CN105525273B - A kind of stainless steel carborundum hydrogen permeation preventing coating and preparation method thereof - Google Patents
A kind of stainless steel carborundum hydrogen permeation preventing coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 96
- 239000011248 coating agent Substances 0.000 title claims abstract description 78
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 61
- 239000001257 hydrogen Substances 0.000 title claims abstract description 61
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 56
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 30
- 239000010935 stainless steel Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 31
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000007704 transition Effects 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 116
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 50
- 238000000034 method Methods 0.000 claims description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000004544 sputter deposition Methods 0.000 claims description 30
- 239000012536 storage buffer Substances 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 12
- 238000005240 physical vapour deposition Methods 0.000 claims description 12
- 238000007747 plating Methods 0.000 claims description 9
- 239000013077 target material Substances 0.000 claims description 9
- 238000007740 vapor deposition Methods 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 3
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 2
- 238000005477 sputtering target Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000002131 composite material Substances 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 9
- 230000035699 permeability Effects 0.000 abstract description 9
- 230000000149 penetrating effect Effects 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- 229910000619 316 stainless steel Inorganic materials 0.000 description 15
- 238000011160 research Methods 0.000 description 15
- 239000010408 film Substances 0.000 description 13
- 230000004888 barrier function Effects 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 229910052722 tritium Inorganic materials 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000005524 ceramic coating Methods 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- 229910000951 Aluminide Inorganic materials 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 229910002060 Fe-Cr-Al alloy Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 238000005269 aluminizing Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052805 deuterium Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011824 nuclear material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910018173 Al—Al Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910017372 Fe3Al Inorganic materials 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- 229910015392 FeAl3 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910000943 NiAl Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000007735 ion beam assisted deposition Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical class O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000010290 vacuum plasma spraying Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
-
- 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
- C23C14/0641—Nitrides
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of stainless steel carborundum hydrogen permeation preventing coating, including transition zone, storage H cushions, the resistance hydrogen layer successively arranged upwards from stainless steel base；The transition zone is made up of layer of titanium metal and TiN layer, and the storage H cushions are amorphous SixC1‑xGraded bedding, 1 ＞ x >=0.5, the resistance hydrogen layer is SiC.The present invention also proposes the preparation method of the carborundum hydrogen permeation preventing coating.The present invention proposes to be combined with storage H cushions with resistance H coatings, prepares the anti-hydrogen permeability coating of matrix/transition zone/storage H cushions/SiC composite constructions.On the resistance H coating SiC Membranous Foundations of Flouride-resistani acid phesphatase, storage H cushions Si is prepared using gas phase deposition technologyxC1‑xGraded bedding, utilize SixC1‑xThe very competent C and Si dangling bonds of hydrogen are largely caught present in graded bedding, optimize the anti-hydrogen penetrating quality of matrix/transition zone/storage H cushions/SiC composite constructions.
Description
Technical Field
The invention belongs to the field of plating of metal materials, and particularly relates to a metal material sputtered with a hydrogen-resistant layer and a preparation method thereof.
Background
In recent years, hydrogen permeation barrier coatings, also called H-barrier coatings, are developed for various base materials, and attempts are made to prevent permeation and leakage of hydrogen and isotopes thereof. Currently, the commonly used H-resistant coatings are mainly classified into the following categories.
