CN116425192B - Powder material special for PS-PVD, preparation method and application - Google Patents
Powder material special for PS-PVD, preparation method and application Download PDFInfo
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- CN116425192B CN116425192B CN202310068141.6A CN202310068141A CN116425192B CN 116425192 B CN116425192 B CN 116425192B CN 202310068141 A CN202310068141 A CN 202310068141A CN 116425192 B CN116425192 B CN 116425192B
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- 239000000843 powder Substances 0.000 title claims abstract description 119
- 239000000463 material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000011248 coating agent Substances 0.000 claims abstract description 32
- 238000000576 coating method Methods 0.000 claims abstract description 32
- 230000008569 process Effects 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 105
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 62
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 238000005507 spraying Methods 0.000 claims description 35
- 239000012074 organic phase Substances 0.000 claims description 31
- 239000007795 chemical reaction product Substances 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 25
- 238000006467 substitution reaction Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 23
- 239000002243 precursor Substances 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000006722 reduction reaction Methods 0.000 claims description 22
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000012071 phase Substances 0.000 claims description 20
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 20
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 238000007363 ring formation reaction Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- 150000001540 azides Chemical class 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- FZASHPCRPMSFEG-UHFFFAOYSA-N 3-(dimethylamino)-2-methylpropan-1-ol Chemical compound OCC(C)CN(C)C FZASHPCRPMSFEG-UHFFFAOYSA-N 0.000 claims description 6
- XLYOGWXIKVUXCL-UHFFFAOYSA-N 4-bromobut-1-yne Chemical compound BrCCC#C XLYOGWXIKVUXCL-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- LMLSBPHXMGSGCR-UHFFFAOYSA-N methyl 2-(3,5-dihydroxyphenyl)acetate Chemical compound COC(=O)CC1=CC(O)=CC(O)=C1 LMLSBPHXMGSGCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 5
- -1 lithium aluminum hydride Chemical compound 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 4
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 claims description 4
- 239000012280 lithium aluminium hydride Substances 0.000 claims description 4
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims description 4
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000012312 sodium hydride Substances 0.000 claims description 4
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 4
- RVRKDGLTBFWQHH-UHFFFAOYSA-N yttrium zirconium Chemical compound [Y][Zr][Y] RVRKDGLTBFWQHH-UHFFFAOYSA-N 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000011343 solid material Substances 0.000 claims 2
- 238000012360 testing method Methods 0.000 abstract description 34
- 230000035939 shock Effects 0.000 abstract description 16
- 230000003068 static effect Effects 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 238000001816 cooling Methods 0.000 abstract description 8
- 230000005611 electricity Effects 0.000 abstract description 8
- 230000002776 aggregation Effects 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000000903 blocking effect Effects 0.000 abstract description 6
- 238000005336 cracking Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000010791 quenching Methods 0.000 abstract description 5
- 230000000171 quenching effect Effects 0.000 abstract description 5
- 239000011258 core-shell material Substances 0.000 abstract description 3
- 238000007747 plating Methods 0.000 abstract description 2
- 238000007259 addition reaction Methods 0.000 description 20
- 239000012720 thermal barrier coating Substances 0.000 description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000008346 aqueous phase Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- 239000010935 stainless steel Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000005240 physical vapour deposition Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 125000000304 alkynyl group Chemical group 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- IVRMZWNICZWHMI-UHFFFAOYSA-N azide group Chemical group [N-]=[N+]=[N-] IVRMZWNICZWHMI-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 125000000623 heterocyclic group Chemical group 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 150000001768 cations Chemical group 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005328 electron beam physical vapour deposition Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- INIGCWGJTZDVRY-UHFFFAOYSA-N hafnium zirconium Chemical compound [Zr].[Hf] INIGCWGJTZDVRY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- ONLCZUHLGCEKRZ-UHFFFAOYSA-N cerium(3+) lanthanum(3+) oxygen(2-) Chemical compound [O--].[O--].[O--].[La+3].[Ce+3] ONLCZUHLGCEKRZ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- 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
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a special powder material for PS-PVD, a preparation method and application thereof, and belongs to the technical field of plating materials. The invention removes powder agglomeration caused by static electricity, the particle size range of the prepared PS-PVD special powder material is 1-30 mu m, the material has a core-shell structure and good fluidity, and the purity of T' phase is more than or equal to 99.9 percent after the material is preserved for 200h at 1200 ℃ and is superior to Metco6700 adopted in the prior art TM . The powder can be used in a PS-PVD process, and can be prevented from blocking during 1h when the powder feeding amount is 20g/min, and in addition, the powder can be fully gasified to form a typical PS-PVD columnar crystal coating. The obtained coating has good combination property with a matrix, and reaches a complete oxidation resistance level in static oxidation resistance. Meanwhile, the coating also has excellent heat and corrosion resistance, and does not have the phenomena of wrinkling, cracking, skin lifting, falling off and the like. The coating can not bubble, peel and layer in the water quenching thermal shock and air cooling thermal shock test.
Description
Technical Field
The invention relates to the technical field of plating materials, in particular to a special powder material for PS-PVD, a preparation method and application.
Background
Plasma spraying-physical vapor deposition (PS-PVD) is a high-performance thermal barrier coating high-efficiency preparation technology which is emerging in recent years, and a coating with columnar crystals and a compact structure can be co-deposited through gas phase, liquid phase and solid phase, so that the thermal barrier coating has good heat insulation performance and thermal shock resistance, is applied to thermal barrier coatings for hot end parts at present, and gradually has a trend of replacing the Atmospheric Plasma Spraying (APS) and electron beam-physical vapor deposition (EB-PVD) technologies in the application of high-performance key parts.
