CN105525273A - Silicon carbide hydrogen permeation barrier coating for stainless steel and preparation method for silicon carbide hydrogen permeation barrier coating - Google Patents

Silicon carbide hydrogen permeation barrier coating for stainless steel and preparation method for silicon carbide hydrogen permeation barrier coating Download PDF

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CN105525273A
CN105525273A CN201510872933.4A CN201510872933A CN105525273A CN 105525273 A CN105525273 A CN 105525273A CN 201510872933 A CN201510872933 A CN 201510872933A CN 105525273 A CN105525273 A CN 105525273A
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sputtering
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张秀廷
刘雪莲
邓宁
陈步亮
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BEIJING TRX SOLAR TECHNOLOGY Co Ltd
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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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Abstract

The invention provides a silicon carbide hydrogen permeation barrier coating for stainless steel. The silicon carbide hydrogen permeation barrier coating comprises a transition layer, an H storage buffer layer and a hydrogen barrier layer which are upwards arranged layer by layer from a stainless steel substrate, wherein the transition layer is composed of a metal titanium layer and a TiN layer; the H storage buffer layer is an amorphous SixC1-x layer, wherein x is greater than or equal to 0.5, but smaller than 1, and the hydrogen barrier layer is SiC. The invention further discloses a preparation method for the silicon carbide hydrogen permeation barrier coating. According to the invention, the H storage buffer layer and the H barrier coating are combined to prepare the hydrogen permeation barrier coating with a substrate/transition layer/H storage buffer layer/SiC composite structure. Based on the radiation-resistant H barrier coating SiC film, the H storage buffer layer SixC1-x gradient layer is prepared by adopting vapor deposition technology, and the hydrogen permeation barrier property of the substrate/transition layer/H storage buffer layer/SiC composite structure is optimized by utilizing a great number of C- and Si- dangling bonds with extremely strong hydrogen catching capacity in the SixC1-x gradient layer.

Description

A kind of stainless steel silicon carbide hydrogen permeation preventing coating and preparation method thereof
Technical field
The invention belongs to the plating field to metallic substance, be specifically related to a kind of sputtering have resistance hydrogen layer metallic substance, and preparation method thereof.
Background technology
In recent years, for various body material exploitation hydrogen permeation barrier coating also known as resistance H coating, attempt to stop hydrogen and isotopic infiltration leakage thereof, carried out large quantity research both at home and abroad, mainly developed various resistance composite for hydrogen and coating technology.Conventional resistance H coating is mainly divided into following a few class at present.
Oxide coating: the advantage such as have that fusing point is high, the simple and resistance H of stable chemical nature, preparation technology is functional is the anti-hydrogen permeation coating studied the earliest.Can be generated by substrate surface direct oxidation or coating oxidation, comprise Al 2o 3, Cr 2o 3, Y 2o 3, SiO 2, Er 2o 3deng.Usual single layer oxide resistance H coating mostly is Cr 2o 3, Al 2o 3, and SiO 2normal and other coating compound use.Y 2o 3the rate of permeation of coating tritium can decline two orders of magnitude, and many and other coating compound use.Japan Atomic Energy Research Institute adopts chemical densification coating technology (CDC) to prepare Cr at 316 stainless steel surface 2o 3-SiO 2pottery hydrogen resistance coating, tritium-permeation stops that the factor (PRF) is greater than 100 (TakayukiTerai, ToshiakiYoneoka, HimhisaTanaka, Tritiumpermeationthroughausteniticstainlesssteelwithchem icallydensifiedcoatingasatritiumpermeationbarrier, JournalofNuclearMaterials, 1994:212/215:976; ).It is micron-sized a-Al that Levchuk etc. utilize PVD method to obtain thickness at Eurofer stainless steel surface 2o 3coating result shows that the PRF of coating 700 ~ 800 DEG C time is 1000 (SerraE, CalzaBiniA, CosoliG, Hydrogenpermeationmeasurementsonalumina, JournaloftheAmericanCeramicSociety, 2005,88 (1): 15).Beijing Non-Ferrous Metal Research General Academy Li Shuai etc. utilizes mocvd method to prepare Al respectively on 316L stainless steel 2o 3, Y 2o 3and Cr 2o 3resistance H coating (Journal of Inorganic Materials, 7 phase Li Shuai in 2013, the hydrogen penetrating quality of He Di, Liu Xiaopeng, Zhang Chao, Wang Shumao, Yu Qinghe, Qiu Haochen, Jiang Lijun, 316L stainless steel base aluminum oxide coating layer, Journal of Inorganic Materials, 2013,28 (7) 775; ), NdFeB permanent magnets is excellent.Wherein Al 2o 3coating is 59 ~ 119 to the 316L stainless hydrogen permeation barrier factor (PRF) 600 ~ 700 DEG C time.Y 2o 3coating PRF 550 ~ 700 DEG C time is 240-410.Cr 2o 3coating PRF 550 ~ 600 DEG C time is 24 ~ 117.
