CN115448720A - Preparation method of plasma spraying yttrium oxide coating powder - Google Patents
Preparation method of plasma spraying yttrium oxide coating powder Download PDFInfo
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- CN115448720A CN115448720A CN202211071316.0A CN202211071316A CN115448720A CN 115448720 A CN115448720 A CN 115448720A CN 202211071316 A CN202211071316 A CN 202211071316A CN 115448720 A CN115448720 A CN 115448720A
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000011248 coating agent Substances 0.000 title claims abstract description 21
- 238000000576 coating method Methods 0.000 title claims abstract description 21
- 238000007750 plasma spraying Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 20
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 229910001593 boehmite Inorganic materials 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005245 sintering Methods 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000005507 spraying Methods 0.000 abstract description 8
- 230000003628 erosive effect Effects 0.000 abstract description 6
- 238000005530 etching Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000007751 thermal spraying Methods 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 239000011224 oxide ceramic Substances 0.000 description 4
- 229910052574 oxide ceramic Inorganic materials 0.000 description 4
- 238000005524 ceramic coating Methods 0.000 description 3
- 102220043159 rs587780996 Human genes 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical group [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3218—Aluminium (oxy)hydroxides, e.g. boehmite, gibbsite, alumina sol
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- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The invention provides a preparation method of yttrium oxide coating powder for plasma spraying, belonging to the technical field of ceramic powder for thermal spraying. The invention adopts the yttrium oxide powder with larger primary crystal size as the raw material, and introduces a small amount of alumina sol as the sintering aid, thereby not only greatly reducing the sintering temperature of the large-size primary crystal yttrium oxide, but also keeping the erosion resistance of the large-size primary crystal yttrium oxide powder, and the aluminum oxide spraying powder can also be used as the spraying material for semiconductor etching, so the final using effect of the powder can not be influenced.
Description
Technical Field
The invention relates to the technical field of ceramic powder for thermal spraying, in particular to a preparation method of yttrium oxide coating powder for plasma spraying.
Background
In the dry etching process of semiconductor manufacture, thermal spraying high-purity yttrium oxide powder is generally used for coating protection of etching equipment, because the reaction of halogen-based corrosive gases such as fluorine-based corrosive gases and chlorine-based corrosive gases is often utilized in the current dry etching processPlasma etching is performed with high performance. Typical corrosive halogen gas components are, for example: fluorine-based gas: SF 6 、CF 4 、CHF 3 、ClF 3 HF, chlorine-based gas: cl 2 、BCl 3 And HCl, and these halogen gases are converted into plasma after microwaves and high frequencies are introduced into the atmosphere of these gases.
All parts of the apparatus exposed to the halogen plasma require high corrosion resistance. Originally, because plasma power is small and temperature is low, anodic oxidation and aluminum oxide coating spraying are selected originally, but as the size of wafers is continuously increased, the power of plasma equipment is also continuously increased, the traditional aluminum oxide ceramic coating can not meet the requirement, and the yttrium oxide coating has the advantages of better plasma corrosion resistance and longer service life than the aluminum oxide ceramic coating, for example, on power equipment with the power of more than 800W, the maintenance period of yttrium oxide is more than four times of that of aluminum oxide, so the yttrium oxide has gradually replaced aluminum oxide ceramic coating materials, and is widely applied to semiconductor and TFT Liquid Crystal Display (LCD) production equipment, for example: chamber walls in etchers of Plasma etch equipment (Plasma etch recipes), ESC Electrostatic chucks (ESC Electrostatic chucks), focus rings, gas injectors, chamber liners, substrate supports, dielectric windows, ring members, clamps, gas distribution plates, wafer cover rings, CVD equipment (cvrequrements), and the like.
The publication number CA102145913A describes a method for preparing nano yttrium oxide precursor powder and then carrying out densification treatment by using a water-stable plasma gun.
The publication number CA103449816B describes a process for preparing yttrium oxide spraying powder by depolymerizing, puffing, pelletizing and high-temperature processing nano or superfine yttrium oxide.
The publication number CA101182207B describes a process for preparing nano or superfine yttrium oxide suspension, granulating, heat treating, and then carrying out water-stable plasma treatment.
