CN115849896B - Zinc oxide target material and preparation method and application thereof - Google Patents
Zinc oxide target material and preparation method and application thereof Download PDFInfo
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- CN115849896B CN115849896B CN202211520371.3A CN202211520371A CN115849896B CN 115849896 B CN115849896 B CN 115849896B CN 202211520371 A CN202211520371 A CN 202211520371A CN 115849896 B CN115849896 B CN 115849896B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 324
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 136
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000013077 target material Substances 0.000 title claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 70
- 238000005238 degreasing Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000000748 compression moulding Methods 0.000 claims abstract description 32
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 73
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000002243 precursor Substances 0.000 claims description 41
- 238000001354 calcination Methods 0.000 claims description 24
- 239000007790 solid phase Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 230000001105 regulatory effect Effects 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 150000007529 inorganic bases Chemical group 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- ZMCUDHNSHCRDBT-UHFFFAOYSA-M caesium bicarbonate Chemical compound [Cs+].OC([O-])=O ZMCUDHNSHCRDBT-UHFFFAOYSA-M 0.000 claims description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 2
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 38
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 26
- 230000000630 rising effect Effects 0.000 description 24
- 239000002002 slurry Substances 0.000 description 24
- 239000007921 spray Substances 0.000 description 18
- 239000011230 binding agent Substances 0.000 description 15
- 238000002156 mixing Methods 0.000 description 14
- 238000000227 grinding Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000011592 zinc chloride Substances 0.000 description 13
- 235000005074 zinc chloride Nutrition 0.000 description 13
- 238000004108 freeze drying Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 230000001276 controlling effect Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000012527 feed solution Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a zinc oxide target material and a preparation method and application thereof. The preparation method of the zinc oxide target material comprises the following steps: the method comprises the following steps: compression molding zinc oxide powder, and performing cold isostatic pressing, degreasing and sintering to obtain a zinc oxide target; wherein the particle size of the zinc oxide powder is 10-20 mu m; the sintering temperature is 1000-1200 ℃; the density of the prepared zinc oxide target material is 5.3g/cm 3 ‑5.6g/cm 3 . The preparation method of the zinc oxide target material is simple and low in cost, and the zinc oxide target material with high density, high purity and uniform color can be prepared by adopting the method, so that the method has wide application prospect.
Description
Technical Field
The invention relates to the technical field of photoelectric functional materials, in particular to a zinc oxide target material and a preparation method and application thereof.
Background
Zinc oxide (ZnO) is a wide forbidden band II-VI semiconductor material, has the advantages of high melting point, low deposition temperature, low electron induced defects and the like, has wide sources of raw materials and simple preparation method, and is widely applied to solar cells, ultraviolet detectors, surface acoustic wave devices, gas sensors, transparent electrodes and the like as a target material.
Related researches show that the density of the target material and the uniformity of the microstructure have important influence on the quality of the sputtered film. In the related art, zinc oxide targets are prepared by adopting hot isostatic pressing and hot-pressed sintering methods, and in order to improve the density of the targets, doping other metal elements such as niobium, tin, indium, aluminum and the like are selected. Although the compactness of the target material is improved to a certain extent, the method is high in cost and difficult to realize large-scale mass production.
Therefore, there is a need for a zinc oxide target material and a method for preparing the same that is low in cost, simple in preparation method, and has good uniformity and density.
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 of the zinc oxide target material, which can effectively improve the density and uniformity of the zinc oxide target material.
The invention also provides a zinc oxide target material prepared by the method.
The invention also provides application of the zinc oxide target in preparation of OLED display.
According to an embodiment of the first aspect of the invention, a preparation method of a zinc oxide target material comprises the following steps:
compression molding zinc oxide powder, and performing cold isostatic pressing, degreasing and sintering to obtain a zinc oxide target;
wherein the particle size of the zinc oxide powder is 10-20 mu m;
the sintering temperature is 1000-1200 ℃;
the density of the prepared zinc oxide target material is 5.3g/cm 3 -5.6g/cm 3 。
The preparation method of the zinc oxide target material has at least the following beneficial effects:
compared with the traditional hot-pressed sintering or hot isostatic pressing sintering, the production cost of the zinc oxide target is obviously reduced, and the prepared zinc oxide target has the characteristics of good uniformity, high density and the like. Secondly, the zinc oxide target material does not need to be doped with other metal elements which assist in densification in the preparation process, so that the prepared zinc oxide target material has higher purity.