The oxide coating has the advantages of high melting point, stable chemical property, simple preparation process, good H resistance and the like, and is the earliest studied hydrogen permeation resistant coating. Formed by direct oxidation of the substrate surface or oxidation of the coating, including Al2O3，Cr2O3，Y2O3，SiO2，Er2O3And the like. In general, the single-layer oxide H-resistant coating is mostly Cr2O3，Al2O3And SiO2Often in combination with other coatings. Y is2O3The permeability of the coating tritium can be reduced by two orders of magnitude, and the coating tritium is often used in combination with other coatings. Chemical densification coating technology (CDC) adopted by Japan atomic energy research institute for preparing Cr on 316 stainless steel surface2O3-SiO2Ceramic hydrogen barrier coatings, tritium permeation barrier factor (PRF) greater than 100(Takayuki Terai, Toshiaki Yoneoka, Himhisa Tanaka, Trititanium permeability through austenitic steady state with chemical characterization as a titanium permeability barrier, Journal of Nuclear Materials,1994:212/215: 976;). Levchuk et Al obtained a-Al on the order of microns in thickness on the surface of Eurofer stainless steel using PVD2O3The coating results show that the PRF of the coating is 1000(Serra E, Calza Bini A, Cosoli G, Hydrogen polymerization measurements on aluminum, Journal of the American ceramic society,2005,88(1):15) at 700-800 ℃. Respectively preparing Al on 316L stainless steel by MOCVD method in Beijing nonferrous metals research institute, litshuai and the like2O3、Y2O3And Cr2O3The H-resistant coating (inorganic material science report, Li Shuai, He Di, Liu Xiao Peng, Zhang super, Wang Shumao, Yuqing river, Qihao Chen, Jian Lijun, 316L stainless steel matrix alumina coating hydrogen permeability, inorganic material science report, 2013,28(7) 775;), has excellent hydrogen resistance. Wherein Al is2O3The hydrogen permeation barrier factor (PRF) of the coating to 316L stainless steel is 59-119 at 600-700 ℃. Y is2O3The PRF of the coating is 240-410 at 550-700 ℃. Cr (chromium) component2O3The PRF of the coating is 24-117 at 550-600 ℃.
The Ti-based ceramic coating has good corrosion resistance and higher H resistance effect. The coating mainly comprises titanium nitride, titanium carbide and a composite or mixed coating of the titanium nitride and the titanium carbide, various titanium-based ceramic coatings can be prepared by adopting a CVD or PVD method, and research results show that the Ti-based ceramic coating has good H resistance at low temperature. Preparing 2-5 microns thick on a 316L stainless steel substrate by using a PVD methodA TiC + TiN coating of micron size (C.Q.Shang, A.J.Wu, Y.J.Li, The behaviourof dispersion and duration of titanium through 316L stainless steel with coating of TiC and TiN + TiC, Journal of Nuclear Materials,1992,191-194: 221; and The like) followed by chemical heat treatment produced a CH4 hydrogen permeation resistant coating on The TiC surface. The test results show that the hydrogen permeability in the coating is reduced by 4-6 orders of magnitude. However, the oxidation of TiC, TiN and TiC/TiN at a temperature above 450 ℃ is difficult to overcome. The yaoshuo and the like add a coating (SiO2 or TiN) with higher oxidation resistance on the surface of the TiN + TiC gradient coating to prevent the TiN + TiC gradient coating from losing efficacy in the use process (research on tritium permeation resistance of different coatings of the yaoshuo and fusion reactor cladding materials, Shuoshi graduate paper of Chinese atomic energy science research institute, 2001). Preparing TiN + TiC + TiN and TiN + TiC + SiO on 316L stainless steel substrate by PVD method2And (4) coating. The coating thickness was 2 microns and 3 microns, respectively. The permeability of the two coatings is reduced by 4-5 and 4-6 orders of magnitude relative to the base material.
The silicide coating is mainly focused on the SiC coating. SiC is the most studied silicide H-barrier coating at present and has been used industrially because of its extremely high hardness and wear resistance and can be used as a superhard coating. SiC reacts with oxygen at high temperature to form a very thin layer of dense SiO2And the passivation film enables SiC to have good high-temperature oxidation resistance and can prevent SiC from being continuously oxidized. The preparation of SiC coatings generally employs CVD and PVD methods. Kingy et al deposited a 2 micron thick SiC coating on 316L stainless steel using ion beam assisted deposition and ion implantation (Kingy, Standy, research on the deposition of SiC on stainless steel surfaces as a hydrogen permeation barrier, reports on metals 1999,35(6): 654;). The coating reduced the hydrogen permeability of the stainless steel substrate by nearly 5 orders of magnitude. Chikada et al prepared SiC H-barrier coatings on 316 and F82H stainless steel substrates using radio frequency magnetron sputtering (Chikada T, Suzuki A, Terai T, Deuterium permanence and Manual coatings of amorphous silicon carbide coatings on steels, Fu-division engineering and Design,2011,86(9):2192), and investigated the H-barrier properties and thermal stability of SiC coatings. The research result shows that the prepared SiC film isAmorphous state. The PRF is about 1000 within the range of 450-550 ℃. When the temperature exceeds 600 ℃, the H-blocking effect is reduced because the H penetration is increased due to microcracks generated inside the SiC when the temperature is too high. The Er2O3/SiC composite coating is adopted by Chinese engineering Physics research institute to improve the H penetration resistance of 316L stainless steel, and a 300nm film layer can reach 500 PRF under the condition of 500 ℃ (Yaoyangyu, Yanghui, Tanshan, Hanhua, research of using SiC film as tritium penetration resistant barrier layer, Nuclear Fusion and plasma Physics,2002,22: 65;).
