CN117285344A - IGZO target material and preparation method thereof - Google Patents
IGZO target material and preparation method thereof Download PDFInfo
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- CN117285344A CN117285344A CN202311225261.9A CN202311225261A CN117285344A CN 117285344 A CN117285344 A CN 117285344A CN 202311225261 A CN202311225261 A CN 202311225261A CN 117285344 A CN117285344 A CN 117285344A
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- Prior art keywords
- igzo
- solution
- igzo target
- carboxymethyl cellulose
- target
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- 239000013077 target material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 22
- 235000015895 biscuits Nutrition 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 26
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 24
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 24
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 23
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000853 adhesive Substances 0.000 claims description 17
- 230000001070 adhesive effect Effects 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 13
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000005238 degreasing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 238000000462 isostatic pressing Methods 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 6
- 238000007908 dry granulation Methods 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 4
- 108010073771 Soybean Proteins Proteins 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 229940071440 soy protein isolate Drugs 0.000 claims description 4
- 235000019710 soybean protein Nutrition 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000007723 die pressing method Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 24
- 239000011787 zinc oxide Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000009694 cold isostatic pressing Methods 0.000 description 4
- 229910003437 indium oxide Inorganic materials 0.000 description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000734 polysilsesquioxane polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- -1 terbium ion Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives thereof
- C04B35/6365—Cellulose or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
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- Structural Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Computer Hardware Design (AREA)
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- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses an IGZO target and a preparation method thereof, and belongs to the technical field of metal oxide target materials. The IGZO target comprises the following raw materials: ga 2 O 3 :18‑30%;ZnO:40‑55%;In 2 O 3 :15‑30%;Tb 4 O 7 :0.8-2%; and (2) a binder: 0.5-1%; dispersing agent: 0.5-1%; and (3) ball milling and mixing the raw materials, spray granulating, compression molding and biscuit sintering to obtain the IGZO target. The IGZO target material prepared by the invention is compactThe high-strength plastic has high stability up to 99.5%, expands the application field and has high industrial utilization value.
Description
Technical Field
The invention belongs to the technical field of metal oxide target materials, and particularly relates to an IGZO target material and a preparation method thereof.
Background
IGZO, which stands for indium gallium zinc oxide (Indium Gallium Zinc Oxide), is a semiconductor material commonly used for the fabrication of Thin Film Transistors (TFTs). IGZO thin film transistors are widely used in display technology, particularly in high resolution liquid crystal displays and OLED (organic light emitting diode) displays. IGZO materials are typically prepared by physical evaporation or chemical vapor deposition, among other methods. The target is a key part of the preparation of these thin film transistors, and its composition is consistent with the required IGZO material. During the preparation process, the performance and the characteristics of the thin film transistor are related to the quality and the purity of the target material.
However, with the development of display technology toward ultra-high definition, high refresh rate, low power consumption, high transparency, and the like, higher requirements are put on mobility and stability of TFTs. TFT mobility of IGZO used in current-scale mass production is only 10cm 2 ﹒V -1 ﹒s -1 About, there is also a problem of serious threshold voltage drift under Negative Bias Illumination Stress (NBIS), and it is difficult to meet the requirement of future display. Therefore, improving TFT mobility and NBIS stability is an urgent problem to be solved by oxide semiconductor materials.
Disclosure of Invention
The invention aims to provide an IGZO target and a preparation method thereof, which aim to solve the problem of low stability of the IGZO target.
The aim of the invention can be achieved by the following technical scheme:
an IGZO target comprises the following raw materials in percentage by mass:
Ga 2 O 3 :18-30%;
ZnO:40-55%;
In 2 O 3 :15-30%;
Tb 4 O 7 :0.8-2%;
and (2) a binder: 0.5-1%;
dispersing agent: 0.5-1%;
the adhesive is prepared through the following steps:
adding soybean protein isolate into deionized water, performing ultrasonic dispersion, heating to 80 ℃ and stirring for 30min, cooling to 50 ℃, adding amino functional carboxymethyl cellulose water solution, stirring in nitrogen atmosphere, adding ammonium persulfate solution, reacting for 2h, and adding CaCl 2 Stirring the solution for 30min to obtain the binder.
