stage in the step (3) is 1550 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.2 percent and the appearance is free from cracking.
Example 7
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the sintering temperature in the first stage in the step (3) is 700 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.03%, and the appearance is free from cracking.
Example 8
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the sintering temperature in the first stage in the step (3) is 900 ℃.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.06%, and the appearance is free from cracking.
Example 9
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the sintering time of the second stage in the step (3) is 5h.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 95 percent and the appearance is free from cracking.
Example 10
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the sintering time of the second stage in the step (3) is 12h.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.05 percent and the appearance is free from cracking.
Example 11
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the sintering atmosphere of the second stage in the step (3) is nitrogen-hydrogen mixed gas.
The relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.3 percent and the appearance is free from cracking.
Example 12
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 99:1.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.2 percent and the appearance is free from cracking.
Example 13
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 98:2.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.15 percent and the appearance is free from cracking.
Example 14
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 97:3.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.21 percent and the appearance is free from cracking.
Example 15
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 96:4.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.10 percent and the appearance is free from cracking.
Example 16
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 95:5.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.12 percent and the appearance is free from cracking.
Example 17
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 94:6.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98%, and the appearance is free from cracking.
Example 18
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 93:7.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 97.96%, and the appearance is free from cracking.
Example 19
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 92:8.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.07 percent and the appearance is free from cracking.
Example 20
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 91:9.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.09 percent and the appearance is free from cracking.
Example 21
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 The weight ratio of the nickel oxide powder to the magnesium oxide powder is 90:10.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.12 percent and the appearance is free from cracking.
Example 22
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 99:1.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.01 percent and the appearance is free from cracking.
Example 23
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gramWith BET at 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 98:2.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.12 percent and the appearance is free from cracking.
Example 24
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 97:3.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.10 percent and the appearance is free from cracking.
Example 25
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 96:4.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.14 percent and the appearance is free from cracking.
Example 26
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 95:5.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.02 percent and the appearance is free from cracking.
Example 27
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 94:6.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.09 percent and the appearance is free from cracking.
Example 28
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 93:7.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 97.99 percent and the appearance is free from cracking.
Example 29
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 92:8.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.02 percent and the appearance is free from cracking.
Example 30
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Oxygen per gramNickel powder and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 91:9.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.14 percent and the appearance is free from cracking.
Example 31
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Per gram of copper oxide powder, wherein the weight ratio of the nickel oxide powder to the copper oxide powder is 90:10.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.09 percent and the appearance is free from cracking.
Example 32
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 99:1.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98%, and the appearance is free from cracking.
Example 33
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 98:2.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.50 percent and the appearance is free from cracking.
Example 34
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 97:3.
the relative density of the nickel oxide-based target prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.10 percent and the appearance is free from cracking.
Example 35
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 96:4.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.07 percent and the appearance is free from cracking.
Example 36
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 95:5.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.20 percent and the appearance is free from cracking.
Example 37
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of nickel oxide powder to niobium oxide powder is 94:6.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 97.89%, and the appearance is free from cracking.
Example 38
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 93:7.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.06%, and the appearance is free from cracking.
Example 39
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 92:8.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.17 percent and the appearance is free from cracking.
Example 40
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 91:9.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.13 percent and the appearance is free from cracking.
Example 41
The difference between this example and example 4 is that a nickel oxide-based target was prepared: the nickel oxide-based powder material in the step (1) is BET of 7m 2 /g～10m 2 Nickel oxide powder per gram and BET of 7m 2 /g～10m 2 Niobium oxide powder per gram, wherein the weight ratio of the nickel oxide powder to the niobium oxide powder is 90:10.
the relative density of the nickel oxide-based target material prepared in the embodiment is measured by adopting an Archimedes method, and the result shows that the relative density is 98.17 percent and the appearance is free from cracking.
Comparative example 1
This comparative example produced a nickel oxide-based target, differing from example 4 in that: the sintering temperature in the first stage in the step (3) is 650 ℃.
The appearance of the nickel oxide-based target material prepared by the method is observed, and the result shows that the nickel oxide-based target material has cracking phenomenon.
Comparative example 2
This comparative example produced a nickel oxide-based target, differing from example 4 in that: the sintering temperature in the first stage in the step (3) is 950 ℃.
The appearance of the nickel oxide-based target material prepared by the method is observed, and the result shows that the nickel oxide-based target material has cracking phenomenon.
Comparative example 3
This comparative example produced a nickel oxide-based target, differing from example 4 in that: the second stage in step (3) is free of a sintering atmosphere (i.e., vacuum).
The appearance of the nickel oxide-based target material prepared by the method is observed, and the result shows that the nickel oxide-based target material has serious cracking phenomenon.
Comparative example 4
This comparative example produced a nickel oxide-based target, differing from example 4 in that: the sintering atmosphere in the second stage in the step (3) is air.
The appearance of the nickel oxide-based target material prepared by the method is observed, and the result shows that the nickel oxide-based target material has serious cracking phenomenon.
In order to facilitate understanding of the technical gist of the present invention, the preparation gist and the properties of the obtained targets of nickel oxide-based targets prepared in examples 1 to 41 and comparative examples 1 to 4 of the present invention were counted, and are specifically shown in table 1.
Table 1: target performance test results obtained in examples 1 to 41 and comparative examples 1 to 4 of the present invention
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From the above table 1, it is apparent from the analysis described in examples 1 to 6 that sintering by the nickel oxide-based target preparation method of the present invention does not cause cracking of the target at the sintering temperature of 1300 to 1550 ℃, and the relative density of the target is further improved as the sintering temperature is increased.
