CN116102050B - Preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder - Google Patents
Preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder Download PDFInfo
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- CN116102050B CN116102050B CN202211215183.XA CN202211215183A CN116102050B CN 116102050 B CN116102050 B CN 116102050B CN 202211215183 A CN202211215183 A CN 202211215183A CN 116102050 B CN116102050 B CN 116102050B
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000005260 corrosion Methods 0.000 title claims abstract description 24
- 230000007797 corrosion Effects 0.000 title claims abstract description 24
- 238000007751 thermal spraying Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000007670 refining Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010891 electric arc Methods 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 8
- 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 8
- 230000008569 process Effects 0.000 claims description 7
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 102220043159 rs587780996 Human genes 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 238000005507 spraying Methods 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 4
- 210000002381 plasma Anatomy 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 239000012798 spherical particle Substances 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000005524 ceramic coating Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 239000011224 oxide ceramic Substances 0.000 description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- 229910020323 ClF3 Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005459 micromachining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The invention provides a preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder, which belongs to the technical field of thermal spraying ceramic powder materials, and comprises the following steps: and (3) carrying out calcination heat treatment on the yttrium oxide raw material, placing the yttrium oxide raw material into an electric arc furnace for batch melting refining before the calcination heat treatment, naturally cooling after the melting refining treatment is finished, crushing, selecting out melted and coagulated pure yttrium oxide crystals, crushing, adding water for modulation, adding an auxiliary agent, granulating and drying, carrying out calcination heat treatment, cooling, and carrying out particle size classification to obtain the plasma corrosion resistant thermal spraying yttrium oxide. The thermal spraying yttrium oxide powder prepared by the invention has high compactness of the coating after spraying, strong corrosion resistance and excellent corrosion resistance.
Description
Technical Field
The invention relates to the technical field of thermal spraying ceramic powder materials, in particular to a preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder.
Background
In the plasma process of semiconductor manufacturing, yttria spray powder is generally used for etching and cleaning because of high reactivity of fluorine-based and chlorine-based etching gases by performing micromachining of equipment using dry plasma etching. For example, a typical corrosive halogen gas component is a fluorine-based gas: SF 6、CF4、CHF3、ClF3, HF, and the like, chlorine-based gases: cl 2、BCl3 and HCl, and these halogen gases are plasmatized after microwave and high frequency are introduced into the atmosphere of these gases. All of the device components exposed to the halogen plasma need to be highly corrosion resistant. The plasma power is small and the temperature is low, so the aluminum oxide coating is selected by people, but as the wafer size is continuously increased, the power of plasma equipment is continuously increased, the traditional aluminum oxide ceramic coating can not meet the requirements, and the yttrium oxide coating has the advantages of high melting point, phase stability, low thermal expansion, better plasma corrosion resistance, longer service life and the like compared with the aluminum oxide ceramic coating, gradually replaces the aluminum oxide ceramic coating material, and is widely applied to the coating protection of semiconductor and TFT Liquid Crystal Display (LCD) production equipment. For example, on 800W power equipment, the yttria coating has a service period that is more than four times that of the alumina coating.
At present, research and report on yttrium oxide thermal spraying powder at home and abroad are that most of yttrium oxide thermal spraying powder is prepared by directly adopting electric melting broken yttrium oxide powder for spraying, or adopting nano yttrium oxide powder with high cost firstly, and then spraying granulation agglomeration is carried out to generate large-particle powder suitable for spraying. Mechanically crushing the powder does not give spherical particles, and the appearance of the particles is often irregular and irregularly shaped. The process for preparing the nano powder is long in process and high in cost, densification cannot be completely realized only by high-temperature calcination, and if plasma spheroidization is added, the investment of equipment is increased undoubtedly, and the production cost is increased.
Disclosure of Invention
In view of the above, the invention provides a preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder, and the preparation method provided by the invention has the advantages that the particle size distribution of materials is concentrated, the materials are easier to melt, the compactness of a coating after spraying is high, the corrosion resistance is strong, the coating has more excellent fluidity compared with common yttrium oxide crushed powder, and a protective coating with excellent corrosion resistance to halogenated gases such as fluorine groups and chlorine groups or plasmas thereof can be formed after the spraying powder provided by the invention is used.
The preparation method of the plasma corrosion resistant thermal spraying yttrium oxide powder provided by the invention comprises the following steps: the method comprises the steps of placing the yttrium oxide raw material into an electric arc furnace for batch melting and refining before the yttrium oxide raw material is subjected to calcination heat treatment, naturally cooling the furnace along with the end of the melting and refining treatment, crushing, selecting fused and condensed pure yttrium oxide crystals, crushing, adding water for modulation, adding an auxiliary agent, granulating and drying, performing calcination heat treatment, cooling, and performing particle size classification to obtain the plasma corrosion resistant thermal spraying yttrium oxide powder.