Further, soy protein isolate, deionized water, amino-functionalized carboxymethyl cellulose, ammonium persulfate solution, and CaCl 2 The dosage ratio of the solution is 2g:50mL:4mL:2mL:1.5mL; wherein the mass fraction of the amino-functionalized carboxymethyl cellulose aqueous solution is 6-10%, the mass fraction of the ammonium persulfate solution is 2.5%, and CaCl is used for preparing the catalyst 2 The mass fraction of the solution was 0.5%.
Further, the amino-functionalized carboxymethyl cellulose is prepared by the steps of:
POSS-NH 2 And adding the carboxymethyl cellulose aqueous solution into methanol, stirring, adding the sodium hydroxide solution, and uniformly stirring to obtain the amino-functionalized carboxymethyl cellulose. POSS-NH is selected for use 2 The purpose of the treatment agent is to introduce more amino groups to facilitate the subsequent reaction.
Further, POSS-NH 2 The dosage ratio of the carboxymethyl cellulose aqueous solution, the methanol and the sodium hydroxide solution is 2g:1.6mL:50mL:2mL; wherein the mass fraction of the carboxymethyl cellulose aqueous solution is 5%, and the pH value of the sodium hydroxide solution is 12.
Further, the dispersant is prepared by the following steps:
adding acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate into deionized water, condensing and refluxing at 50 ℃, protecting with nitrogen, adding ammonium persulfate, reacting for 3 hours at 70 ℃, and adjusting the pH of the solution to 7-8 by sodium hydroxide solution to obtain the dispersing agent.
The monomer hydroxyethyl methacrylate in the dispersing agent has hydroxyl groups, and can effectively interact with the surfaces of raw material particles in the grinding process, and be adsorbed on the surfaces of the particles to enable the particles to be in a dispersed state, so that the particles are promoted to be broken, and therefore, the dispersing agent has better dispersing and grinding assisting effects on the raw material particles.
Further, the dosage ratio of acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, hydroxyethyl methacrylate, deionized water and ammonium persulfate was 4.5g:13g:1g:50mL:0.4g.
The invention also provides a preparation method of the IGZO target, which comprises the following steps:
first step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 Adding ZnO, a dispersing agent, an adhesive, a ball milling medium and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, drying granulating powder, mould pressing for 3-5min, demoulding, and isostatic pressing to obtain an IGZO target biscuit;
thirdly, sintering the IGZO target biscuit, and heating to a degreasing temperature at a degreasing heating rate to completely degrease the biscuit; and then heating to the sintering temperature at the sintering temperature rising rate, preserving the heat for 6 hours in the oxygen atmosphere, and cooling to obtain the IGZO target.
Further, the ball milling medium is zirconia, and the size is 0.2-3mm; the diameter of the ball milling product is 0.1-2 mu m; wherein the solid content of the IGZO mixed slurry is 60%.
Further, the die pressing is set to 40-60MPa, and the isostatic pressing pressure is set to 220-250MPa; the degreasing temperature rising rate is 0.5-0.8 ℃/min, and the degreasing temperature is 600 ℃; the sintering temperature rising rate is 2-3 ℃/min, and the sintering temperature is 1300-1500 ℃.
The invention has the beneficial effects that:
the invention grafts Soy Protein Isolate (SPI) on carboxymethyl cellulose (CMC-NH) with amino 2 ) The amide bond is introduced through amidation reaction, so that the side chain of CMC is prolonged, entanglement among binder molecules is enhanced, and the viscosity of the binder is improved; and Ca is introduced on the basis 2+ The formed macromolecules are inserted between the structures of the adhesive, so that the adhesive strength and the mechanical property of the adhesive are improved, and the adhesive can bear the stress change of the target in the molding and sintering processes; a large number of hydrogen bonds and ionic bonds exist in the adhesive, so that the adhesive has certain self-repairing capability; and the addition of the hydroxymethyl cellulose binder in the process of preparing the IGZO target is beneficial to improving the density of the IGZ0 target, and ensures the yield and the production efficiency of the IGZO target.
In the process of preparing the IGZO target material, firstly, adding lanthanoid element-terbium (Tb) into indium oxide, wherein the terbium ion radius is close to the indium ion radius, and after Tb doping, in 2 O 3 The grain size change of (2) is small, namely the lattice distortion change is small, and under the condition of low content, the space overlapping between 5s orbitals of vacant In can not be basically destroyed after Tb doping; therefore, tb element with extremely strong bond energy is doped into indium oxide, and the introduction of lanthanide Tb element can effectively inhibit oxygen vacancy defect caused by indium oxide, improve the stability of indium oxide, further inhibit the concentration of oxygen vacancy defect in IGZO target material, thereby improving the mobility of TFT, greatly improving the NBIS stability, and providing a choice for the new application of oxide thin film transistor in the display direction.