In the examples of the present invention, a specific surface area of 5m was used 2 /g-15m 2 The result shows that the zinc oxide powder with the specific surface area has higher sintering activity and is easier to sinter, and the zinc oxide target with higher density and purity can be obtained by screening relevant preparation parameters.
According to some embodiments of the invention, D of the zinc oxide powder 50 8 μm to 12 μm.
The smaller the particle size of the zinc oxide powder in the present invention, the higher the sintering activity, the easier it is to burn the high density and uniformity.
According to some embodiments of the invention, D of the zinc oxide powder 50 Is 10 μm.
According to some embodiments of the present invention, the method for preparing zinc oxide powder comprises the steps of:
step S1: uniformly stirring zinc raw material liquid, adding a pH regulator, regulating the pH to 6-8 for reaction, carrying out solid-liquid separation after the reaction is completed, collecting a solid phase, drying the solid phase, and calcining to obtain a zinc oxide precursor;
step S2: and spraying and granulating the zinc oxide precursor to obtain the zinc oxide powder.
According to some embodiments of the invention, the pH is adjusted to 6-7.
According to some embodiments of the invention, the pH is adjusted to 7.
According to some embodiments of the invention, the reaction is ball milled or emulsified.
Ball milling or emulsification treatment is beneficial to improving the specific surface area of the solid product, avoiding aggregation of the solid product, and further reducing the surface energy and interface energy of the system.
According to some embodiments of the invention, the zinc feed solution is a zinc chloride solution.
According to some embodiments of the invention, the molar concentration of zinc in the zinc feed solution is 0.1mol/L to 0.3mol/L.
According to some embodiments of the invention, the molar concentration of zinc in the zinc feed solution is 0.2mol/L to 0.3mol/L.
According to some embodiments of the invention, the molar concentration of zinc in the zinc feed solution is 0.2mol/L.
According to some embodiments of the invention, the pH adjuster is an inorganic base or carbonate.
According to some embodiments of the invention, the inorganic base is at least one of sodium hydroxide, potassium hydroxide, cesium hydroxide, and ammonia monohydrate.
According to some embodiments of the invention, the carbonate is at least one of sodium carbonate, potassium carbonate, cesium carbonate, sodium bicarbonate, potassium bicarbonate, and cesium bicarbonate.
According to some embodiments of the invention, the temperature of the reaction is 20 ℃ to 45 ℃.
According to some embodiments of the invention, the temperature of the reaction is 20 ℃ to 40 ℃.
According to some embodiments of the invention, the temperature of the reaction is 25 ℃ to 35 ℃.
According to some embodiments of the invention, the temperature of the reaction is 30 ℃.
The reaction temperature directly affects the utilization rate of raw materials and the filtration performance of products. When the temperature is too low, the zinc raw material liquid is difficult to form a certain supersaturation degree, the incomplete reaction is easy to cause, and the product yield is low; when the temperature is too high, the yield of the product is obviously improved, but the reaction temperature has influence on the grain growth and the crystal nucleus formation speed, so that the obtained particle sizes are different at different reaction temperatures, the crystal nucleus growth speed is accelerated to a certain extent due to the too high temperature, larger solid particles are formed, and the surface performance of the solid particles is further influenced.
According to some embodiments of the invention, the solid phase prior to calcination has a specific surface area of 60m 2 /g-130m 2 /g。
According to some embodiments of the invention, the solid phase prior to calcination has a specific surface area of 80m 2 /g-120m 2 /g。
According to some embodiments of the invention, the solid phase prior to calcination has a specific surface area of 100m 2 /g-110m 2 /g。
According to some embodiments of the invention, the solid phase prior to calcination has a specific surface area of 100m 2 /g。
According to some embodiments of the invention, the calcination temperature is 700 ℃ to 1000 ℃.
According to some embodiments of the invention, the calcination temperature is 800 ℃ to 1000 ℃.
According to some embodiments of the invention, the calcination temperature is 800 ℃ to 900 ℃.
According to some embodiments of the invention, the calcination temperature is 860 ℃.