Chinese patent CN108103431a provides a thermal barrier coating powder for plasma physical vapor deposition and a preparation method thereof, the powder has a dual-phase structure and high aperture ratio, the powder is obtained by agglomerating and granulating nano-sized powder a and micro-sized powder B, and the mass ratio of powder B to powder a is 1:1 to 3:1, whereinAfter ball milling and dispersing the powder A, adding the powder B, carrying out agglomeration and granulation by using a centrifugal spray drying or two-fluid spray drying mode, and finally drying, screening and checking the powder to obtain the spray powder. The apparent density of the spray powder is 1.0-1.3 g/cm 3 The tap density is 1.1-1.5 g/cm 3 The granularity range is 5-25 mu m, and the powder has a high-aperture ratio structure with coarse and fine particles. The invention can stably convey in the PS-PVD process, and meanwhile, due to high aperture ratio, the powder is at the outlet position of the spray gun, and the binder volatilization and agglomeration powder dispersion are rapidly realized, so that small particle powder can obtain good acceleration, melting and gasification effects at the center position of plasma, and the preparation of a high-performance PS-PVD coating is ensured.
Chinese patent CN108546907a discloses a yttria-stabilized zirconia doped lanthanum ceric acid material powder for plasma physical vapor deposition, and a preparation method and application thereof, and the invention comprises the steps of: 1:0.08:1, carrying out ball milling treatment on the mixture in a molar ratio to obtain a ball milling product, filtering and drying the product, carrying out ball milling and mixing uniformly with deionized water, a binder and a dispersing agent after drying to obtain slurry, and carrying out spray drying treatment on the slurry to obtain granules; and sintering the granules, and then screening to obtain the yttrium oxide stabilized zirconium oxide doped lanthanum cerium oxide material powder for plasma physical vapor deposition. When the coating is prepared, heating powder in a powder feeder, starting plasma physical vapor deposition equipment, vacuumizing to a pressure lower than 0.08mbar, and filling argon into a vacuum chamber to 130mbar; and then spraying to obtain the coating. The method has simple steps, saves cost, improves the material performance, and can be used for mass industrial production.
Furthermore, APS spray powders are generally not suitable for PS-PVD processes due to the process specificity. In commercial production or research, the current thermal barrier coating powder is mainly manufactured by Metco6700 TM 、Metco206A TM The powder is mainly. The powder provided by the prior art has the technical defect of poor fluidity, has the phenomenon of powder blockage in the continuous powder feeding process of PS-PVD treatment, and is difficult to meet the process requirements of PS-PVD.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a powder material special for PS-PVD, a preparation method and application thereof.
The PS-PVD process has high deposition efficiency and good heat insulation effect, but the process has high requirement on powder flowability. In the production process, the PS-PVD equipment powder feeder needs to keep the powder feeding fluidity for a long time, and the high-frequency powder blocking phenomenon cannot occur. The fluidity of PS-PVD powder is closely related to the aggregation caused by static electricity, and the powder particles are tiny, so that static electricity is easy to generate and aggregate, and the powder feeding process is blocked.
The invention removes powder agglomeration caused by static electricity, the particle size range of the prepared PS-PVD special powder material is 1-30 mu m, the material has a core-shell structure and good fluidity, and the purity of T' phase is more than or equal to 99.9 percent after the material is preserved for 200h at 1200 ℃ and is superior to Metco6700 adopted in the prior art TM . The powder can be gasified fully to form a typical PS-PVD columnar crystal coating in the PS-PVD process. The obtained coating has good combination property with a matrix, and reaches a complete oxidation resistance level in static oxidation resistance. Meanwhile, the coating also has excellent heat and corrosion resistance, and does not have the phenomena of wrinkling, cracking, skin lifting, falling off and the like. The coating can not bubble, peel and layer in the water quenching thermal shock and air cooling thermal shock test.
A preparation method of a special powder material for PS-PVD comprises the following steps:
s1, preparing zirconium oxychloride and yttrium carbonate according to the proportion of 4mol% of yttria-stabilized zirconia, uniformly mixing the zirconium oxychloride, the yttrium carbonate and a surfactant, and reacting under a heating condition to obtain a precursor for later use;
s2, transferring the precursor into a vacuum environment, and achieving and maintaining a stable state of gas-liquid saturation under heating and stirring conditions to obtain a mixture for later use;
s3, carrying out microwave treatment on the mixture to obtain an amorphous solid matter with yttrium zirconium uniformly mixed, removing residual organic matters from the amorphous solid matter, and then adding an antistatic treatment agent to obtain the PS-PVD special powder material.
Preferably, the heating temperature in step S1 is 60 to 120 ℃.
Preferably, the heating temperature in step S2 is 60 to 120 ℃, and the maintenance time of the gas-liquid saturated steady state is 1 to 2 hours.
Preferably, the working temperature of the microwave treatment in the step S3 is 80-200 ℃ and the treatment time is 3-5 min.
Preferably, the method for removing residual organic matters in the step S3 is calcining for 12-24 hours at 1000-1200 ℃.
Preferably, the antistatic agent in the step S3 is added in an amount of 0.1 to 0.5wt% of the total mass of zirconium oxychloride, yttrium carbonate and absolute ethyl alcohol.