The densification degree of the IGZO target prepared by the method can reach 99.5%, the IGZO target has high stability and high conductivity, and the utilization rate of the IGZO target is further improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides an adhesive, which is prepared by the following steps:
preparing amino-functionalized carboxymethyl cellulose:
adding 4mL of gamma-aminopropyl triethoxysilane and 7.5mL of hydrochloric acid solution into 90mL of methanol, stirring, heating and refluxing at 90 ℃ for 18h, cooling to room temperature, adding 62.5mL of tetrahydrofuran, centrifugally washing, and drying at 40 ℃ for 24h to obtain amino-terminated cage polysilsesquioxane (POSS-NH) 2 ). 2g of POSS-NH 2 And 1.6mL of carboxymethyl cellulose water solution are added into 50mL of methanol, stirred, added with 2mL of sodium hydroxide solution and uniformly stirred to obtain amino functionalized carboxymethylAnd (3) base cellulose.
Preparing an adhesive:
adding 2g of soybean protein isolate into 50mL of deionized water, performing ultrasonic dispersion, heating to 80 ℃ and stirring for 30min, cooling to 50 ℃, adding 4mL of amino-functionalized carboxymethyl cellulose aqueous solution (the mass fraction of the carboxymethyl cellulose aqueous solution is 7%) into nitrogen atmosphere, stirring, adding 2mL of ammonium persulfate solution, reacting for 2h, and adding 1.5mLCaCl 2 Stirring the solution for 30min to obtain the binder.
Example 2
Not only does this embodiment 1:
preparing an adhesive:
adding 2g of soybean protein isolate into 50mL of deionized water, performing ultrasonic dispersion, heating to 80 ℃ and stirring for 30min, cooling to 50 ℃, adding 4mL of amino-functionalized carboxymethyl cellulose aqueous solution (the mass fraction of the carboxymethyl cellulose aqueous solution is 9%) into nitrogen atmosphere, stirring, adding 2mL of ammonium persulfate solution, reacting for 2h, and adding 1.5mLCaCl 2 Stirring the solution for 30min to obtain the binder.
Example 3
This example provides a dispersant made by the steps of:
4.5g of acrylic acid, 13g of 2-acrylamide-2-methylpropanesulfonic acid and 1g of hydroxyethyl methacrylate are added into 50mL of deionized water, condensed and refluxed at 50 ℃, and reacted for 3 hours at 70 ℃ under the protection of nitrogen, 0.4g of ammonium persulfate is added, and the pH of the solution is regulated to 7 by sodium hydroxide solution, so as to obtain the dispersing agent.
Example 4
The embodiment provides a preparation method of an IGZO target, which comprises the following specific steps:
weighing the following raw materials in percentage by mass:
Ga 2 O 3 :25%;ZnO:48%;In 2 O 3 :25%;Tb 4 O 7 :0.8%; and (2) a binder: 0.6%; dispersing agent: 0.6%.
First step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 ZnO, dispersant, adhesive, oxygenAdding zirconium oxide and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, putting the dried granulating powder into a hydraulic press, setting the mould pressing pressure to 40MPa, maintaining the pressure for 5min, demoulding, further performing press forming in a cold isostatic pressing machine by using a flexible mould, setting the pressure to 235MPa, and obtaining the IGZO target biscuit with high density, good uniformity and regular shape;
thirdly, placing the IGZO target biscuit into a sintering furnace, and heating to the degreasing temperature of 600 ℃ at the heating rate of 0.5 ℃/min to completely degrease the biscuit; and then heating to 1350 ℃ at a heating rate of 2 ℃/min, introducing oxygen in the heating process, preserving heat for 6 hours, and cooling to obtain the IGZO target.
Example 5
Weighing the following raw materials in percentage by mass:
Ga 2 O 3 :25%;ZnO:50%;In 2 O 3 :23%;Tb 4 O 7 :0.5%; and (2) a binder: 0.75%; dispersing agent: 0.75%.