The aluminide composite coating mainly comprises A1/Fe + Al2O3And an AlN coating layer formed by causing a concentration gradient of aluminum in the vicinity of the surface of the base metal to form an aluminum-based intermetallic compound layer, the aluminum content of the base metal being gradably changed to 30% to 80% Al from the aluminum content to the surface aluminum content. The aluminide coating is easy to fall off due to the difference of the thermal expansion coefficients of the substrate and the coating material, which is a technical problem at present. The greater the difference in thermal expansion coefficients during cold and hot changes, the greater the stresses that are generated. The cold and hot process is repeated, the stress is accumulated and enhanced continuously, and cracks are possibly generated until the coating falls off. Preparation of A1/Fe + Al2O3The H-blocking coating can be prepared by hot dip coating, flame spraying, vacuum plasma spraying, ion implantation, chemical vapor deposition, magnetron sputtering, hot isostatic pressing, embedded aluminizing and the like. Kalin et Al put Crl8Nil0Ti austenitic stainless steel into 10% Al + 90% Li melt and aluminize for 5-100 h at 600-800 ℃, and the obtained coating has a complex intermetallic compound multiphase structure, such as FeAl3, FeAl, Fe3Al and NiAl, AlCr2 and a-Fe, and the thickness varies with different temperatures and time. The results of the study showed that the barrier effect of the two-sided aluminizing was the best, PRF was 2000 and 2700(B.A. kalin, V.L. Yakushin, E.P. Fomina, Tritie barrier definition for austenitizing steel substrates alloying in a lithium melt 1998, Fusion Engineering and design 1998,41: 119;). Fazio et Al prepared Fe-Cr-Al coating by atmospheric plasma spraying method, and substrate selected from MANETII and F82H2mod steel. The coating has certain H permeation resistance, but the coating is combined withThere is a large residual stress between the substrates, making the coating susceptible to flaking during use (Fazio C, Stein-Fechner K, Serra E, invasion on the substrate of plasma sprayed Fe-Cr-Al coatings evaluation barrier, J nucleic Material 1999,273: 233). The uniform, compact and stable Al-Al can be obtained by performing vacuum thermal oxidation treatment on aged silver and the like by utilizing a PECVD (surface technology 2008,37(3): 41) of research on preparing Al-Al2O3 composite hydrogen-resistant coating by using a PECVD technology (silver aged, aged-Changan, Zhangchengcheng, PECVD)2O3Thin film composites, but small amounts of carbide impurities are present. The film has obvious deuterium resistance performance below 450 ℃, and the H resistance factor can reach 244.
The novel H-resistant material: in recent years, the H resistance of graphene and BN attracts wide attention, and a large number of H resistance material systems based on BN and graphene emerge. Tamura et al, using a magnetic enhanced plating-ion-plating, obtained a BN coating on a 316L stainless steel substrate, the coating thickness was 1.5 μm, and after the BN coating was plated on the 316L stainless steel Surface, the H penetration rate of the stainless steel could be effectively reduced, within the range of 300-500 ℃, the PRF value of BN was 100(M.Tamura, M.Nomab, M.Yamashitic, Characteric change of hydrogen permeability steel plate by BN coating, Surface and Coatings Technology,2014,260: 148;).
Although the research on H-resistant coatings has made many advances in material system design, performance optimization and mechanism, etc., the H-resistant coatings have been applied in engineering practice. However, recent studies have found that, for "thin" hydrogen atoms, the atomic spacing in corundum, a coating with excellent H-barrier properties, is so large that the hydrogen atoms can "walk" freely in it and form many tiny pits on the metal substrate side. With the continuous "growth" of the pits, the hydrogen atoms have enough space to recombine to form hydrogen molecules and exert pressure on the oxide film. When the diameter of the pit is large enough to reach a certain critical dimension, the oxide film is supported to be plastically deformed and bubble-formed outward, destroying the effect of the H-barrier coating (D.G. Xie, Z.J. Wang, J.Sun, J.Li, E.Ma, Z.W. Shann, In situ termination of the initiation of hydrogen bubbles at the aluminum metal/oxide interface, Nature Materials,2015,10.1038: 4336). In addition, recent research also shows that hydrogen can easily penetrate through two-dimensional materials such as graphene and BN, and the process can be significantly accelerated by heating and adding a catalyst, which means that the conventional thought that hydrogen cannot penetrate through two-dimensional materials such as defect-free graphene does not work well.