The invention provides an antistatic treatment agent and a preparation method thereof. In the preparation method, 3- (dimethylamino) -2-methyl-1-propanol and 3, 5-dihydroxyphenylacetic acid methyl ester are subjected to addition reaction and combined, the obtained addition product is reduced under catalysis, and then substitution reaction is carried out with 4-bromo-n-butyne and terminal alkynyl is introduced; finally, the substitution product after methylation is combined with the eight-arm polyethylene glycol azide through cyclization reaction, and the substitution product and the azide group form a heterocycle through terminal alkynyl to be connected, so that the antistatic treatment agent is obtained.
The eight-arm polyethylene glycol azide has an azide group at each end of the eight arms attached to a hexaglycerol core, forming a hydrophobic heterocycle by reaction with terminal alkynyl groups and introducing two cationic groups at each branch, the steric hindrance provided by the biscationic groups being capable of preventing the reaction of the active groups with the methylene groups, thereby enhancing its stability. In addition, the antistatic treatment agent has multi-branch and multi-cation groups and high local ion concentration, and flexible ether bonds and alkyl spacers in the side chains can increase the mobility of the cation groups, so that the transfer capacity of charges is improved, and the high-efficiency removal of static electricity is realized. The elements of the antistatic treatment agent are mainly carbon, oxygen, hydrogen and nitrogen, and in the PS-PVD spraying process, the antistatic treatment agent is excited to decompose to form gaseous micromolecules without participating in the process of forming thermal barrier powder by powder, so that the coating structure is not influenced.
Preferably, the antistatic treatment agent is prepared by the following steps:
m1, under the anaerobic condition, uniformly mixing 3- (dimethylamino) -2-methyl-1-propanol, 3, 5-dihydroxyphenylacetic acid methyl ester and tetrahydrofuran, adding a catalyst, and carrying out addition reaction; after the addition reaction is finished, tetrahydrofuran is removed by reduced pressure distillation, residues are mixed with diethyl ether, filtrate is collected by filtration, diethyl ether is removed by reduced pressure distillation, residues are mixed with dichloromethane, hydrochloric acid is added, water phase is separated, pH of the water phase is adjusted to be alkaline, and then dichloromethane is used for extraction and organic phase is collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain an addition reaction product for later use;
m2, mixing the addition reaction product with tetrahydrofuran uniformly, adding a reducing agent, and carrying out reduction reaction; after the reduction reaction is finished, hydrochloric acid is added to stop the reaction, the water phase is collected and the pH of the water phase is adjusted to be neutral, and then dichloromethane is used for extraction and organic phase is collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reduction reaction product for later use;
m3, taking the reduction reaction product, the catalyst and tetrahydrofuran to be uniformly mixed, adding 4-bromo-n-butyne and carrying out substitution reaction; after the substitution reaction is finished, adding saturated ammonium chloride aqueous solution to stop the reaction, extracting with dichloromethane, collecting an organic phase, drying the organic phase, and distilling under reduced pressure to remove the dichloromethane to obtain a substitution reaction product for later use;
m4, taking the substitution reaction product, uniformly mixing methyl iodide and 15-25 parts of acetonitrile, and reacting; pouring the product into excessive diethyl ether after the reaction is finished, filtering, collecting precipitate, washing the precipitate with diethyl ether, and drying to obtain a reaction precursor for later use;
m5, under the anaerobic condition, uniformly mixing the reaction precursor, the eight-arm polyethylene glycol azide and the N-methylpyrrolidone, and adding a catalyst for cyclization reaction; and after the cyclization reaction is finished, pouring the product into excessive isopropanol, filtering, collecting the precipitate, washing the precipitate by deionized water, and drying to obtain the antistatic treatment agent.
Specifically, the preparation method of the antistatic treatment agent comprises the following steps of:
under the protection of M1 and nitrogen, 1.90-2.45 parts of 3- (dimethylamino) -2-methyl-1-propanol, 1.30-1.70 parts of 3, 5-dihydroxyphenylacetic acid methyl ester and 30-40 parts of tetrahydrofuran are uniformly mixed, and then 4.20-5.50 parts of triphenylphosphine and 3.25-4.25 parts of diisopropyl azodicarboxylate are added for addition reaction; after the addition reaction is finished, removing tetrahydrofuran by reduced pressure distillation, mixing residues with 30-50 parts of diethyl ether, filtering and collecting filtrate, then removing diethyl ether by reduced pressure distillation, mixing residues with 25-40 parts of dichloromethane, adding 50-100 parts of hydrochloric acid, separating a water phase, adjusting the pH of the water phase to 10.0-11.5, extracting with dichloromethane, and collecting an organic phase; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain an addition reaction product for later use;
m2, taking 2.15-2.85 parts of the addition reaction product and 40-50 parts of tetrahydrofuran, uniformly mixing, adding 0.50-0.65 part of lithium aluminum hydride and carrying out reduction reaction; after the reduction reaction is finished, 45-60 parts of hydrochloric acid is added to stop the reaction, the water phase is collected, the pH value of the water phase is adjusted to be neutral, and then dichloromethane is used for extraction and an organic phase is collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reduction reaction product for later use;
m3, taking 1.60-2.10 parts of the reduction reaction product, 0.30-0.45 part of sodium hydride and 15-20 parts of tetrahydrofuran, uniformly mixing, adding 0.65-0.85 part of 4-bromo-n-butyne, and carrying out substitution reaction; after the substitution reaction is finished, adding 20-30 parts of saturated ammonium chloride aqueous solution to stop the reaction, then extracting with dichloromethane, collecting an organic phase, drying the organic phase, and distilling under reduced pressure to remove the dichloromethane to obtain a substitution reaction product for later use;
m4, taking 2.10 to 2.70 parts of the substitution reaction product, 5.50 to 7.15 parts of methyl iodide and 15 to 25 parts of acetonitrile to be uniformly mixed and reacted; pouring the product into excessive diethyl ether at 0-4 ℃ after the reaction is finished, filtering, collecting precipitate, washing the precipitate with diethyl ether, and drying to obtain a reaction precursor for later use;
under the protection of M5 and nitrogen, 2.45 to 3.20 parts of reaction precursor, 0.85 to 1.10 parts of eight-arm polyethylene glycol azide and 40 to 60 parts of N-methylpyrrolidone are taken and uniformly mixed, and 0.35 to 0.50 part of pentamethyl diethylenetriamine and 0.15 to 0.20 part of copper bromide are added for cyclization reaction; after the cyclization reaction is finished, pouring the product into excessive isopropanol at the temperature of 0-4 ℃, filtering, collecting the precipitate, washing the precipitate by deionized water, and drying to obtain the antistatic treatment agent.