First step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 Adding ZnO, a dispersing agent, an adhesive, zirconia and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, putting the dried granulating powder into a hydraulic press, setting the mould pressing pressure to be 50MPa, maintaining the pressure for 5min, demoulding, further pressing and forming the biscuit in a cold isostatic pressing machine by using a flexible mould, setting the pressure to be 240MPa, and obtaining the IGZO target biscuit with high density, good uniformity and regular shape;
thirdly, placing the IGZO target biscuit into a sintering furnace, and heating to the degreasing temperature of 600 ℃ at the heating rate of 0.6 ℃/min to completely degrease the biscuit; and then heating to the sintering temperature of 1400 ℃ at a heating rate of 3 ℃/min, introducing oxygen in the heating process, preserving heat for 6 hours, and cooling to obtain the IGZO target.
Example 6
Weighing the following raw materials in percentage by mass:
Ga 2 O 3 :23%;ZnO:52%;In 2 O 3 :23%;Tb 4 O 7 :1%; and (2) a binder: 0.5%; dispersing agent: 0.5%.
First step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 Adding ZnO, a dispersing agent, an adhesive, zirconia and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, putting the dried granulating powder into a hydraulic press, setting the mould pressing pressure to 55MPa, maintaining the pressure for 5min, demoulding, further performing press forming in a cold isostatic pressing machine by using a flexible mould, setting the pressure to 225MPa, and obtaining the IGZO target biscuit with high density, good uniformity and regular shape;
thirdly, placing the IGZO target biscuit into a sintering furnace, and heating to the degreasing temperature of 600 ℃ at the heating rate of 0.7 ℃/min to completely degrease the biscuit; and then heating to the sintering temperature of 1450 ℃ at a heating rate of 2 ℃/min, introducing oxygen in the heating process, preserving heat for 6 hours, and cooling to obtain the IGZO target.
Example 7
Weighing the following raw materials in percentage by mass:
Ga 2 O 3 :20%;ZnO:43%;In 2 O 3 :25%;Tb 4 O 7 :0.8%; and (2) a binder: 0.5%; dispersing agent: 0.7%.
First step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 Adding ZnO, a dispersing agent, an adhesive, zirconia and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, putting the dried granulating powder into a hydraulic press, setting the mould pressing pressure to be 50MPa, maintaining the pressure for 5min, demoulding, further pressing and forming the biscuit in a cold isostatic pressing machine by using a flexible mould, setting the pressure to be 230MPa, and obtaining the IGZO target biscuit with high density, good uniformity and regular shape;
thirdly, placing the IGZO target biscuit into a sintering furnace, and heating to the degreasing temperature of 600 ℃ at the heating rate of 0.8 ℃/min to completely degrease the biscuit; and then heating to the sintering temperature of 1500 ℃ at a heating rate of 3 ℃/min, introducing oxygen in the heating process, preserving heat for 6 hours, and cooling to obtain the IGZO target.
Comparative example 1
The IGZO target was obtained without the binder of example 4, and the remaining raw materials and preparation process were kept unchanged.
Comparative example 2
The dispersing agent in example 4 is not added, so that the IGZO target material is obtained, and the rest raw materials and the preparation process are kept unchanged.
Density testing was performed on examples 4-7 and comparative examples 1-2: the relative density of the IGZO target was determined using archimedes' displacement method.
The test results are shown in table 1:
TABLE 1
Project | Example 4 | Example 5 | Example 6 | Examples7 | Comparative example 1 | Comparative example 2 |
Relative density/% | 99.2 | 99.4 | 99.5 | 99.5 | 98.1 | 98.3 |
As can be seen from Table 1, the relative densities obtained in examples 4-7 were very high, indicating that the IGZO targets produced by the present invention have very high densities.
The IGZO targets prepared in examples 4 to 7 and comparative examples 1 to 2 were subjected to a sputtering process using a JGP-450 type magnetron sputtering machine to prepare an IGZO thin film having a diameter of 76mm, and the following test was performed:
hall effect test: the resistivity and hall mobility were measured using the us 8400 hall effect test with a sample size of 10mm x 10mm and a magnetic field size set to 0.5T.
Optical performance test: the light transmittance was measured using a TU-1901 type double beam ultraviolet-visible photometer.