The calcination temperature is too low, which is easy to lead to incomplete decomposition of solid products and low purity of zinc oxide precursor; too high a temperature tends to increase the particle size of the zinc oxide precursor and may cause agglomeration of the grains, affecting the quality of the zinc oxide precursor.
According to some embodiments of the invention, the zinc oxide precursor has a specific surface area of 5m 2 /g-15m 2 /g。
According to some embodiments of the invention, the specific surface area of the zinc oxide precursor is 8m 2 /g-12m 2 /g。
According to some embodiments of the invention, the specific surface area of the zinc oxide precursor is 10m 2 /g-12m 2 /g。
According to some embodiments of the invention, the specific surface area of the zinc oxide precursor is 10m 2 /g。
The specific surface area of the zinc oxide precursor is an important influencing factor for preparing the high-density zinc oxide target, and if the specific surface area of the zinc oxide precursor is too low, the high-density zinc oxide target is difficult to prepare; if the specific surface area of the zinc oxide precursor is too high, the zinc oxide target can be cracked. Therefore, the proper specific surface area of the zinc oxide precursor is selected, so that the density of the zinc oxide target can be improved, and the cracking state of the zinc oxide target can be effectively avoided.
According to some embodiments of the invention, the specific steps of spray granulation include: mixing the zinc oxide precursor, water and a binder in a ratio of 60:38:2, mixing the solid and the liquid in a ratio, and then placing the mixture into a spray tower for spray granulation;
preferably, the air inlet temperature of the spray tower is 220-280 ℃;
preferably, the air outlet temperature of the spray tower is 110-130 ℃.
According to some embodiments of the invention, the compression molding is performed at a pressure of 0.1MPa to 0.8MPa.
According to some embodiments of the invention, the compression molding is performed at a pressure of 0.2MPa to 0.6MPa.
According to some embodiments of the invention, the compression molding is performed at a pressure of 0.3MPa to 0.5MPa.
According to some embodiments of the invention, the compression molding is performed at a pressure of 0.4Mpa.
According to some embodiments of the invention, the cold isostatic pressure is 200MPa-400MPa.
According to some embodiments of the invention, the cold isostatic pressure is 300MPa-400MPa.
According to some embodiments of the invention, the cold isostatic pressure is 350MPa.
The cold isostatic pressing mode is favorable for reducing friction among zinc oxide powder during forming, further improves density distribution of pressed billets, and a certain amount of forming agent is needed to be added in the traditional cold isostatic pressing forming process to promote forming, but because the zinc oxide has higher chemical activity, any residual forming agent can cause negative effects in the subsequent sintering process and pollute products, and no forming agent is added in the invention, so that negative influence of the forming agent in the subsequent sintering process is reduced to a certain extent.
In the cold isostatic pressing forming process, the proper pressure is favorable for improving the quality of the blank target, in general, the relative density of the blank target is increased along with the increase of the forming pressure, but the blank target is easily cracked due to the fact that the pressure is too high, and the quality of the target is further influenced.
According to some embodiments of the invention, the degreasing temperature is 400 ℃ to 700 ℃.
According to some embodiments of the invention, the degreasing temperature is 450 ℃ to 600 ℃.
According to some embodiments of the invention, the degreasing temperature is 500 ℃.
Suitable degreasing temperatures facilitate rapid removal of the binder incorporated during spray granulation.
According to some embodiments of the invention, the degreasing is performed at a heating rate of 0.5 ℃/min to 2 ℃/min.
According to some embodiments of the invention, the degreasing is performed at a heating rate of 0.5 ℃/min to 1 ℃/min.
According to some embodiments of the invention, the degreasing is performed at a heating rate of 1 ℃/min.
According to some embodiments of the invention, the degreasing and heating are performed for 4-6 hours.
According to some embodiments of the invention, the degreasing is kept for 5 hours after heating.
According to some embodiments of the invention, the sintering temperature is 1000 ℃ to 1500 ℃.
According to some embodiments of the invention, the sintering temperature is 1000 ℃ to 1400 ℃.
According to some embodiments of the invention, the sintering temperature is 1000 ℃ to 1200 ℃.
According to some embodiments of the invention, the sintering temperature is 1150 ℃.
With the increase of sintering temperature, the shrinkage rate is increased, but the temperature is too high, so that crystals are easy to grow up, and the quality of products is further affected.