Preferably, the addition reaction in step M1 is carried out in two stages, first at 0 to 4℃for 2 to 5 hours and then at 65 to 80℃for 12 to 18 hours with reflux.
Preferably, the temperature of the reduction reaction in the step M2 is 25-40 ℃ and the reaction time is 12-18 h.
Preferably, the temperature of the substitution reaction in the step M3 is 25-35 ℃ and the reaction time is 9-15 h.
Preferably, the temperature of the reaction in the step M4 is 20-30 ℃ and the reaction time is 18-36 h.
Preferably, the temperature of the cyclization reaction in the step M5 is 50-65 ℃ and the reaction time is 12-36 h.
Preferably, the concentration of the hydrochloric acid is 1.0-1.5 mol/L independently.
Preferably, the average molecular weight of the eight-arm polyethylene glycol azide is 1000-5000.
The invention provides application of the special powder material for PS-PVD in a PS-PVD process, which comprises the following steps:
taking a PS-PVD special powder material as a spraying raw material, and adopting PS-PVD spraying equipment to prepare a coating on a base material; in the PS-PVD spraying process, the argon flow is 30-40L/min, the helium flow is 50-70L/min, the current is 2400-2600A, the spraying distance is 800-1000 mm, and the powder feeding amount of the powder feeder is 5-35 g/min.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the invention.
The invention has the following description and functions of partial raw materials in the formula:
zirconium oxychloride: a chemical substance with molecular formula of ZrOCl 2 ·8H 2 O isThe white needle-like crystal, zirconium oxychloride is the main raw material for producing other zirconium products such as zirconium dioxide, zirconium carbonate, zirconium sulfate, composite zirconium oxide and zirconium hafnium for separating and preparing metal zirconium hafnium, and can also be used for products such as textiles, leather, rubber additives, metal surface treatment agents, paint drying agents, refractory materials, ceramics, catalysts, fireproof agents and the like.
Yttrium carbonate: white or colorless powder, which is mainly used for manufacturing catalyst, ceramic material, yttrium compound intermediate, chemical reagent and other industries.
The invention has the beneficial effects that:
compared with the prior art, the invention removes powder agglomeration caused by static electricity, the particle size range of the prepared PS-PVD special powder material is 1-30 mu m, the material has a core-shell structure and good fluidity, and the purity of T' phase is more than or equal to 99.9 percent after heat preservation for 200 hours at 1200 ℃ and is superior to Metco6700 adopted in the prior art TM . The powder can be gasified fully to form a typical PS-PVD columnar crystal coating in the PS-PVD process. The obtained coating has good combination property with a matrix, and reaches a complete oxidation resistance level in static oxidation resistance. Meanwhile, the coating also has excellent heat and corrosion resistance, and does not have the phenomena of wrinkling, cracking, skin lifting, falling off and the like. The coating can not bubble, peel and layer in the water quenching thermal shock and air cooling thermal shock test.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The comparative example and the examples of the present invention have the following parameters of part of raw materials:
eight-arm polyethylene glycol azide, average molecular weight: 2000, product number: 80040407-2000, guangzhou, inc. of carbohydrate technology;
Metco 6700 TM eurorey Kang Mei family surface technologies inc;
Metco 206A TM eurorey Kang Mei family surface technology limited.
Example 1
The thermal barrier coating is prepared by adopting the following PS-PVD process:
taking a special powder material for PS-PVD as a spraying raw material, and adopting PS-PVD spraying equipment to prepare a coating on a 316L stainless steel base material; in the PS-PVD spraying process, the argon flow is 35L/min, the helium flow is 60L/min, the current is 2500A, the spraying distance is 900mm, and the powder feeding amount of the powder feeder is 20g/min.
The PS-PVD special powder material is prepared by the following steps:
s1, preparing zirconium oxychloride and yttrium carbonate according to the proportion of 4mol% of yttria-stabilized zirconia, uniformly mixing the zirconium oxychloride, the yttrium carbonate and absolute ethyl alcohol, and reacting at 60 ℃ until the zirconium oxychloride, the yttrium carbonate and the absolute ethyl alcohol become a clear and transparent solution, so as to obtain a precursor for later use;
s2, transferring the precursor into a vacuum environment, and maintaining the precursor in a stable state of gas-liquid saturation under the stirring condition at 120 ℃ for 2 hours to obtain a mixture for later use;
s3, carrying out microwave treatment on the mixture at 140 ℃ for 4min to obtain an amorphous solid matter with yttrium zirconium uniformly mixed, removing residual organic matters from the amorphous solid matter, and adding an antistatic treatment agent to obtain the PS-PVD special powder material.