The erosion resistance that Ti base ceramic coating tool is good and higher resistance H effect.This type coating mainly comprises titanium nitride, titanium carbide and both compounds or mixed coating, and various titanium-base ceramics coating all can adopt the method for CVD or PVD to prepare, and result of study shows, Ti base ceramic coating has well resistance H performance at low temperatures.Utilize PVD method to prepare on the 316L stainless steel-based end TiC+TiN coating (C.Q.Shang that thickness is 2 ~ 5 microns such as mountain Chang Qi, A.J.Wu, Y.J.Li, Thebehaviourofdiffusionandpermeationoftritiumthrough316L stainlesssteelwithcoatingofTiCandTiN+TiC, JournalofNuclearMaterials, 1992,191-194:221; ), then utilize thermo-chemical treatment to prepare one deck CH4 hydrogen permeation preventing coating on TiC surface.Test result shows hydrogen permeability reduction in the coating 4-6 order of magnitude.But oxidation occurs more than 450 DEG C of temperature for TiC, TiN and TiC/TiN is difficult to overcome.Yao Zhenyu etc. add the higher coating of one deck oxidation-resistance (SiO2 or TiN) on TiN+TiC gradient cladding surface and in use to lose efficacy (Yao Zhenyu to prevent TiN+TiC gradient cladding, the anti-tritium diffusion performance study of fusion reactor blanket material different coating, China Atomic Energy Science Research Institute master Diplomarbeit, 2001).On the 316L stainless steel-based end, TiN+TiC+TiN and TiN+TiC+SiO is prepared by PVD method 2coating.Coat-thickness is respectively 2 microns and 3 microns.Two kinds of coating penetration rates reduce 4 ~ 5 and 4 ~ 6 orders of magnitude respectively relative to base material.
Silicide coating mainly concentrates on SiC coating.SiC is the silicide resistance H permeation coating of current most study, and is industrially applied, and reason is that it has high hardness and wear resisting property, can use as superhard coating.First react with oxygen during SiC high temperature and generate the very thin fine and close SiO of one deck 2passive film, makes SiC have good high temperature oxidation resistance, and SiC can be stoped to continue oxidation.Preparation SiC coating adopts CVD and PVD method usually.Wang Peixuan etc. utilize ion-beam assisted deposition and ion implantation deposited on 316L stainless steel thickness be 2 microns SiC coating (Wang Peixuan, Wang Yu, history is valuable, stainless steel surface deposition SiC is as the research of hydrogen penetration barrier layer, Acta Metallurgica Sinica, 1999,35 (6): 654; ).Coating make the stainless steel-based end nearly 5 orders of magnitude of hydrogen permeability reduction.The people such as Chikada have prepared SiC with radio-frequency magnetron sputter method and have hindered H coating (ChikadaT on 316 and the F82H stainless steel-based end, SuzukiA, TeraiT, Deuteriumpermeationandthermalbehaviorsofamorphoussilicon carbidecoatingsonsteels, Fu-sionEngineeringandDesign, 2011,86 (9): 2192), have studied resistance H performance and the thermostability of SiC coating.Result of study shows, the SiC film of preparation is non-crystalline state.Within the scope of 450 ~ 550 DEG C, PRF is about 1000.When temperature is more than 600 DEG C, resistance H effect can decline to some extent, and reason is that temperature too high SiC inside generation tiny crack causes H to permeate aggravation.China Engineering Physics Research Institute adopts Er2O3/SiC compound coating to improve the stainless anti-H penetrating quality of 316L, thickness is that 300nm rete can reach 500 (Yao Zhenyu by PRF under 500 DEG C of conditions, Yan Hui, Tan Liwen, Han Hua, does the research of Tritium Permeation Barrier, NuclearFusionandPlasmaPhysics with SiC film, 2002,22:65; ).