According to some embodiments of the invention, the sintering is at a rate of temperature rise of 0.5 ℃/min to 5 ℃/min.
According to some embodiments of the invention, the sintering is at a rate of temperature rise of 2 ℃/min to 3 ℃/min.
According to some embodiments of the invention, the sintering is at a rate of 2 ℃/min.
In the invention, the temperature rise and drop speed is too high, and cracking is easy to occur.
According to some embodiments of the invention, the cooling rate of the sintering is 5 ℃/min-10 ℃/min.
According to some embodiments of the invention, the cooling rate of the sintering is between 6 ℃/min and 7 ℃/min.
According to some embodiments of the invention, the cooling rate of the sintering is 6 ℃/min.
According to some embodiments of the invention, the sintering process is performed at 101.325kPa (normal pressure).
According to the zinc oxide target material, the zinc oxide target material is prepared by adopting the preparation method of the zinc oxide target material.
The zinc oxide target material adopts all the technical schemes of the preparation method of the zinc oxide target material in the embodiment, so that the zinc oxide target material has at least all the beneficial effects brought by the technical schemes of the embodiment.
The application of the zinc oxide target in preparing OLED display according to the embodiment of the third aspect of the invention.
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.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a diagram of a zinc oxide target prepared in example 1 of the present 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 an embodiment of the present invention, the binder is polyvinyl alcohol, purchased from national pharmaceutical chemicals, inc.
No particular technique or condition is identified in the embodiments, as per the techniques and conditions described in the literature in this field, or as per the product specifications. The reagents or apparatus used, not designated the manufacturer, are all conventional products commercially available through regular channels.
Example 1
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.1mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 15m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 2
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 3
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.3mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 5m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 4
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 6 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 12m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 5
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 8 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 8m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 6
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1000 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 7
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1050 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 8
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor, wherein the specific surface of zinc oxide precursorThe product is 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1100 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Example 9
The embodiment is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1200 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
And S5, grinding the sintered blank into a sheet shape to obtain a zinc oxide target material, and carrying out test characterization on the zinc oxide target material.
Comparative example 1
The comparative example is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.05mol/L, regulating the pH value to 7 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, and calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 22m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Comparative example 2
The comparative example is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, regulating the pH value to 8.5 by dropwise adding a sodium hydroxide solution for reaction, controlling the reaction temperature to be about 30 ℃, simultaneously circulating a reaction solution through ball milling in the reaction process, and carrying out solid-liquid separation after the reaction is completed; collecting solid phase, washing, freeze drying, calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 18m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1150 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Comparative example 3
The comparative example is a preparation method of a zinc oxide target, comprising the following steps:
step S1, fully and uniformly stirring a zinc chloride solution with the concentration of 0.2mol/L, and adjusting the pH value to 7 by dropwise adding a sodium hydroxide solution to react, wherein the reaction temperature is controlled to be about 30 ℃, and the reaction process is carried outMeanwhile, the reaction liquid is circulated through ball milling, and after the reaction is completed, solid and liquid are separated; collecting solid phase, washing, freeze drying, calcining at 860 deg.C for 2 hr to obtain zinc oxide precursor with specific surface area of 10m 2 /g。
Step S2, mixing a zinc oxide precursor, water and a binder in a ratio of 60:38:2, obtaining slurry, then granulating the slurry in a spray tower to obtain zinc oxide powder, wherein the air inlet temperature is 250 ℃ and the air outlet temperature is 120 ℃ in the granulating process, and the zinc oxide powder D is obtained 50 Is 10 μm.
And step S3, carrying out compression molding on zinc oxide powder under the pressure of 0.4MPa, and carrying out cold isostatic pressing after compression molding under the pressure of 350MPa to obtain the blank target.
Step S4, degreasing the blank target at 500 ℃, and sintering the degreased blank target at 1550 ℃ for 300min to obtain a zinc oxide target; wherein the temperature rising speed of the degreasing temperature is 1 ℃/min, and the degreasing temperature is kept for 5 hours after being raised to 500 ℃; the temperature rising speed of sintering is 2 ℃/min; the temperature reduction rate of sintering is 6 ℃/min.
And S5, grinding the sintered blank into a sheet shape to obtain the zinc oxide target.