(Algara-Siller,G.O.Lehtinen,F.C.Wang,R.R.Nair,U.Kaiser,H.A.Wu,A.K.Geim,I.V.Grigorieva,Square ice in graphene nanocapillaries,Nature,2015,519(7544):443)
Meanwhile, in recent years, the development and research of hydrogen energy technology as clean and efficient energy have obviously progressed, and important reference is provided for solving the problem of hydrogen permeation prevention. In summary, these new recognitions and discoveries provide important references to many of the unsolved puzzles associated with hydrogen-related applications. Therefore, the performance regulation and mechanism research of the hydrogen permeation resistant composite coating is developed, the design of a hydrogen permeation resistant material system and the development of related technologies are guided, the performance of the H-resistant coating is optimized, and the controllability of the H-resistant coating is improved, so that the hydrogen permeation resistant composite coating becomes a research hotspot in the field of hydrogen-related application.
Disclosure of Invention
To overcome the above-mentioned drawbacks of the prior art, it is an object of the present invention to provide a hydrogen permeation resistant coating composed of a matrix/transition layer/H storage buffer layer/SiC composite structure.
Another object of the present invention is to propose a method for preparing said hydrogen permeation barrier coating.
The technical scheme for realizing the purpose of the invention is as follows:
a silicon carbide hydrogen permeation resistant coating for stainless steel comprises a transition layer, an H storage buffer layer and a hydrogen permeation resistant layer which are arranged from a stainless steel substrate upwards layer by layer; the transition layer is composed of a metal titanium layer and a TiN layer, and the gradient layer is amorphous SixC1-xX is more than 1 and more than or equal to 0.5, and the hydrogen-resistant layer is SiC.
Wherein,the transition layer consists of a Ti layer and a TiN layer, wherein the Ti layer is 100-300 nm thick, the TiN layer is 200-500 nm thick, and the H storage buffer layer is amorphous SixC1-xAnd the gradient layer, x is more than 1 and more than or equal to 0.5, the thickness is 1-4 mu m, and the thickness of the hydrogen resistance layer is 500 nm-1 mu m.
Wherein the material of the stainless steel substrate is one of 316L, 304 and 321.
The invention relates to a preparation method of a silicon carbide hydrogen permeation resistant coating for stainless steel, which is characterized by comprising the following steps of:
s1 preparing Ti/TiN transition layer by magnetron sputtering method, depositing Ti layer by using Ti target as sputtering target, vacuumizing to 10%-5～10-3Pa, introducing argon gas for direct current sputtering, wherein the current is 5-8A, the working vacuum is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm; then sputtering a TiN layer by adopting an intermediate frequency power supply or a radio frequency power supply;
s2, preparing an H storage buffer layer on the transition layer by using a vapor deposition method, wherein the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method;
s3, preparing the SiC hydrogen-resistant layer on the H storage buffer layer by using a vapor deposition method, wherein the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method.
The preparation method of the TiN layer in the transition layer in S1 comprises the following steps:
depositing TiN on the metal Ti layer, and pre-vacuumizing to 10 DEG-5～10-3Pa, introducing argon and nitrogen, Ar/N2The flow ratio is 2-8, medium-frequency magnetron sputtering (adopting a medium-frequency power supply) is adopted, the current is 5-8A, the working vacuum is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm.
Or, the preparation method of the TiN layer in the S1 comprises the following steps: firstly, pre-vacuuming to 10-5～10-3Pa, introducing argon and nitrogen, Ar/N2The flow ratio is 2-8, the sputtering power is 100-200W (a radio frequency power supply is adopted)) The working vacuum is 0.3 Pa-2 Pa, the heating temperature is 150-300 ℃, the target base distance is 80-100mm, and the thickness is 200-500 nm.