Known data prove that in the etching field, the erosion resistance of fused dense yttrium oxide is more than sintered yttrium oxide ceramic body is more than plasma spraying large-grain yttrium oxide is more than plasma spraying nano yttrium oxide is more than an aluminum oxide material, so an yttrium oxide coating prepared from nano powder is not strong in erosion resistance, and the larger the original crystal size of yttrium oxide powder is, the more difficult the sintering is, for example, yttrium oxide granulated powder with original grains of D50=1 micron, the sintering temperature is over 1750 ℃, and the sintering of the powder by the existing sintering equipment is very difficult.
Disclosure of Invention
Based on the above, the invention aims to provide a preparation method of plasma spraying yttrium oxide coating powder, wherein a small amount of alumina sol is introduced into yttrium oxide powder with larger primary crystal size as a sintering aid, so that the sintering temperature of large-size primary crystal yttrium oxide can be greatly reduced, the erosion resistance of large-size primary crystal yttrium oxide powder can be kept, and the aluminum oxide spraying powder can also be used as a spraying material for semiconductor etching, so that the final using effect of the powder is not influenced.
The preparation method of the plasma spraying yttrium oxide coating powder comprises the following steps:
(1) Selecting boehmite, adding pure water for dilution, heating to 80-84 ℃, adding concentrated nitric acid while stirring, and aging at 80-84 ℃ for 5 hours to obtain alumina sol;
(2) Mixing high-purity yttrium oxide powder with pure water, stirring and dispersing, adding the alumina sol prepared in the step (1), adding a binder, a dispersing agent and a defoaming agent, stirring and wrapping to form slurry;
(3) Granulating and drying the slurry obtained in the step (2) by adopting a spray granulation process to obtain granulated powder;
(4) Calcining the granulated powder at 1400-1700 ℃, cooling, and screening and classifying.
Preferably, the mass ratio of the boehmite to the pure water in the step (1) is 3-4: 1, the concentration of the concentrated nitric acid is more than 65%.
Preferably, the high-purity yttrium oxide powder in step (2) is micron-sized high-purity yttrium oxide powder, the purity of the micron-sized high-purity yttrium oxide powder is greater than 99.9%, and the particle size D50 of the micron-sized high-purity yttrium oxide powder is smaller than 6 microns.
Preferably, the micron-sized high-purity yttrium oxide powder is at least one of common yttrium oxide powder, electric melting yttrium oxide powder or yttrium oxide melted by an induction furnace.
Preferably, the mass ratio of the high-purity yttrium oxide powder in the step (2) to the pure water is 5-6:1-2.
Preferably, the adding amount of the alumina sol in the step (2) is less than or equal to 20 percent of the content of the alumina sol in the yttrium oxide powder based on the calcined alumina.
Preferably, the adding amount of the aluminum sol is less than or equal to 10 percent of the content of the aluminum sol in the yttrium oxide powder, calculated by calcined aluminum oxide.
Compared with the prior art, the invention has the following beneficial effects:
the process for preparing the plasma spraying yttrium oxide coating powder has the advantages that the use of yttrium oxide raw materials is not limited any more, all yttrium oxides with the purity of more than 99.9 percent can be used, and even the yttrium oxide melted by an electric melting furnace or an induction furnace can be used, so the manufacturing cost is greatly reduced. The introduction of the alumina sol forms part of the nano-sized alumina during the post-sintering process and also partially synthesizes the Y generated in situ from the alumina and yttria x Al y O z Phase of Y x Al y O z The phase can play a role in dispersing, toughening and strengthening a phase interface, the interface bonding between coating layers is good, and particularly when the coating is sprayed on an aluminum alloy base material, the toughness and the thermal shock resistance of the coating can be improved. And the nanometer alumina after the alumina sol is calcined can greatly reduce the sintering temperature of the large-size primary crystal yttrium oxide, and compared with the plasma spheroidizing process, the preparation cost is reduced, the erosion resistance of the large-size primary crystal yttrium oxide powder can be kept, and the problem of reduced erosion caused by the adoption of the high-cost nanometer yttrium oxide as the raw material is solved. In addition, the aluminum oxide spraying powder can be used as a spraying material for etching semiconductors, so that the final using effect of the powder is not influenced.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of plasma spraying yttrium oxide coating powder comprises the following steps:
(1) Adding 28 kg of pure water into 3.47 kg of pseudo-boehmite, heating to 82 ℃ while stirring, slowly dripping 2 kg of concentrated nitric acid, and aging in a 82 ℃ water bath kettle for 5 hours to obtain 33.47 kg of alumina sol;
(2) Weighing 100 kg of high-purity yttrium oxide powder with the purity of 99.999% and the particle size D50=1.2 microns, adding 20 kg of pure water, stirring and dispersing, adding 33.47 kg of the alumina sol prepared in the step (1), simultaneously adding 1.5 kg of a binder, 450 g of a dispersing agent and 15 g of a defoaming agent, stirring for 2 hours in a stirring barrel, and wrapping to form slurry; the binder is polyvinyl alcohol, the dispersant is sodium polyacrylate or sodium tripolyphosphate, and the defoaming agent is n-octanol;
(3) Granulating and drying on a spray granulator to obtain granulated powder;
(4) The granulated powder was calcined at 1600 ℃ for 4 hours to give a particle size D50=28 μm, a flow rate of 48 seconds, and a bulk density of 1.26g/cm 3 The yttrium oxide powder of (1).