Aluminide compound coating mainly comprises A1/Fe+Al 2o 3with AlN coating, by causing a concentration gradient containing aluminium at substrate metal near surface, forming an aluminum based metal compound layer, can graded be 30%-80%Al by the aluminium content of matrix metal to surfaces of aluminum content.Due to the difference of thermal expansivity between matrix and coated material, cause aluminide coating easily to come off, this is the technical barrier faced at present.In cold and hot change procedure, difference of thermal expansion coefficients is larger, and the stress of generation is also larger.This cold and hot process iterative cycles, the effect of stress just can be accumulated and constantly strengthen, and likely cracks, until coating shedding.Preparation A1/Fe+Al 2o 3the method of resistance H coating has hot dip process, flame plating, vacuum plasma spray, ion implantation, chemical vapour deposition, magnetron sputtering, hot isostatic pressing and pack cementation aluminizing etc.Crl8Nil0Ti austenitic stainless steel is put into 10%Al+90%Li melt at 600 ~ 800 DEG C of temperature range aluminising 5 ~ 100h by Kalin etc., the coating obtained has complicated intermetallic compound heterogeneous structure, as FeAl3, FeAl, Fe3Al and NiAl, AlCr2 and a-Fe etc., thickness is different because temperature and time is different.Result of study shows, the blocking effect of two sides aluminising is best, PRF is respectively 2000 and 2700 (B.A.Kalin, V.L.Yakushin, E.P.Fomina, Tritiumbarrierdevelopmentforaustenitiestainlesssteelbyit saluminizinginalithiummelt, FusionEngineeringandDesign1998,41:119; ).Fazio etc. have utilized air plasma spraying legal system for Fe-Cr-Al coating, MANETII and F has been selected in substrate respectively 82h 2mod steel.Coating possesses certain resistance H penetrating power, but there is larger unrelieved stress between coating and substrate, coating is made in use easily to peel off (FazioC, Stein-FechnerK, SerraE, InvestigationonthesuitabilityofplasmasprayedFe-Cr-Alcoat ingsastritiumpermeationbarrier, JNuclearMaterial1999,273:233).Chen Yin etc. utilize PECVD technology (silver old, Chen Changan, Zhang Pengcheng, PECVD prepare the research of Al-Al2O3 compound hydrogen resistance coating, sufacing, 2008,37 (3): 41; ) even, fine and close, stable Al-Al can be obtained after Vacuum Heat oxide treatment 2o 3laminated film, but there is a small amount of carbide impurity.It is obvious that film hinders deuterium performance below 450 DEG C, and the resistance H factor can reach 244.
Novel resistance H material: in recent years, the resistance H performance of Graphene and BN attracts wide attention, and has emerged in large numbers a large amount of resistance H material system based on BN and Graphene.The magneticallyenhancedplasma-ion-plating such as Tamura obtains BN coating on the 316L stainless steel-based end, coat-thickness is 1.5 microns, after 316L stainless steel surface is coated with BN coating, effectively can reduce stainless H infiltration rate, 300 ~ 500 DEG C of scopes are interior, the PRF value of BN is 100 (M.Tamuraa, M.Nomab, M.Yamashitac, Characteristicchangeofhydrogenpermeationinstainlesssteel platebyBNcoating, SurfaceandCoatingsTechnology, 2014,260:148; ).