The preparation method of the H storage buffer layer in S2 comprises the following steps:
adopting pure silicon target material, firstly pre-vacuumizing to 10 DEG-5～10-3Pa, then introducing Ar and C2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio is 2-20, the sputtering current is 4-10A, the sputtering air pressure is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm.
Preferably, during the process of the gradient layer plating, the flow of the introduced Ar is constant, the sputtering current is increased from 4A to 10A in a gradient manner, or the C is reduced in a gradient manner2H2At a gas flow rate of Ar/C2H2The flow ratio is from 2 to 20, 2 to 5 gradients are arranged in total, each gradient sputtering current is kept for 10 to 20min, and a single layer is obtained, and the total thickness is controlled to be 1 to 4 mu m.
Or, the preparation method of the H storage buffer layer in S2 comprises the following steps:
the precursor material is methyl trichlorosilane, and the carrier gas is H2The diluent gas is argon, the deposition temperature is 1100 DEG～1300℃，MTS+H2The flow rate is increased from 0.35L/min to 0.8L/min in a gradient way, the flow rate of Ar of the diluent gas is 160L/H, and the flow rate of H of the diluent gas is increased from 0.35L/min in a gradient way2The flow rate is increased from 1L/min to 4L/min in a gradient manner, 2-5 gradients are set in total, and each gradient is MTS + H2The flow rate is kept for 10-20 min.
The diluent gas is the working gas in CVD, and does not participate in the reaction. The hydrogen gas together with MTS is carrier gas, the carrier gas has the function of carrying a gas sample or gasified sample gas together into the vacuum chamber at a certain flow rate, so that the hydrogen gas serving as the carrier gas enters together with MTS, and the hydrogen gas serving as the diluting gas enters from the other gas inlet.
The preparation method of the SiC hydrogen-resistant layer in S3 comprises the following steps:
using pure silicon targetsThe wood is firstly pre-vacuumized to 10 degrees-5～10-3Pa; then Ar and C are introduced2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio is 2-20, the sputtering current is 4-10A, the sputtering air pressure is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm.
Or, the preparation method of the SiC hydrogen-resistant layer in S3 comprises the following steps:
adopting SiC target material, firstly pre-vacuumizing to 10 DEG C-5～10-3Pa; then Ar is introduced, the sputtering power is 120-160W, the sputtering pressure is 0.3-0.6 Pa, the heating temperature is 300-600 ℃, and the target base distance is 80-100 mm.
The invention has the beneficial effects that:
SiC is the most studied silicide H-barrier coating at present and has been used industrially because of its extremely high hardness and wear resistance and can be used as a superhard coating. SiC reacts with oxygen at high temperature to form a very thin layer of dense SiO2And the passivation film enables SiC to have good high-temperature oxidation resistance and can prevent SiC from being continuously oxidized. Furthermore, amorphous SixC1-xThe film contains a large amount of C-and Si-dangling bonds, and can play a role in storing H. The combination of the two materials not only plays a role in resisting H permeation, but also can further fix the part H penetrating through the SiC H-resisting layer, and is the combination of chemical bonds, so that the combination is stronger, and the effect of preventing hydrogen permeation can be achieved.
Based on a series of challenges faced by the H-resistant coating in practical application, we have purposefully pre-probed in earlier work. Not only the low-temperature growth mechanism, the structure of the SiC film and the relation and the mechanism of the retention, diffusion and permeation of tritium are researched from the theoretical aspect. Meanwhile, by combining the surface treatment of the matrix and the buffer layer, the SiC film with uniform thickness and firm combination is obtained on the surface of the matrix with a complex shape at the tempering temperature far lower than 316L stainless steel, and the structural test shows that the SiC film has excellent radiation resistance and tritium permeation resistance.
The invention provides a hydrogen-permeability-resistant coating with a matrix/transition layer/H storage buffer layer/SiC composite structure, which is prepared by combining an H storage buffer layer with an H-resistant coating. Preparing a buffer layer Si for storing H by adopting a vapor deposition technology on the basis of an anti-irradiation H-resistant coating SiC filmxC1-xGraded layer of SixC1-xA large number of C-and Si-dangling bonds with extremely strong capability of capturing hydrogen exist in the gradual change layer, the hydrogen permeation resistance of the matrix/transition layer/H storage buffer layer/SiC composite structure is optimized, and the controllability of the matrix/transition layer/H storage buffer layer/SiC composite structure is improved.