The mass ratio of the total mass of zirconium oxychloride and yttrium carbonate to the absolute ethyl alcohol is 1:0.5; the addition amount of the antistatic treatment agent is 0.3 weight percent of the total mass of zirconium oxychloride, yttrium carbonate and absolute ethyl alcohol.
The preparation method of the antistatic treatment agent comprises the following steps:
under the protection of M1 and nitrogen, 1.90kg of 3- (dimethylamino) -2-methyl-1-propanol, 1.30kg of 3, 5-dihydroxyphenylacetic acid methyl ester and 30kg of tetrahydrofuran are uniformly mixed, then 4.20kg of triphenylphosphine and 3.25kg of diisopropyl azodicarboxylate are added for carrying out an addition reaction, the addition reaction is carried out in two stages, firstly, the reaction is carried out for 3 hours at 0 ℃, and then the reflux reaction is carried out for 15 hours at 70 ℃; after the addition reaction, tetrahydrofuran was distilled off under reduced pressure, the residue was mixed with 30kg of diethyl ether, the filtrate was collected by filtration, then diethyl ether was distilled off under reduced pressure, the residue was mixed with 25kg of methylene chloride, 50kg of hydrochloric acid having a concentration of 1.0mol/L was added and the aqueous phase was separated, the pH of the aqueous phase was adjusted to 11, and then extraction with methylene chloride and the organic phase was collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain an addition reaction product for later use;
m2, mixing 2.15kg of the addition reaction product with 40kg of tetrahydrofuran uniformly, adding 0.50kg of lithium aluminum hydride, and carrying out reduction reaction at 35 ℃ for 12 hours; after completion of the reduction reaction, 45kg of hydrochloric acid at a concentration of 1.0mol/L was added to terminate the reaction, the aqueous phase was collected and the pH of the aqueous phase was adjusted to neutral, followed by extraction with methylene chloride and collection of the organic phase; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reduction reaction product for later use;
m3, taking 1.60kg of the reduction reaction product, 0.30kg of sodium hydride and 15kg of tetrahydrofuran, uniformly mixing, adding 0.65kg of 4-bromo-n-butyne, and carrying out substitution reaction at the temperature of 30 ℃ for 12 hours; after the substitution reaction is finished, adding 20kg of saturated ammonium chloride aqueous solution to stop the reaction, then extracting with dichloromethane, collecting an organic phase, drying the organic phase, distilling the organic phase under reduced pressure to remove the dichloromethane, and obtaining a substitution reaction product for later use;
m4, taking 2.10kg of the substitution reaction product, 5.50kg of methyl iodide and 15kg of acetonitrile, uniformly mixing and reacting at 25 ℃ for 24 hours; pouring the product into excessive diethyl ether at 0 ℃ after the reaction is finished, filtering, collecting precipitate, washing the precipitate by diethyl ether, and drying to obtain a reaction precursor for later use;
under the protection of M5 and nitrogen, 2.45kg of reaction precursor, 0.85kg of eight-arm polyethylene glycol azide and 40kg of N-methylpyrrolidone are taken and uniformly mixed, 0.35kg of pentamethyldiethylenetriamine and 0.15kg of copper bromide are added for cyclization reaction, the temperature of the cyclization reaction is 60 ℃, and the reaction time is 18 hours; after the cyclization reaction is finished, the product is poured into excessive isopropanol at the temperature of 0 ℃, and the precipitate is filtered, collected, washed by deionized water and dried to obtain the antistatic treatment agent.
In the embodiment, the purity of the T' phase of the powder material special for PS-PVD is more than or equal to 99.9%, and the particle size distribution of the powder is 1-30 mu m; the powder feeder of the PS-PVD spraying equipment is normal in powder feeding, and the powder blocking phenomenon does not occur in 60min of powder feeding.
Example 2
The thermal barrier coating is prepared by adopting the following PS-PVD process:
taking a special powder material for PS-PVD as a spraying raw material, and adopting PS-PVD spraying equipment to prepare a coating on a 316L stainless steel base material; in the PS-PVD spraying process, the argon flow is 35L/min, the helium flow is 60L/min, the current is 2500A, the spraying distance is 900mm, and the powder feeding amount of the powder feeder is 20g/min.
The PS-PVD special powder material is prepared by the following steps:
s1, preparing zirconium oxychloride and yttrium carbonate according to the proportion of 4mol% of yttria-stabilized zirconia, uniformly mixing the zirconium oxychloride, the yttrium carbonate and absolute ethyl alcohol, and reacting at 60 ℃ until the zirconium oxychloride, the yttrium carbonate and the absolute ethyl alcohol become a clear and transparent solution, so as to obtain a precursor for later use;
s2, transferring the precursor into a vacuum environment, and maintaining the precursor in a stable state of gas-liquid saturation under the stirring condition at 120 ℃ for 2 hours to obtain a mixture for later use;
s3, carrying out microwave treatment on the mixture at 140 ℃ for 4min to obtain an amorphous solid matter with yttrium and zirconium uniformly mixed, and carrying out residual organic matter removal treatment on the amorphous solid matter to obtain the PS-PVD special powder material.
The mass ratio of the total mass of zirconium oxychloride and yttrium carbonate to the absolute ethyl alcohol is 1:0.5.
in the embodiment, the purity of the T' phase of the powder material special for PS-PVD is more than or equal to 99.9%, and the particle size distribution of the powder is 1-30 mu m; powder blocking phenomenon occurs when the powder feeder of the PS-PVD spraying equipment feeds powder for 14 min.