Although the research of resistance H coating has obtained many progress in material system design, performance optimization and mechanism etc., and in engineering in fact also existing application.But current research finds, for the hydrogen atom of " fine ", resistance H excellent performance coating---corundum Atom gap is so big, to such an extent as to hydrogen atom, and can form much small hole in metallic matrix side wherein casual " migration ".Along with continuous " the growing up " in hole, hydrogen atom has enough space recombine and forms hydrogen molecule and produce pressure to oxide film.When the diameter of cheating arrives greatly a certain critical size, oxide film will be supportted viscous deformation occurs, and bulges formation bubble, destroy the effect (D.G.Xie of resistance H coating, Z.J.Wang, J.Sun, J.Li, E.Ma, Z.W.Shan, Insitustudyoftheinitiationofhydrogenbubblesatthealuminiu mmetal/oxideinterface, NatureMaterials, 2015,10.1038:4336).In addition, current research also shows, hydrogen can relatively easily pass through the two-dimensional material such as Graphene and BN, and heats up and add catalyzer and can significantly accelerate this process, this means that the resistance H thinking that hydrogen that traditional view is thought cannot penetrate not containing the two-dimensional material such as Graphene of defect is also unworkable.
(Algara-Siller,G.O.Lehtinen,F.C.Wang,R.R.Nair,U.Kaiser,H.A.Wu,A.K.Geim,I.V.Grigorieva,Squareiceingraphenenanocapillaries,Nature,2015,519(7544):443)
Meanwhile, in recent years, making great progress with research as Hydrogen Technology exploitation that is clean, high efficient energy sources, providing important references for solving anti-hydrogen infiltration problem.In a word, these new cognitions and discovery to much to relate to hydrogen and apply relevant unsolved mystery and provide important reference.Therefore, carry out performance regulation and control and the study mechanism of anti-hydrogen infiltration compound coating, the controllability of the resistance H coating that instructs anti-hydrogen penetration material System Design and correlation technique to develop, optimize the performance of resistance H coating, improves, has become the study hotspot relating to hydrogen Application Areas.
Summary of the invention
For overcoming the above-mentioned defect of prior art, the object of this invention is to provide a kind of hydrogen permeation preventing coating be made up of matrix/transition layer/storage H buffer layer/SiC composite structure.
Another object of the present invention is the preparation method proposing described hydrogen permeation preventing coating.
The technical scheme realizing the object of the invention is:
A kind of stainless steel silicon carbide hydrogen permeation preventing coating, comprises transition layer, storage H buffer layer, the resistance hydrogen layer upwards successively arranged from stainless steel base; Described transition layer is made up of layer of titanium metal and TiN layer, and described graded bedding is amorphous Si xc 1-x, 1 > x>=0.5, described resistance hydrogen layer is SiC.
Wherein, described transition layer is made up of Ti layer and TiN layer, wherein Ti thickness 100 ~ 300nm, the thick 200 ~ 500nm of TiN layer, and described storage H buffer layer is amorphous Si xc 1-xgraded bedding, 1 > x>=0.5, thickness 1 ~ 4 μm, described resistance hydrogen layer thickness is 500nm ~ 1 μm.
Wherein, the material of described stainless steel base is the one in 316L, 304 and 321.
The preparation method of stainless steel silicon carbide hydrogen permeation preventing coating of the present invention, is characterized in that, comprise the following steps:
S1 uses the method for magnetron sputtering to prepare transition layer Ti/TiN, first with Ti target for sputtering target material metal refining Ti layer, first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and carries out d.c. sputtering, and electric current is 5 ~ 8A, and working vacuum is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm; Then intermediate frequency power supply or radio-frequency power supply sputtering TiN layer is adopted;
S2 uses vapour deposition process to prepare storage H buffer layer on transition layer, and described vapour deposition process is physical vaporous deposition or chemical Vapor deposition process;
S3 uses vapour deposition process to prepare SiC resistance hydrogen layer on storage H buffer layer, and described vapour deposition process is physical vaporous deposition or chemical Vapor deposition process.
Wherein, in transition layer described in S1, the preparation method of TiN layer is:
Depositing TiN on metal Ti layer, first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and nitrogen, Ar/N 2throughput ratio is 2-8, and adopt medium frequency magnetron sputtering (employing intermediate frequency power supply), electric current is 5 ~ 8A, and working vacuum is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm.