Drawings
FIG. 1 is a view of the structure of the coating of the present invention.
Detailed Description
The following detailed description is illustrative of the invention and is not to be construed as limiting the invention.
The magnetron sputtering equipment is TRX-750 vacuum magnetron sputtering equipment manufactured by Beijing Tianrui starlight thermal technology development Co. The chemical vapor deposition equipment model is NEE-4000(M) electron beam evaporation system, produced by Nano, China, Inc.
In the examples, unless otherwise specified, the technical means used are those conventional in the art.
Example 1:
the method comprises plating transition layer Ti/TiN on 316L austenitic stainless steel substrate, preparing by medium frequency magnetron sputtering, plating metal Ti, and setting background vacuum of 1 × 10-3Pa, the working pressure is 0.6Pa, the argon flow is 120sccm, the Ti target current is 8A, the voltage is 550V, the target base distance is 80mm, and the time is 10min, so that the thickness of the prepared titanium layer is about 200 nm. Depositing TiN on the basis of metal TiBottom vacuum of 1X 10-3Pa, working pressure of 0.6Pa, argon flow of 120sccm, nitrogen flow of 15sccm, Ti target current of 8A, voltage of 530V, target base distance of 80mm, time of 20min and thickness of about 350 nm.
The CVD method is adopted to prepare the H storage buffer layer, and the specific parameters are as follows:
the precursor raw material is MTS, and the carrier gas is H2(purity 99.8%), argon as diluent gas, deposition temperature 1100 deg.C, MTS + H2The flow rate is increased from the first gradient of 0.35L/min, the second gradient of 0.45L/min, the third gradient of 0.6L/min, the fourth gradient of 0.8L/min to 0.8L/min, each gradient is kept for 15min, the Ar (dilution) flow rate is 160L/H, H2The flow rate of (dilution) was increased from 1L/min to 4L/min in a gradient manner to control the thickness of the obtained gradient layer to 1.5. mu.m.
Preparing the SiC hydrogen-resistant layer by adopting a chemical vapor deposition method: trichloromethylsilane (MTS) is used as a raw material, and the process conditions are that the temperature is 1100 ℃, MTS + H2Flow rate 0.3L/min, H2The flow rate (dilution) is 0.5L/min, and the flow rate of Ar is 0.8L/min; the furnace pressure is 3kPa, and the thickness of the SiC hydrogen-resistant layer is 1 μm.
The structure of the hydrogen permeation resistant coating prepared in the embodiment is shown in fig. 1, and the transition layer, the H storage buffer layer and the hydrogen resistance layer are arranged from the stainless steel substrate upwards layer by layer, and through tests, the PRF of the composite coating is 1500 within the range of 500-600 ℃.
Example 2:
the method comprises the steps of plating a transition layer Ti/TiN on a substrate of 316L austenitic stainless steel, and preparing the austenitic stainless steel by adopting a medium-frequency magnetron sputtering method, wherein metal Ti is plated firstly, the background vacuum is 1 multiplied by 10 < -3 > Pa, the working pressure is 0.3Pa, the argon flow is 90sccm, the Ti target current is 8A, the voltage is 560V, the target base distance is 80mm, the time is 10min, and the thickness is about 200 nm. Depositing TiN on the basis of metal Ti, wherein the background vacuum is 1 multiplied by 10 < -3 > Pa, the working pressure is 0.3Pa, the argon flow is 90sccm, the nitrogen flow is 15sccm, the Ti target current is 8A, the voltage is 540V, the target base distance is 80mm, the time is 20min, and the thickness is 350 nm.
The PVD method is adopted to prepare the H storage buffer layer, and the specific parameters are as follows:
adopting pure silicon target material, firstly pre-vacuumizing to 1 × 10-3Pa; then Ar and C are introduced2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio is 5, and Ar and C are introduced in the process of the gradient layer plating2H2The flow of the mixed gas is unchanged, the mixed gas is divided into five gradients, each gradient is increased by 1A, the current of the Si target is increased from 4A to 8A, each gradient current obtains a single layer, the sputtering pressure is 0.6Pa, the heating temperature is 250 ℃, the target base distance is 80mm, and the thickness of the gradient layer is controlled to be 1.2 mu m.