The test results are shown in table 2:
TABLE 2
As can be seen from table 2, the IGZO films prepared in examples 4 to 7 were excellent in optical properties with respect to the average transmittance in comparative examples 1 to 2, and had potential as transparent conductive materials; the lower resistivity and higher mobility in examples 4-7 indicate that the IGZO target prepared by the method is very excellent in stability and has a wide application prospect.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The IGZO target is characterized by comprising the following raw materials in percentage by mass:
Ga 2 O 3 :18-30%;
ZnO:40-55%;
In 2 O 3 :15-30%;
Tb 4 O 7 :0.8-2%;
and (2) a binder: 0.5-1%;
dispersing agent: 0.5-1%;
the adhesive is prepared through the following steps:
adding soybean protein isolate into deionized water, performing ultrasonic dispersion, heating to 80 ℃ and stirring for 30min, cooling to 50 ℃, adding amino functional carboxymethyl cellulose water solution, stirring in nitrogen atmosphere, adding ammonium persulfate solution, reacting for 2h, and adding CaCl 2 Stirring the solution for 30min to obtain the binder.
2. A according to claim 1IGZO target material is characterized in that soy protein isolate, deionized water, amino functional carboxymethyl cellulose, ammonium persulfate solution and CaCl 2 The dosage ratio of the solution is 2g:50mL:4mL:2mL:1.5mL; wherein the mass fraction of the amino-functionalized carboxymethyl cellulose aqueous solution is 6-10%, the mass fraction of the ammonium persulfate solution is 2.5%, and CaCl is used for preparing the catalyst 2 The mass fraction of the solution was 0.5%.
3. The IGZO target material according to claim 1, characterized in that the amino-functionalized carboxymethyl cellulose is prepared by the steps of:
POSS-NH 2 And adding the carboxymethyl cellulose aqueous solution into methanol, stirring, adding the sodium hydroxide solution, and uniformly stirring to obtain the amino-functionalized carboxymethyl cellulose.
4. An IGZO target according to claim 3, characterized by POSS-NH 2 The dosage ratio of the carboxymethyl cellulose aqueous solution, the methanol and the sodium hydroxide solution is 2g:1.6mL:50mL:2mL; wherein the mass fraction of the carboxymethyl cellulose aqueous solution is 5%, and the pH value of the sodium hydroxide solution is 12.
5. The IGZO target material according to claim 1, wherein the dispersant is prepared by:
adding acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate into deionized water, condensing and refluxing at 50 ℃, protecting with nitrogen, adding ammonium persulfate, reacting for 3 hours at 70 ℃, and adjusting the pH of the solution to 7-8 by sodium hydroxide solution to obtain the dispersing agent.
6. The IGZO target of claim 5, wherein the ratio of acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, hydroxyethyl methacrylate, deionized water, and ammonium persulfate is 4.5g:13g:1g:50mL:0.4g.
7. The method for preparing an IGZO target according to claim 1, comprising the steps of:
first step, in 2 O 3 、Tb 4 O 7 、Ga 2 O 3 Adding ZnO, a dispersing agent, an adhesive, a ball milling medium and pure water into a ball mill, and ball milling for 36 hours to obtain IGZO mixed slurry; placing the IGZO mixed slurry into an atomization granulator, and spray-drying to obtain dry granulation powder;
secondly, adopting a mould pressing-isostatic pressing mode, drying granulating powder, mould pressing for 3-5min, demoulding, and isostatic pressing to obtain an IGZO target biscuit;
thirdly, sintering the IGZO target biscuit, and heating to a degreasing temperature at a degreasing heating rate to completely degrease the biscuit; and then heating to the sintering temperature at the sintering temperature rising rate, preserving the heat for 6 hours in the oxygen atmosphere, and cooling to obtain the IGZO target.
8. The method for preparing the IGZO target material according to claim 7, wherein the ball milling medium is zirconia, and the size is 0.2-3mm; the diameter of the ball milling product is 0.1-2 mu m; wherein the solid content of the IGZO mixed slurry is 60%.
9. The method for producing an IGZO target according to claim 7, wherein the die pressing is set to 40 to 60MPa, and the isostatic pressing pressure is set to 220 to 250MPa; the degreasing temperature rising rate is 0.5-0.8 ℃/min, and the degreasing temperature is 600 ℃; the sintering temperature rising rate is 2-3 ℃/min, and the sintering temperature is 1300-1500 ℃.
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