Or in S1, the preparation method of TiN layer is: first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and nitrogen, Ar/N 2throughput ratio is 2-8, and sputtering power is 100 ~ 200W (employing radio-frequency power supply), and working vacuum is 0.3Pa ~ 2Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm, and thickness is 200 ~ 500nm.
Wherein, the preparation method storing up H buffer layer in S2 is:
Adopt pure silicon target, first forvacuum to 10 -5~ 10 -3pa, then passes into Ar and C 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 2 ~ 20, and sputtering current is 4 ~ 10A, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, target-substrate distance 80-100mm.
Preferably, in the process that graded bedding is coated with, the Ar flow passed into is constant, and gradient increases sputtering current from 4A to 10A, or gradient reduces C 2h 2gas flow, make Ar/C 2h 2throughput ratio, from 2 to 20, arranges 2 ~ 5 gradients altogether, and each gradient sputtering current keeps 10 ~ 20min, obtains an individual layer and controls total thickness at 1 ~ 4 μm.
Or the preparation method storing up H buffer layer described in S2 is:
Precursor raw material is METHYL TRICHLORO SILANE, and carrier gas is H 2, diluent gas is argon gas, depositing temperature 1100 ~ 1300dEG C, MTS+H 2flow rises to 0.8L/min from 0.35L/min gradient, carrier gas Ar flow 160L/h, carrier gas H 2flow rises to 4L/min from 1L/min gradient, arranges 2 ~ 5 gradients altogether, each gradient MTS+H 2flow keeps 10 ~ 20min.
Diluent gas is the working gas in CVD, does not participate in reaction.Hydrogen together with MTS is carrier gas, the effect of carrier gas enters vacuum chamber together with certain flow velocity carrier band gaseous sample or the sample gas after gasification, enter together so the hydrogen serving as carrier gas is same MTS, and the hydrogen serving as diluent gas enters from another one inlet mouth.
Wherein, the preparation method of the resistance of SiC described in S3 hydrogen layer is:
Adopt pure silicon target, first forvacuum to 10 -5~ 10 -3pa; Then Ar and C is passed into 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 2 ~ 20, and sputtering current is 4 ~ 10A, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, target-substrate distance 80 ~ 100mm.
Or the preparation method that SiC described in S3 hinders hydrogen layer is:
Adopt SiC target material, first forvacuum to 10 -5~ 10 -3pa; Then pass into Ar, sputtering power is 120 ~ 160W, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 300 ~ 600 DEG C, target-substrate distance 80 ~ 100mm.
Beneficial effect of the present invention is:
SiC is the silicide resistance H permeation coating of current most study, and is industrially applied, and reason is that it has high hardness and wear resisting property, can use as superhard coating.First react with oxygen during SiC high temperature and generate the very thin fine and close SiO of one deck 2passive film, makes SiC have good high temperature oxidation resistance, and SiC can be stoped to continue oxidation.In addition, amorphous Si xC 1-xcontaining a large amount of C-and Si-dangling bonds in film, the effect of storage H can be played.The two combines, and not only plays the effect of resistance H infiltration, and more the part H hindering H layer through SiC can be fixed further, and be the combination of chemical bond, such combination is stronger, can play the effect of anti-hydrogen infiltration.
Based on the series of challenges that resistance H coating faces in actual applications, in previous work, we have carried out pre-exploration targetedly.Not only from the low-temperature epitaxy mechanism of theoretical side research SiC film, structure and the delay of tritium, the relation of diffus-sion and permeation and mechanism thereof.Simultaneously, in conjunction with surface treatment and the buffer layer of matrix, well below under the stainless tempering temperature of 316L, complex-shaped matrix surface obtain thickness evenly, combine firmly SiC film, structured testing shows that SiC film has excellent Flouride-resistani acid phesphatase, anti-tritium diffusion performance.
The present invention proposes to combine with resistance H coating with storage H buffer layer, prepares the anti-hydrogen permeability coating of matrix/transition layer/storage H buffer layer/SiC composite structure.On the resistance H coating SiC Membranous Foundations of Flouride-resistani acid phesphatase, adopt gas phase deposition technology preparation storage H buffer layer Si xc 1-xgraded bedding, utilizes Si xc 1-xvery competent C-and Si-of a large amount of seizure hydrogen existed in graded bedding hangs key, optimizes the anti-hydrogen penetrating quality of matrix/transition layer/storage H buffer layer/SiC composite structure, improves its controllability.