Example 3
The thermal barrier coating is prepared by adopting the following PS-PVD process:
taking a special powder material for PS-PVD as a spraying raw material, and adopting PS-PVD spraying equipment to prepare a coating on a 316L stainless steel base material; in the PS-PVD spraying process, the argon flow is 35L/min, the helium flow is 60L/min, the current is 2500A, the spraying distance is 900mm, and the powder feeding amount of the powder feeder is 20g/min.
The PS-PVD special powder material is prepared by the following steps:
s1, preparing zirconium oxychloride and yttrium carbonate according to the proportion of 4mol% of yttria-stabilized zirconia, uniformly mixing the zirconium oxychloride, the yttrium carbonate and absolute ethyl alcohol, and reacting at 60 ℃ until the zirconium oxychloride, the yttrium carbonate and the absolute ethyl alcohol become a clear and transparent solution, so as to obtain a precursor for later use;
s2, transferring the precursor into a vacuum environment, and maintaining the precursor in a stable state of gas-liquid saturation under the stirring condition at 120 ℃ for 2 hours to obtain a mixture for later use;
s3, carrying out microwave treatment on the mixture at 140 ℃ for 4min to obtain an amorphous solid matter with yttrium zirconium uniformly mixed, removing residual organic matters from the amorphous solid matter, and adding an antistatic treatment agent to obtain the PS-PVD special powder material.
The mass ratio of the total mass of zirconium oxychloride and yttrium carbonate to the absolute ethyl alcohol is 1:0.5; the addition amount of the antistatic treatment agent is 0.3 weight percent of the total mass of zirconium oxychloride, yttrium carbonate and absolute ethyl alcohol.
The preparation method of the antistatic treatment agent comprises the following steps:
under the protection of M1 and nitrogen, 2.45kg of 3- (dimethylamino) -2-methyl-1-propanol, 1.70kg of 3, 5-dihydroxyphenylacetic acid methyl ester and 40kg of tetrahydrofuran are uniformly mixed, then 5.50kg of triphenylphosphine and 4.25kg of diisopropyl azodicarboxylate are added for carrying out addition reaction, the addition reaction is carried out in two stages, firstly, the reaction is carried out for 3 hours at 0 ℃, and then the reflux reaction is carried out for 15 hours at 70 ℃; after the addition reaction, tetrahydrofuran was distilled off under reduced pressure, the residue was mixed with 50kg of diethyl ether, the filtrate was collected by filtration, then diethyl ether was distilled off under reduced pressure, the residue was mixed with 40kg of methylene chloride, 100kg of hydrochloric acid having a concentration of 1.0mol/L was added and the aqueous phase was separated, the pH of the aqueous phase was adjusted to 11, and then extraction with methylene chloride and the organic phase was collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain an addition reaction product for later use;
m2, mixing 2.85kg of the addition reaction product with 50kg of tetrahydrofuran uniformly, adding 0.65kg of lithium aluminum hydride, and carrying out reduction reaction at 35 ℃ for 12 hours; after completion of the reduction reaction, 60kg of hydrochloric acid at a concentration of 1.0mol/L was added to terminate the reaction, the aqueous phase was collected and the pH of the aqueous phase was adjusted to neutral, followed by extraction with methylene chloride and collection of the organic phase; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reduction reaction product for later use;
m3, taking 2.10kg of the reduction reaction product, 0.45kg of sodium hydride and 20kg of tetrahydrofuran, uniformly mixing, adding 0.85kg of 4-bromo-n-butyne, and carrying out substitution reaction at 30 ℃ for 12 hours; after the substitution reaction is finished, 30kg of saturated ammonium chloride aqueous solution is added to stop the reaction, then dichloromethane is used for extraction, an organic phase is collected, and the organic phase is dried and distilled under reduced pressure to remove the dichloromethane, so that a substitution reaction product is obtained for later use;
m4, taking 2.70kg of the substitution reaction product, 7.15kg of methyl iodide and 25kg of acetonitrile, uniformly mixing and reacting at 25 ℃ for 24 hours; pouring the product into excessive diethyl ether at 0 ℃ after the reaction is finished, filtering, collecting precipitate, washing the precipitate by diethyl ether, and drying to obtain a reaction precursor for later use;
under the protection of M5 and nitrogen, 3.20kg of reaction precursor, 1.10kg of eight-arm polyethylene glycol azide and 60kg of N-methylpyrrolidone are taken and uniformly mixed, 0.50kg of pentamethyldiethylenetriamine and 0.20kg of copper bromide are added for cyclization reaction, the temperature of the cyclization reaction is 60 ℃, and the reaction time is 18 hours; after the cyclization reaction is finished, the product is poured into excessive isopropanol at the temperature of 0 ℃, and the precipitate is filtered, collected, washed by deionized water and dried to obtain the antistatic treatment agent.
In the embodiment, the purity of the T' phase of the powder material special for PS-PVD is more than or equal to 99.9%, and the particle size distribution of the powder is 1-30 mu m; the powder feeder of the PS-PVD spraying equipment is normal in powder feeding, and the powder blocking phenomenon does not occur in 60min of powder feeding.
Comparative example 1
The thermal barrier coating is prepared by adopting the following PS-PVD process:
by Metco6700 TM For spraying raw materials, a PS-PVD spraying device is adopted to spray the raw materials on a 316L stainless steel baseCoating preparation is carried out on the bulk material; in the PS-PVD spraying process, the argon flow is 35L/min, the helium flow is 60L/min, the current is 2500A, the spraying distance is 900mm, and the powder feeding amount of the powder feeder is 20g/min.