The powder was subjected to plasma spray tests on die steel and aluminum alloy substrates, respectively, with data as in table 1:
TABLE 1
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of plasma spraying yttrium oxide coating powder is characterized by comprising the following steps:
(1) Selecting boehmite, adding pure water for dilution, heating to 80-84 ℃, adding concentrated nitric acid while stirring, and aging at 80-84 ℃ for 5 hours to obtain alumina sol;
(2) Mixing high-purity yttrium oxide powder with pure water, stirring and dispersing, adding the alumina sol prepared in the step (1), adding a binder, a dispersing agent and a defoaming agent, stirring and wrapping to form slurry;
(3) Granulating and drying the slurry obtained in the step (2) by adopting a spray granulation process to obtain granulated powder;
(4) Calcining the granulated powder at 1400-1700 ℃, cooling, and screening and classifying.
2. The plasma spray yttria coating powder of claim 1, wherein the mass ratio of the boehmite to the pure water in step (1) is 3-4: 1, wherein the concentration of the concentrated nitric acid is more than 65 percent.
3. The plasma spray yttria coating powder of claim 1, wherein the high purity yttria powder of step (2) is micron grade high purity yttria powder, the purity is more than 99.9%, and the particle size D50 is less than 6 microns.
4. The plasma spray yttria coating powder of claim 3, wherein the micron-sized high-purity yttria powder is at least one of common yttria powder, electrofused yttria powder or yttria powder melted by an induction furnace.
5. The plasma spray yttria coating powder of claim 1, wherein the mass ratio of the high purity yttria powder of step (2) to pure water is 5-6:1-2.
6. The plasma spray yttria coating powder of claim 1, wherein the amount of alumina sol added in step (2) is less than or equal to 20% in the yttria powder based on the calcined alumina.
7. The plasma sprayed yttria coating powder of claim 6, wherein the alumina sol is added in an amount of less than or equal to 10% of the yttria powder based on the calcined alumina.
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| CN202211071316.0A CN115448720A (en) | 2022-09-01 | 2022-09-01 | Preparation method of plasma spraying yttrium oxide coating powder |
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| CN202211071316.0A Pending CN115448720A (en) | 2022-09-01 | 2022-09-01 | Preparation method of plasma spraying yttrium oxide coating powder |
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Cited By (3)
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| CN115849906A (en) * | 2022-12-28 | 2023-03-28 | 常州市卓群纳米新材料有限公司 | Preparation method of spherical yttrium-based composite ceramic for thermal spraying |
| CN116573662A (en) * | 2023-04-22 | 2023-08-11 | 苏州高芯众科半导体有限公司 | Preparation method for producing yttrium oxide spraying powder by hydrothermal method |
| CN118702490A (en) * | 2024-08-30 | 2024-09-27 | 山东拓普新材料科技有限公司 | Yttria granulated powder for plasma corrosion resistant thermal spraying and its preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115849906A (en) * | 2022-12-28 | 2023-03-28 | 常州市卓群纳米新材料有限公司 | Preparation method of spherical yttrium-based composite ceramic for thermal spraying |
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| CN116573662A (en) * | 2023-04-22 | 2023-08-11 | 苏州高芯众科半导体有限公司 | Preparation method for producing yttrium oxide spraying powder by hydrothermal method |
| CN118702490A (en) * | 2024-08-30 | 2024-09-27 | 山东拓普新材料科技有限公司 | Yttria granulated powder for plasma corrosion resistant thermal spraying and its preparation method and application |
| CN118702490B (en) * | 2024-08-30 | 2024-11-15 | 山东拓普新材料科技有限公司 | Yttria granulated powder for plasma corrosion resistant thermal spraying and its preparation method and application |
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