Preparing a SiC hydrogen-resistant layer by adopting a radio frequency magnetron sputtering method:
using SiC target material, firstly pre-vacuumizing to 1 × 10-3Pa; then Ar is introduced, the sputtering power is 120W, the sputtering pressure is 0.3Pa, the heating temperature is 300 ℃, the target base distance is 80mm, and the total thickness is controlled at 800 nm.
The PRF of the composite coating is about 1500 in the range of 500-600 ℃ after testing.
Example 3:
plating a transition layer Ti/TiN on a base body of 304 stainless steel: the method adopting medium-frequency magnetron sputtering comprises the following steps: first plating metal Ti, setting background vacuum 1X 10-3Pa, working pressure of 0.3Pa, argon flow of 90sccm, Ti target current of 8A, voltage of 560V, target base distance of 80mm, time of 10min, and Ti layer thickness of 200 nm. Then depositing a TiN layer by using a radio frequency power supply for magnetron sputtering on the basis of metal Ti: background vacuum 1X 10-3Pa, the working pressure is 0.3Pa, the argon flow is 90sccm, the nitrogen flow is 15sccm, the sputtering power is 100-200W, the target base distance is 80mm, the time is 25min, and the thickness of the TiN layer is 450 nm.
The PVD method is adopted to prepare the H storage buffer layer, and the specific parameters are as follows:
the precursor raw material is MTS, and the carrier gas is H2(purity 99.8%), the diluent gas is argon, and the deposition temperature is lowTemperature 1150 deg.C, MTS + H2The flow rate is controlled from the first gradient of 0.4L/min, the second gradient of 0.5L/min, the third gradient of 0.6L/min, the fourth gradient of 0.7L/min, each gradient is kept for 10min, the Ar (dilution) flow rate is 160L/H, H2The flow rate of (dilution) was increased from 1L/min to 4L/min in a gradient manner to control the thickness of the obtained gradient layer to 1.1. mu.m.
Preparing a SiC hydrogen-resistant layer by adopting a radio frequency magnetron sputtering method:
using SiC target material, firstly pre-vacuumizing to 1 × 10-3Pa; then Ar is introduced, the sputtering power is 120W, the sputtering pressure is 0.3Pa, the heating temperature is 300 ℃, the target base distance is 80mm, and the total thickness is 700 nm.
The other operations were the same as in example 2.
The PRF of the composite coating is about 1500 in the range of 500-600 ℃ after testing.
Example 4:
the PVD method is adopted to prepare the H storage buffer layer, and the specific parameters are as follows:
adopting pure silicon target material, firstly pre-vacuumizing to 10 DEG-4Pa, then introducing Ar and C2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio was 5 (first gradient), the sputtering current was 10A, the sputtering gas pressure was 0.5Pa, the heating temperature was 300 ℃ and the target base distance was 80 mm. Constant Ar flow and decreasing gradient C2H2At a gas flow rate of Ar/C2H2The flow ratio is changed from 5 to 10, 4 gradients are arranged in total, and Ar/C of each gradient2H2Flow ratio of 5, 6, 8, 10, each gradient C2H2The gas flow was maintained for 20min to obtain 4 monolayers with a graded layer thickness of 1.6 μm.
The other operations were the same as in example 2.
The PRF of the composite coating is about 1400 after testing within the range of 500-600 ℃.
The above embodiments are merely illustrative of the present invention, and not restrictive, and many modifications and changes may be made by those skilled in the art without departing from the spirit of the invention, and it is intended that all such modifications and changes as fall within the true spirit of the invention and the scope of the claims be determined by those skilled in the art.
Claims (9)
1. A silicon carbide hydrogen permeation resistant coating for stainless steel is characterized by comprising a transition layer, an H storage buffer layer and a hydrogen permeation resistant layer which are arranged from a stainless steel substrate upwards layer by layer; the transition layer is composed of a metal titanium layer and a TiN layer, and the H storage buffer layer is amorphous SixC1-xX is more than 1 and more than or equal to 0.5, and the hydrogen-resistant layer is SiC;
the transition layer consists of a Ti layer and a TiN layer, wherein the Ti layer is 100-300 nm thick, the TiN layer is 200-500 nm thick, and the H storage buffer layer is amorphous SixC1-xA gradient layer, 1 > x is more than or equal to 0.5, and the thickness1-4 μm, and the thickness of the hydrogen-resistant layer is 500 nm-1 μm.