In this example, metco6700 TM The purity of the T' phase of the powder is 93-95%, and the particle size distribution of the powder is 5-40 mu m; powder blocking phenomenon occurs when the powder feeder of the PS-PVD spraying equipment feeds powder for 11 min.
Comparative example 2
The thermal barrier coating is prepared by adopting the following PS-PVD process:
with Metco206A TM Coating preparation is carried out on 316L stainless steel matrix material by adopting PS-PVD spraying equipment for spraying raw materials; in the PS-PVD spraying process, the argon flow is 35L/min, the helium flow is 60L/min, the current is 2500A, the spraying distance is 900mm, and the powder feeding amount of the powder feeder is 20g/min.
In this embodiment, metco206A TM The particle size of the powder is 40-100 mu m, due to Metco206A TM Cannot be applied to PS-PVD processes, and therefore, no corresponding thermal barrier coating is produced.
Test example 1
According to the method and the steps specified by the thermal cycle test standard Q/AVIC06016.1-2013 of the middle-voyage industry, the thermal shock test is carried out on the thermal barrier coating prepared by the method. The test uses a standard sheet specimen, the specification (mm): Φ25.4x5. The thermal shock test is divided into a coating thermal shock (water quenching) test and a coating thermal shock (air cooling) test; the detection method of the thermal shock (water quenching) test of the coating is as follows: preserving heat at 1100 ℃ for 10min, water-cooling for 10min, and sampling at different circulation times; the detection method of the thermal shock (air cooling) test of the coating is as follows: preserving the temperature at 1050 ℃ for 10min, air-cooling for 5min, and sampling at different circulation times. And after the thermal barrier coating is cycled to the target times, the appearance state of the coating is detected, and the thermal shock test results of the thermal barrier coating are shown in table 1.
Table 1:
as can be seen from the test results of the thermal shock test, the methodThe thermal barrier coating prepared from the powder material has good thermal vibration performance and has no defects under the target test cycle. Whereas the existing foundation adopts Metco6700 TM Under the same air cooling thermal shock test condition, the powder material has defects after 3100 times of circulation, and the comprehensive performance of the powder material is superior to that of the prior art.
Test example 2
The gas hot corrosion test of the thermal barrier coating prepared in part of the examples or the comparative examples in the invention is carried out by referring to the specific steps in the standard HB 7740-2004 gas hot corrosion test method. The test uses cylindrical samples, 5 pieces per group. The test temperature was 900℃and the test duration was 300h. The results of the tests are calculated as an average value, and the results of the gas hot corrosion test of the thermal barrier coating are shown in Table 1.
Table 2:
| name of the name | Average corrosion rate [ g/(m) 2 ·h)] |
| Example 1 | 0.0814 |
| Example 2 | 0.1931 |
| Example 3 | 0.0837 |
| Comparative example 1 | 0.2479 |
After the test, the samples of the example 1 do not have the phenomena of wrinkling, cracking, skin lifting, falling off and the like; example 2 and comparative example 1 showed different degrees of wrinkling, cracking, skinning, and peeling, among which the phenomenon of comparative example 1 was the most serious.
Test example 3
The test of the oxidation resistance of the thermal barrier coating prepared in some examples or comparative examples in the present invention is performed by referring to the specific steps in HB 5258-2000 test method for measuring the oxidation resistance of Steel and superalloy. The experimental group is 316L stainless steel with the surface covered with the thermal barrier coating in the examples and the comparative examples, and the blank control group is common 316L stainless steel. The test uses cylindrical samples, 5 pieces per group. The test method is a weight increasing method, the test temperature is 1100 ℃, and the test time is 200 hours. The oxidation resistance was evaluated according to the classification method of Table 4 in the standard, and the test results are shown in Table 3.
Table 3:
as can be seen from the test results of the above test examples, the powder agglomeration caused by static electricity is removed in example 1, and the provided PS-PVD-dedicated powder material has good flowability. When the method is suitable for PS-PVD process, the powder can be fully gasified to form a typical PS-PVD columnar crystal coating. The obtained coating has good combination property with a matrix, and achieves complete antioxidation level after static antioxidation for 200 hours at 1100 ℃. Meanwhile, the coating also has excellent heat and corrosion resistance, and has no phenomena of wrinkling, cracking, skin lifting, falling off and the like after being subjected to a gas hot corrosion test for 300 hours at 900 ℃.
The reason for this result may be that in the antistatic treatment agent employed in the present invention, the octa-arm polyethylene glycol azide has an azide group at each end of the octa-arm attached to one hexaglycerin core, and the steric hindrance provided by the biscationic group can prevent the reaction of the active group with the methylene group by reacting with the terminal alkynyl group to form a hydrophobic heterocycle and introducing two cationic groups at each branch, thereby improving the stability thereof. In addition, the antistatic treatment agent has multi-branch and multi-cation groups and high local ion concentration, and flexible ether bonds and alkyl spacers in the side chains can increase the mobility of the cation groups, so that the transfer capacity of charges is improved, and the high-efficiency removal of static electricity is realized. The elements of the antistatic treatment agent are mainly carbon, oxygen, hydrogen and nitrogen, and in the PS-PVD spraying process, the antistatic treatment agent is excited to decompose to form gaseous micromolecules without participating in the process of forming thermal barrier powder by powder, so that the coating structure is not influenced.