Test case
The surface area, density and appearance of the zinc oxide targets prepared in examples 1 to 9 and comparative examples 1 to 3 were examined and observed, and the test results are shown in table 1.
Table 1: test results of Performance of Zinc oxide targets prepared in examples 1-9 and comparative examples 1-3 of the present invention
As can be seen from examples 1, 2 and 3, as the concentration of the zinc solution increases, the BET value before the stage firing decreases, the BET decreases gradually after the firing and the target density decreases gradually under the same firing conditions, and when the BET value is too high, cracking occurs during the sintering of the target. Under the same conditions, the higher the solution concentration, the lower the sintering activity of the powder and the lower the sintering density of the target, wherein the zinc oxide target prepared in example 1 is shown in fig. 1.
It can be seen from examples 2, 4, 5 that the magnitude of the pH has a significant effect on the sintering activity of the powder, the lower the pH the higher the sintering density.
Further, it can be seen from examples 2, 6, 7, 8, 9 that the effect of different sintering temperatures on the target density, the higher the temperature, the higher the sintering density, but the slower the growth rate.
In conclusion, the preparation method of the zinc oxide target material adopts a cold isostatic pressing mode to prepare the target material, so that higher density and uniformity can be obtained at lower temperature and normal pressure, and compared with the traditional hot-pressed sintering or hot isostatic pressing sintering, the production cost is obviously reduced. Secondly, the zinc oxide target material does not need to be doped with other metal elements which assist in densification in the preparation process, so that the prepared zinc oxide target material has higher purity.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the zinc oxide target is characterized by comprising the following steps:
compression molding zinc oxide powder, and performing cold isostatic pressing, degreasing and sintering to obtain a zinc oxide target;
wherein the particle size of the zinc oxide powder is 10-20 mu m;
the sintering temperature is 1000-1200 ℃;
the density of the prepared zinc oxide target material is 5.3g/cm 3 -5.6g/cm 3 ；
The preparation method of the zinc oxide powder comprises the following steps:
step S1: uniformly stirring zinc raw material liquid, adding a pH regulator, regulating the pH to 6-7 for reaction, carrying out solid-liquid separation after the reaction is completed, collecting a solid phase, drying the solid phase, and calcining to obtain a zinc oxide precursor;
step S2: spraying and granulating the zinc oxide precursor to obtain zinc oxide powder;
ball milling or emulsification is needed in the reaction;
the specific surface area of the zinc oxide precursor is 8m 2 /g-15 m 2 /g；
The molar concentration of zinc in the zinc raw material liquid is 0.15mol/L-0.3mol/L.
2. The method for preparing a zinc oxide target according to claim 1, wherein the pH adjuster is an inorganic base or carbonate.
3. The method for preparing a zinc oxide target according to claim 2, wherein the inorganic base is at least one of sodium hydroxide, potassium hydroxide, cesium hydroxide and ammonia monohydrate.
4. The method for preparing a zinc oxide target according to claim 2, wherein the carbonate is at least one of sodium carbonate, potassium carbonate, cesium carbonate, sodium bicarbonate, potassium bicarbonate, and cesium bicarbonate.
5. The method for preparing a zinc oxide target according to claim 1, wherein the reaction temperature is 20-45 ℃.
6. The method for preparing a zinc oxide target according to claim 1, wherein the calcining temperature is 700 ℃ to 1000 ℃.
7. The method for producing a zinc oxide target according to any one of claims 1 to 6, wherein the pressure of the compression molding is 0.1MPa to 0.8MPa.
8. The method for preparing a zinc oxide target according to any one of claims 1 to 6, wherein the pressure of the cold isostatic pressing is 200MPa to 400MPa.
9. The method for preparing a zinc oxide target according to any one of claims 1 to 6, wherein the degreasing temperature is 400 ℃ to 700 ℃.
10. A zinc oxide target, characterized in that it is prepared by the preparation method of any one of claims 1 to 9.
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| CN103193262A (en) * | 2013-04-09 | 2013-07-10 | 桂林电子科技大学 | Indium-gallium-zinc oxide powder and preparation method of ceramic target thereof |
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| 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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| JP2014172783A (en) * | 2013-03-08 | 2014-09-22 | Ube Material Industries Ltd | Zinc oxide powder and method for producing the same |
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