Accompanying drawing explanation
Fig. 1 is coating structure figure of the present invention.
Embodiment
Following embodiment for illustration of the present invention, but should not be construed as limitation of the present invention.
The equipment of magnetron sputtering is TRX-750 vacuum magnetic-control sputtering equipment, starlight thermal technology development corporation, Ltd. of Beijing Tianrui system.The unit type of chemical vapour deposition is NEE-4000 (M) electron beam evaporation system, and that Nuo Zhong Co., Ltd produces.
In embodiment, if no special instructions, technique means used is the technique means of this area routine.
Embodiment 1:
Select to be coated with transition layer Ti/TiN on the matrix of austenitic stainless steel 316 L, adopt the method preparation of medium frequency magnetron sputtering, be first coated with metal Ti, base vacuum 1 × 10 is set -3pa, operating air pressure 0.6Pa, argon flow amount 120sccm, Ti target current 8A, voltage 550V, target-substrate distance is 80mm, time 10min, obtained that titanium layer thickness is about 200nm.Depositing TiN on the basis of metal Ti, base vacuum 1 × 10 -3pa, operating air pressure 0.6Pa, argon flow amount 120sccm, nitrogen flow 15sccm, Ti target current 8A, voltage 530V, target-substrate distance is 80mm, time 20min, and thickness is about 350nm.
Adopt CVD preparation storage H buffer layer, design parameter is as follows:
Precursor raw material is MTS, and carrier gas is H 2(its purity 99.8%), diluent gas is argon gas, depositing temperature 1100 DEG C, MTS+H 2flow is from the first gradient 0.35L/min, and the second gradient 0.45L/min, the 3rd gradient 0.6L/min, the 4th gradient 0.8L/min, rises to 0.8L/min, and each gradient stops 15min, Ar (dilution) flow 160L/h, H 2(dilution) flow rises to 4L/min from 1L/min gradient, controls the graded layer thickness 1.5 μm obtained.
Adopt chemical Vapor deposition process to prepare SiC and hinder hydrogen layer: adopt trichloromethyl silane (MTS) to be raw material, processing condition are: temperature 1100 DEG C, MTS+H 2flow 0.3L/min, H 2(dilution) flow 0.5L/min, Ar flow 0.8L/min; Furnace pressure 3kPa, obtained SiC hinders hydrogen layer thickness 1 μm.
The hydrogen permeation preventing coating structure that the present embodiment obtains is as Fig. 1, and from transition layer, storage H buffer layer, resistance hydrogen layer that stainless steel base is upwards successively arranged, through test, this compound coating PRF within the scope of 500 ~ 600 DEG C is 1500.
Embodiment 2:
Select to be coated with transition layer Ti/TiN on the matrix of austenitic stainless steel 316 L, adopt the method preparation of medium frequency magnetron sputtering, first metal Ti is coated with, base vacuum 1 × 10-3Pa, operating air pressure 0.3Pa, argon flow amount 90sccm, Ti target current 8A, voltage 560V, target-substrate distance is 80mm, time 10min, thickness is about 200nm.Depositing TiN on the basis of metal Ti, base vacuum 1 × 10-3Pa, operating air pressure 0.3Pa, argon flow amount 90sccm, nitrogen flow 15sccm, Ti target current 8A, voltage 540V, target-substrate distance is 80mm, time 20min, and thickness is 350nm.
Adopt PVD legal system standby storage H buffer layer, design parameter is as follows:
Adopt pure silicon target, first forvacuum to 1 × 10 -3pa; Then Ar and C is passed into 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 5, in the process that graded bedding is coated with, Ar and C passed into 2h 2mixed gas flow is constant, and the electric current dividing five gradients, each gradient to increase 1A, Si target is increased to 8A from 4A, and each gradient current obtains an individual layer, and sputtering pressure is 0.6Pa, and Heating temperature is 250 DEG C, target-substrate distance 80mm, controls graded layer thickness at 1.2 μm.