Claims (7)
1. The preparation method of the special powder material for PS-PVD is characterized by comprising the following steps:
s1, preparing zirconium oxychloride and yttrium carbonate according to the proportion of 4mol% of yttria-stabilized zirconia, uniformly mixing the zirconium oxychloride, the yttrium carbonate and a surfactant, and reacting under a heating condition to obtain a precursor for later use;
s2, transferring the precursor into a vacuum environment, and achieving and maintaining a stable state of gas-liquid saturation under heating and stirring conditions to obtain a mixture for later use;
s3, carrying out microwave treatment on the mixture to obtain an amorphous solid material with yttrium zirconium uniformly mixed, removing residual organic matters from the amorphous solid material, and then adding an antistatic treatment agent to obtain a PS-PVD special powder material;
the heating temperature in the step S1 is 60-120 ℃; the heating temperature in the step S2 is 60-120 ℃, and the maintaining time of the gas-liquid saturated stable state is 1-2 h; the working temperature of the microwave treatment in the step S3 is 80-200 ℃ and the treatment time is 3-5 min;
the preparation method of the antistatic treatment agent comprises the following steps of:
under the protection of M1 and nitrogen, 1.90-2.45 parts of 3- (dimethylamino) -2-methyl-1-propanol, 1.30-1.70 parts of 3, 5-dihydroxyphenylacetic acid methyl ester and 30-40 parts of tetrahydrofuran are uniformly mixed, and then 4.20-5.50 parts of triphenylphosphine and 3.25-4.25 parts of diisopropyl azodicarboxylate are added for reaction; after the reaction is finished, removing tetrahydrofuran by reduced pressure distillation, mixing residues with 30-50 parts of diethyl ether, filtering and collecting filtrate, then removing diethyl ether by reduced pressure distillation, mixing residues with 25-40 parts of dichloromethane, adding 50-100 parts of hydrochloric acid, separating a water phase, adjusting the pH of the water phase to 10.0-11.5, extracting with dichloromethane, and collecting an organic phase; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reaction product for later use;
m2, taking 2.15-2.85 parts of the reaction product and 40-50 parts of tetrahydrofuran to be uniformly mixed, adding 0.50-0.65 part of lithium aluminum hydride and carrying out reduction reaction; after the reduction reaction is finished, 45-60 parts of hydrochloric acid is added to stop the reaction, the water phase is collected, the pH value of the water phase is adjusted to be neutral, and then dichloromethane is used for extraction and an organic phase is collected; drying the organic phase, and distilling under reduced pressure to remove dichloromethane to obtain a reduction reaction product for later use;
m3, taking 1.60-2.10 parts of the reduction reaction product, 0.30-0.45 part of sodium hydride and 15-20 parts of tetrahydrofuran, uniformly mixing, adding 0.65-0.85 part of 4-bromo-n-butyne, and carrying out substitution reaction; after the substitution reaction is finished, adding 20-30 parts of saturated ammonium chloride aqueous solution to stop the reaction, then extracting with dichloromethane, collecting an organic phase, drying the organic phase, and distilling under reduced pressure to remove the dichloromethane to obtain a substitution reaction product for later use;
m4, taking 2.10 to 2.70 parts of the substitution reaction product, 5.50 to 7.15 parts of methyl iodide and 15 to 25 parts of acetonitrile to be uniformly mixed and reacted; pouring the product into excessive diethyl ether at 0-4 ℃ after the reaction is finished, filtering, collecting precipitate, washing the precipitate with diethyl ether, and drying to obtain a reaction precursor for later use;
under the protection of M5 and nitrogen, 2.45 to 3.20 parts of reaction precursor, 0.85 to 1.10 parts of eight-arm polyethylene glycol azide and 40 to 60 parts of N-methylpyrrolidone are taken and uniformly mixed, and 0.35 to 0.50 part of pentamethyl diethylenetriamine and 0.15 to 0.20 part of copper bromide are added for cyclization reaction; after the cyclization reaction is finished, pouring the product into excessive isopropanol at the temperature of 0-4 ℃, filtering, collecting the precipitate, washing the precipitate by deionized water, and drying to obtain the antistatic treatment agent.
2. The method for preparing the PS-PVD specialized powder material according to claim 1, wherein: the reaction in the step M1 is carried out in two stages, namely, firstly, the reaction is carried out at the temperature of 0-4 ℃ for 2-5 h, and then, the reflux reaction is carried out at the temperature of 65-80 ℃ for 12-18 h.
3. The method for preparing the PS-PVD specialized powder material according to claim 1, wherein: the temperature of the reduction reaction in the step M2 is 25-40 ℃ and the reaction time is 12-18 h; the temperature of the substitution reaction in the step M3 is 25-35 ℃ and the reaction time is 9-15 h.
4. The method for preparing the PS-PVD specialized powder material according to claim 1, wherein: the temperature of the reaction in the step M4 is 20-30 ℃ and the reaction time is 18-36 h.
5. The method for preparing the PS-PVD specialized powder material according to claim 1, wherein: the temperature of the cyclization reaction in the step M5 is 50-65 ℃ and the reaction time is 12-36 h.
6. A special powder material for PS-PVD is characterized in that: the method according to any one of claims 1 to 5.
7. The use of the PS-PVD specific powder material according to claim 6 in a PS-PVD process, comprising the steps of:
taking a PS-PVD special powder material as a spraying raw material, and adopting PS-PVD spraying equipment to prepare a coating on a base material; in the PS-PVD spraying process, the argon flow is 30-40L/min, the helium flow is 50-70L/min, the current is 2400-2600A, the spraying distance is 800-1000 mm, and the powder feeding amount of the powder feeder is 5-35 g/min.
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