Preferably, the preparation method of the plasma corrosion resistant thermal spraying yttrium oxide powder comprises the following steps:
(1) The high-purity yttrium oxide is taken as a raw material to be fed into an electric arc furnace in batches for melting and refining, and then the temperature is reduced in a mode of naturally cooling along with the furnace, so as to obtain a cooled melt;
(2) Crushing the cooled melt, and selecting pure yttrium oxide crystal parts which are thoroughly fused and condensed in the melt, so as to eliminate unmelted materials;
(3) Crushing pure yttrium oxide crystals, adding deionized water to prepare slurry, adding a binder, a dispersing agent and a defoaming agent into the slurry, and granulating and drying the slurry by adopting a spray granulator to obtain spherical particles;
(4) Finally, carrying out calcination heat treatment on the spherical particles, cooling, and carrying out particle size classification to obtain the plasma corrosion resistant thermal spraying yttrium oxide powder.
Preferably, the yttria feedstock has a purity of > 99.99%.
Preferably, the electric arc furnace may also be a high frequency furnace or other smelting equipment, more preferably a three phase ac electric arc furnace.
Preferably, the melting temperature is 2200-2600 ℃, and the refining temperature is 2400-2600 ℃.
Preferably, the voltage of the melting refining is 110-180V, and the current is 4000-8000 KA.
Preferably, the particle size after comminution is controlled between d50=0.4 and 1.2 microns.
Preferably, the solid content of the slurry obtained after the water is added for modulation is more than or equal to 65 percent.
Preferably, the auxiliary agent comprises a binder polyvinyl alcohol, a dispersant sodium polyacrylate or sodium tripolyphosphate and an antifoaming agent n-octanol.
Preferably, the temperature of the calcination heat treatment is 1600 to 1800 ℃, and more preferably, the temperature of the calcination heat treatment is 1650 to 1750 ℃.
Preferably, in the granulating process, the temperature of an air inlet of the granulator is controlled to be 180-280 ℃, and the temperature of an air outlet of the granulator is controlled to be 100-180 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. In the plasma spraying process, although the plasma arc light temperature is very high, all sprayed powder cannot be guaranteed to fall in a high-temperature arc light area to be completely melted during spraying, a part of powder in a low-temperature area at the periphery of the arc light can be adhered to the surface of a coating, the corrosion resistance and compactness of the coating can be reduced only by the powder subjected to the calcination process, and the problem can be effectively solved by the powder melted in advance, and the cost is far lower than that of the plasma spheroidizing process in the later stage of powder preparation.
2. Compared with irregular powder which is directly crushed, spherical particles manufactured by adopting spray granulation after melting have obviously better fluidity than the crushed irregular particles under the same particle size, and particularly, the spherical particles are more obviously expressed in fine particle powder required by compact yttrium oxide coating.
Drawings
FIG. 1 is an electron micrograph of a plasma etch resistant thermal spray yttria powder prepared in accordance with an embodiment of the present invention;
FIG. 2 is an electron micrograph of a commercially available yttria spherical powder (Japanese) provided in comparative example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the invention, are within the scope of the invention.
The test methods or test methods described in the following examples are all conventional methods unless otherwise specified; the starting materials and auxiliaries, unless otherwise specified, are obtained commercially from conventional sources or are prepared in conventional manner.
Examples
A preparation method of plasma corrosion resistant thermal spraying yttrium oxide powder comprises the following specific steps:
(1) Adding 5000KG yttrium oxide with purity more than 99.999% as a raw material into a three-phase alternating current arc furnace in batches, setting smelting voltage to 128V, and operating current to 6500KA for smelting and refining, wherein the smelting temperature is 2410 ℃, smelting for 45min after adding yttrium oxide each time until the raw material is fully melted, refining for 30min under the temperature condition of 2410 ℃, and then cooling by adopting a natural furnace-following cooling mode to obtain a cooled melt;
(2) Crushing the cooled melt to granules below 10cm, sorting out pure yttrium oxide crystal parts which are thoroughly fused and coagulated in the melt, eliminating incompletely fused materials, and cleaning the sorted crystals with deionized water for 2 times;
(3) Coarse crushing by a crusher with a ceramic lining plate, crushing by a jet mill with a ceramic lining embedded therein, crushing yttrium oxide crystals into ultrafine powder with the granularity D50=0.8 microns, adding deionized water into the ultrafine powder to prepare slurry with the solid content of 72%, adding polyvinyl alcohol, sodium tripolyphosphate and n-octanol into the slurry, granulating and drying the slurry by a spray granulator, wherein the temperature of an air inlet of the granulator is controlled at 250 ℃, and the temperature of an air outlet of the granulator is controlled at 150 ℃, so as to obtain spherical particles;
(4) Finally, the spherical particles are subjected to calcination heat treatment at the temperature of 1750 ℃, and are subjected to screening particle size classification after being cooled, wherein the screening particle size is controlled between 22 and 63 mu m, so that the plasma corrosion resistant thermal spraying yttrium oxide powder is obtained, and an electron microscope photograph of the yttrium oxide powder is shown in figure 1.
Comparative example 1
A commercially available yttrium oxide spherical powder having a particle size of 22-63um (Japanese FUJIMI Co., ltd., product model Ra 30).
Comparative example 2
Commercially available crushed powder (model DY, zhengzhou Zhenzhong electric smelting new materials Co., ltd.) with particle size of 22-63 um.