Adopt radio-frequency magnetron sputter method to prepare SiC and hinder hydrogen layer:
Adopt SiC target material, first forvacuum to 1 × 10 -3pa; Then pass into Ar, sputtering power is 120W, and sputtering pressure is 0.3Pa, and Heating temperature is 300 DEG C, and target-substrate distance 80mm, total thickness controls at 800nm.
Compound coating is through test, and within the scope of 500 ~ 600 DEG C, PRF is about 1500.
Embodiment 3:
304 stainless matrixes are coated with transition layer Ti/TiN: adopt the method for medium frequency magnetron sputtering: be first coated with metal Ti, base vacuum 1 × 10 is set -3pa, operating air pressure 0.3Pa, argon flow amount 90sccm, Ti target current 8A, voltage 560V, target-substrate distance is 80mm, and time 10min, Ti layer thickness is 200nm.Then on the basis of metal Ti, radio-frequency power supply magnetron sputtering deposition TiN layer is used: base vacuum 1 × 10 -3pa, operating air pressure 0.3Pa, argon flow amount 90sccm, nitrogen flow 15sccm, sputtering power is 100 ~ 200W, and target-substrate distance is 80mm, time 25min, and TiN layer thickness is 450nm.
Adopt PVD legal system standby storage H buffer layer, design parameter is as follows:
Precursor raw material is MTS, and carrier gas is H 2(its purity 99.8%), diluent gas is argon gas, depositing temperature 1150 DEG C, MTS+H 2flow is from the first gradient 0.4L/min, and the second gradient 0.5L/min, the 3rd gradient 0.6L/min, the 4th gradient 0.7L/min, each gradient stops 10min, Ar (dilution) flow 160L/h, H 2(dilution) flow rises to 4L/min from 1L/min gradient, controls the graded layer thickness 1.1 μm obtained.
Adopt radio-frequency magnetron sputter method to prepare SiC and hinder hydrogen layer:
Adopt SiC target material, first forvacuum to 1 × 10 -3pa; Then pass into Ar, sputtering power is 120W, and sputtering pressure is 0.3Pa, and Heating temperature is 300 DEG C, target-substrate distance 80mm, and total thickness is 700nm.
Other operations are with embodiment 2.
Compound coating is through test, and within the scope of 500 ~ 600 DEG C, PRF is about 1500.
Embodiment 4:
Adopt PVD legal system standby storage H buffer layer, design parameter is as follows:
Adopt pure silicon target, first forvacuum to 10 -4pa, then passes into Ar and C 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 5 (first gradient), and sputtering current is 10A, and sputtering pressure is 0.5Pa, and Heating temperature is 300 DEG C, target-substrate distance 80mm.Ar flow is constant, and gradient reduces C 2h 2gas flow, make Ar/C 2h 2throughput ratio fades to 10 from 5, arranges 4 gradients altogether, the Ar/C of each gradient 2h 2throughput ratio is 5,6,8,10, each gradient C 2h 2gas flow keeps 20min, and obtain 4 individual layers, graded layer thickness is 1.6 μm.
Other operations are with embodiment 2.
Compound coating is through test, and within the scope of 500 ~ 600 DEG C, PRF is about 1400.
Above embodiment is only be described the specific embodiment of the present invention; not scope of the present invention is limited; those skilled in the art also can do numerous modifications and variations on the basis of existing technology; under not departing from the present invention and designing the prerequisite of spirit; the various modification that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.

Claims (10)

1. a stainless steel silicon carbide hydrogen permeation preventing coating, is characterized in that, comprises transition layer, storage H buffer layer, the resistance hydrogen layer upwards successively arranged from stainless steel base; Described transition layer is made up of layer of titanium metal and TiN layer, and described storage H buffer layer is amorphous Si xc 1-x, 1 > x>=0.5, described resistance hydrogen layer is SiC.
2. stainless steel silicon carbide hydrogen permeation preventing coating according to claim 1, it is characterized in that, described transition layer is made up of Ti layer and TiN layer, wherein Ti thickness 100 ~ 300nm, the thick 200 ~ 500nm of TiN layer, and described storage H buffer layer is amorphous Si xc 1-xgraded bedding, 1 > x>=0.5, thickness 1 ~ 4 μm, described resistance hydrogen layer thickness is 500nm ~ 1 μm.