2. The silicon carbide hydrogen permeation resistant coating for stainless steel of claim 1, wherein the material of the stainless steel substrate is one of 316L, 304 and 321.
3. A method for producing a silicon carbide hydrogen permeation preventing coating for stainless steel according to claim 1 or 2, comprising the steps of:
s1 preparing Ti/TiN transition layer by magnetron sputtering method, depositing Ti layer by using Ti target as sputtering target, vacuumizing to 10%-5～10-3Pa, introducing argon gas for direct current sputtering, wherein the current is 5-8A, the working vacuum is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm; then sputtering a TiN layer by adopting an intermediate frequency power supply or a radio frequency power supply;
s2, preparing an H storage buffer layer on the transition layer by using a vapor deposition method, wherein the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method;
s3, preparing the SiC hydrogen-resistant layer on the H storage buffer layer by using a vapor deposition method, wherein the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method.
4. The method for preparing the TiN layer in the transition layer according to the claim 3, wherein the method for preparing the TiN layer in the transition layer comprises the following steps:
depositing TiN on the metal Ti layer, and pre-vacuumizing to 10 DEG-5～10-3Pa, introducing argon and nitrogen, Ar/N2The flow ratio is 2-8, medium-frequency magnetron sputtering is adopted, the current is 5-8A, the working vacuum is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm;
or in the preparation method of the transition layer, the preparation method of the TiN layer comprises the following steps: firstly, pre-vacuuming to 10-5～10-3Pa, introducing argon and nitrogen, Ar/N2The flow ratio is 2-8, the sputtering power is 100-200W, the working vacuum is 0.3-2 Pa, and the heating is carried outThe temperature is 150-300 ℃, the target base distance is 80-100mm, and the thickness is 200-500 nm.
5. The preparation method of claim 3 or 4, wherein the preparation method of the H storage buffer layer is as follows:
adopting pure silicon target material, firstly pre-vacuumizing to 10 DEG-5～10-3Pa, then introducing Ar and C2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio is 2-20, the sputtering current is 4-10A, the sputtering air pressure is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm.
6. The preparation method of claim 5, wherein in the process of plating the H storage buffer layer, the flow of Ar introduced is unchanged, and the sputtering current is increased from 4A to 10A in a gradient manner; or gradient reduction C2H2At a gas flow rate of Ar/C2H2The flow ratio is from 2 to 20, 2 to 5 gradients are arranged in total, and the sputtering current or C of each gradient2H2The gas flow is kept for 10-20 min, and 2-5 single layers are obtained.
7. The preparation method of claim 3 or 4, wherein the preparation method of the H storage buffer layer is as follows:
the precursor material is methyl trichlorosilane, and the carrier gas is H2The dilution gas is argon, the deposition temperature is 1100-1300 ℃, and MTS + H2The flow rate is increased from 0.35L/min to 0.8L/min in a gradient manner, 2-5 gradients are set in total, and each gradient is MTS + H2The flow is kept for 10-20 min, the flow of Ar of the diluent gas is 160L/H, and the flow of H of the diluent gas is kept2The flow rate was increased from a gradient of 1L/min to 4L/min.
8. The production method according to claim 3 or 4, characterized in that the SiC hydrogen-blocking layer is produced by:
adopting pure silicon target material, firstly pre-vacuumizing to 10 DEG-5～10-3Pa; then Ar and C are introduced2H2Performing medium frequency magnetron sputtering with mixed gas, Ar/C2H2The flow ratio is 2-20, the sputtering current is 4-10A, the sputtering air pressure is 0.3-0.6 Pa, the heating temperature is 150-300 ℃, and the target base distance is 80-100 mm.
9. The production method according to claim 3 or 4, characterized in that the SiC hydrogen-blocking layer is produced by:
adopting SiC target material, firstly pre-vacuumizing to 10 DEG C-5～10-3Pa, then introducing Ar, wherein the sputtering power is 120-160W, the sputtering pressure is 0.3-0.6 Pa, the heating temperature is 300-600 ℃, and the target base distance is 80-100 mm.
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