Further, as can be seen from comparing examples 6 to 7 of the present invention with comparative examples 1 to 2, the method of the present invention is used for the staged calcination, and when the calcination temperature in the first stage of sintering is 700 to 900 ℃, a target material with high relative density can be obtained without cracking; when the calcination temperature in the first stage of sintering is lower than 600 ℃ or higher than 900 ℃, as shown in comparative examples 1 and 2, the produced target material has a serious cracking phenomenon.
It can be seen from comparing examples 4, 9 and 10 of the present invention that increasing the sintering time in the second stage of sintering is also advantageous for increasing the relative density of the target.
Comparing examples 4 and 11 of the present invention with comparative examples 3 and 4, it is known that the sintering atmosphere is critical to improve the quality of the target material during the sintering process, and when the sintering atmosphere is oxygen or a nitrogen-hydrogen mixture,the prepared target material has high density and no cracking phenomenon, particularly as shown in the examples 4 and 11 of the invention, and when any atmosphere is not introduced in the sintering process or the sintering atmosphere is changed into air, the target material has obvious cracking phenomenon, mainly because the components of the target material can maintain an oxygen-enriched state, namely, the target material is all Ni 2 O 3 Does not generate oxygen deficiency component, i.e. does not cause density difference of different components of the target material, and does not generate cracking, when introducing nitrogen-hydrogen mixed gas (N 2 /H 2 When the target component is in an anoxic state, the component is NiO, i.e., the oxygen-enriched component is not present, so that the density difference of different components of the target is not caused, and cracking is not caused.
According to the description of examples 12-21, examples 22-31 and examples 32-41, the preparation method of the present invention can be used to obtain a target material with a higher density when doped with a proper amount of magnesium oxide, copper oxide or niobium oxide, and the doping is beneficial to improving cracking conditions, mainly because different dopants form small amounts of components with different densities, and the components can be used as buffers when the density of the target material changes, release a certain amount of stress, and reduce the risk of cracking.
In summary, the preparation method of the nickel oxide-based target material is simple, and the nickel oxide-based target material prepared by the method has high density and is not easy to crack when being cooled after sintering.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (11)
1. A preparation method of a nickel oxide-based target material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1, preparing nickel oxide-based powder material, dispersing agent, binder and water into slurry, and performing treatmentSpray granulation to obtain spherical granules, wherein D of the slurry 50 Less than 250nm, D of the spherical particles 50 Less than 25 μm, D of the spherical particles 90 Less than 48 μm;
step S2, performing compression molding and cold isostatic pressing on the spherical particles to obtain blank targets;
step S3, degumming the blank target material, and cooling after sectional sintering;
in step S3, the step of sintering includes a first-stage sintering and a second-stage sintering, wherein:
the sintering temperature of the first-stage sintering is 700-900 ℃, the heat preservation time is 5-10 hours, and the vacuum degree is 0.08-0.1 mpa;
the sintering temperature of the second-stage sintering is 1300-1500 ℃, the sintering time is 5-12 h, and oxygen or nitrogen-hydrogen mixture is introduced after reaching the sintering temperature of the second-stage sintering for 0.8-1.2 h;
the sintering pressure of the second stage is 0.05 mpa-0.1 mpa.
2. The method of manufacturing according to claim 1, characterized in that: the nickel oxide-based powder material is further doped with at least one oxide of magnesium oxide, copper oxide, and niobium oxide.
3. The method of manufacturing according to claim 1, characterized in that: in the nickel oxide-based powder material, the mass fraction of nickel oxide is not less than 90%.
4. The method of manufacturing according to claim 1, characterized in that: in the step S2, the pressure of compression molding is 0.1-0.8 mpa.
5. The method of manufacturing according to claim 1, characterized in that: in the step S2, the pressure of the cold isostatic pressing is 250-300 mpa.
6. The method of manufacturing according to claim 1, characterized in that: in the step S3, the degumming temperature is 400-500 ℃.
7. The method of manufacturing according to claim 1, characterized in that: the temperature rising rate when the sintering temperature of the first stage rises to the sintering temperature of the second stage is 0.5 ℃/min-1.5 ℃/min.
8. The method of manufacturing according to claim 1, characterized in that: the volume ratio of nitrogen to hydrogen in the nitrogen-hydrogen mixed gas is 98-100: 2.
9. the method of manufacturing according to claim 1, characterized in that: in the step S3, the pressure in the cooling process is 0.1 Mpa-0.5 Mpa.
10. A nickel oxide-based target, characterized in that the nickel oxide-based target is produced by the production method according to any one of claims 1 to 9.
11. Use of the nickel oxide-based target according to claim 10 for the production of perovskite solar cells.
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| CN110436922A (en) * | 2019-07-26 | 2019-11-12 | 中国建筑材料科学研究总院有限公司 | Nickel-tungsten oxide target and preparation method thereof |
| CN112456971A (en) * | 2020-11-13 | 2021-03-09 | 北京航大微纳科技有限公司 | Cold isostatic pressing preparation method of nickel oxide-based ceramic target material |
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| CN110436922A (en) * | 2019-07-26 | 2019-11-12 | 中国建筑材料科学研究总院有限公司 | Nickel-tungsten oxide target and preparation method thereof |
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