Performance measurements were performed on the yttria powders provided in examples, comparative example 1, and comparative example 2, and the results are shown in table 1:
TABLE 1
| Specification of specification | Examples | Comparative example 1 | Comparative example 2 |
| Yttria content (%) | 99.96 | 99.98 | 99.02 |
| Median diameter D50 (μm) | 27.17 | 26.28 | 32 |
| Bulk Density (g/cm 3) | 1.429 | 1.496 | 1.45 |
| Flow Rate (s/50 g) | 88 | 86 | No flow rate |
Comparing the performance of the yttrium oxide powder provided by the example and the comparative example 1, the invention is verified that the spray powder prepared by melting the common yttrium oxide powder with the common purity of more than 99.999 percent has no obvious difference in the subsequent corrosion resistance comparison test compared with the powder prepared by directly granulating and plasma spheroidizing the nano powder in the comparative example 1, and the manufacturing cost of the yttrium oxide spray powder is greatly reduced, and the detailed comparison result is shown in table 2:
TABLE 2
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. The preparation method of the plasma corrosion resistant thermal spraying yttrium oxide powder comprises the steps of carrying out calcination heat treatment on yttrium oxide raw materials, and is characterized in that before the calcination heat treatment is carried out on the yttrium oxide raw materials, firstly, placing the yttrium oxide raw materials in an electric arc furnace for batch melting and refining, naturally cooling after the melting and refining treatment is finished, then crushing, sorting out pure yttrium oxide crystals which are melted and coagulated, crushing, adding water for modulation, adding an auxiliary agent, granulating and drying, carrying out calcination heat treatment, and carrying out particle size classification after cooling, thus obtaining the plasma corrosion resistant thermal spraying yttrium oxide powder;
The melting temperature is 2200-2600 ℃, and the refining temperature is 2400-2600 ℃;
the voltage of the melting refining is 110-180V, and the current is 4000-8000 KA;
The particle size after crushing is controlled between D50=0.4 and 1.2 microns;
the solid content of the slurry obtained after the water is added for modulation is more than or equal to 65 percent;
The auxiliary agent comprises a binder, a dispersing agent and a defoaming agent;
in the granulating process, the temperature of an air inlet of the granulator is controlled at 180-280 ℃, and the temperature of an air outlet of the granulator is controlled at 100-180 ℃;
the temperature of the calcination heat treatment is 1600-1800 ℃.
2. The method for preparing the plasma corrosion resistant thermal spraying yttrium oxide powder according to claim 1, wherein the purity of the yttrium oxide raw material is more than 99.99%.
3. The method of producing a plasma corrosion resistant thermal sprayed yttria powder of claim 1, wherein the electric arc furnace is a high frequency furnace.
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|---|---|---|---|---|
| JPH04130055A (en) * | 1990-09-21 | 1992-05-01 | Santoku Kinzoku Kogyo Kk | Molded body of fused yttrium oxide |
| KR102348171B1 (en) * | 2021-08-12 | 2022-01-06 | 최진식 | Manufacturing method of yttrium oxide powder for plasma spray |
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| JP4209277B2 (en) * | 2003-07-24 | 2009-01-14 | コバレントマテリアル株式会社 | Method for producing plasma corrosion resistant thermal spray member |
| CN101182207B (en) * | 2007-11-16 | 2010-06-16 | 北京矿冶研究总院 | Spraying powder containing yttrium oxide and preparation method thereof |
| CN100595157C (en) * | 2008-04-24 | 2010-03-24 | 淄博市周村磊宝耐火材料有限公司 | Method for producing high-purity electro-melting yttrium oxide sand |
| KR101338090B1 (en) * | 2012-07-27 | 2014-01-20 | 경상대학교산학협력단 | Full density yttria ceramic sintered by using for conventional sintering method with fused yttria as starting materials |
| CN108408754B (en) * | 2018-02-05 | 2019-11-12 | 常州市卓群纳米新材料有限公司 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
| CN108623315A (en) * | 2018-05-03 | 2018-10-09 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of titanium alloy smelting oxidation yttrium powder |
| CN109355612A (en) * | 2018-11-29 | 2019-02-19 | 沈阳富创精密设备有限公司 | A method of yttria coating is prepared with air plasma spraying |
| CN109928754B (en) * | 2019-04-22 | 2021-07-06 | 郑州振中电熔新材料有限公司 | Method for preparing modified yttrium oxide |
| CN113666408A (en) * | 2021-09-08 | 2021-11-19 | 常州市卓群纳米新材料有限公司 | Preparation method of low-porosity plasma-corrosion-resistant yttrium oxide composite ceramic coating powder |
| CN114672756B (en) * | 2022-04-02 | 2023-11-17 | 华东理工大学 | High-entropy superhigh-temperature zirconia-based thermal barrier coating material, preparation method and application thereof, and zirconia-based thermal barrier coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH04130055A (en) * | 1990-09-21 | 1992-05-01 | Santoku Kinzoku Kogyo Kk | Molded body of fused yttrium oxide |
| KR102348171B1 (en) * | 2021-08-12 | 2022-01-06 | 최진식 | Manufacturing method of yttrium oxide powder for plasma spray |
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