3. stainless steel silicon carbide hydrogen permeation preventing coating according to claim 1, is characterized in that, the material of described stainless steel base is the one in 316L, 304 and 321.
4. the preparation method of the arbitrary described stainless steel silicon carbide hydrogen permeation preventing coating of claims 1 to 3, is characterized in that, comprise the following steps:
S1 uses the method for magnetron sputtering to prepare transition layer Ti/TiN, first with Ti target for sputtering target material metal refining Ti layer, first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and carries out d.c. sputtering, and electric current is 5 ~ 8A, and working vacuum is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm; Then intermediate frequency power supply or radio-frequency power supply sputtering TiN layer is adopted;
S2 uses vapour deposition process to prepare storage H buffer layer on transition layer, and described vapour deposition process is physical vaporous deposition or chemical Vapor deposition process;
S3 uses vapour deposition process to prepare SiC resistance hydrogen layer on storage H buffer layer, and described vapour deposition process is physical vaporous deposition or chemical Vapor deposition process.
5. preparation method according to claim 4, is characterized in that, in described transition layer, the preparation method of TiN layer is:
Depositing TiN on metal Ti layer, first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and nitrogen, Ar/N 2throughput ratio is 2 ~ 8, and adopt medium frequency magnetron sputtering, electric current is 5 ~ 8A, and working vacuum is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm;
Or in the preparation method of described transition layer, the preparation method of TiN layer is: first forvacuum to 10 -5~ 10 -3pa, passes into argon gas and nitrogen, Ar/N 2throughput ratio is 2 ~ 8, and sputtering power is 100 ~ 200W, and working vacuum is 0.3Pa ~ 2Pa, and Heating temperature is 150 ~ 300 DEG C, and target-substrate distance is 80 ~ 100mm, and thickness is 200 ~ 500nm.
6. the preparation method according to claim 4 or 5, is characterized in that, the preparation method of described storage H buffer layer is:
Adopt pure silicon target, first forvacuum to 10 -5~ 10 -3pa, then passes into Ar and C 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 2 ~ 20, and sputtering current is 4 ~ 10A, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, target-substrate distance 80 ~ 100mm.
7. preparation method according to claim 6, is characterized in that, in the process that storage H buffer layer is coated with, the Ar flow passed into is constant, and sputtering current is increased to 10A from 4A gradient; Or gradient reduces C 2h 2gas flow, make Ar/C 2h 2throughput ratio, from 2 to 20, arranges 2 ~ 5 gradients, the sputtering current of each gradient or C altogether 2h 2gas flow keeps 10 ~ 20min, obtains 2 ~ 5 individual layers.
8. the preparation method according to claim 4 or 5, is characterized in that, the preparation method of described storage H buffer layer is:
Precursor raw material is METHYL TRICHLORO SILANE, and carrier gas is H 2, diluent gas is argon gas, depositing temperature 1100 ~ 1300 DEG C, MTS+H 2flow rises to 0.8L/min from 0.35L/min gradient, arranges 2 ~ 5 gradients altogether, each gradient MTS+H 2flow keeps 10 ~ 20min, carrier gas Ar flow 160L/h, carrier gas H 2flow rises to 4L/min from 1L/min gradient.
9. the preparation method according to claim 4 or 5, is characterized in that, the preparation method that described SiC hinders hydrogen layer is:
Adopt pure silicon target, first forvacuum to 10 -5~ 10 -3pa; Then Ar and C is passed into 2h 2mixed gas carries out medium frequency magnetron sputtering, Ar/C 2h 2throughput ratio is 2 ~ 20, and sputtering current is 4 ~ 10A, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 150 ~ 300 DEG C, target-substrate distance 80 ~ 100mm.
10. the preparation method according to claim 4 or 5, is characterized in that, the preparation method that described SiC hinders hydrogen layer is:
Adopt SiC target material, first forvacuum to 10 -5~ 10 -3pa, then passes into Ar, and sputtering power is 120 ~ 160W, and sputtering pressure is 0.3Pa ~ 0.6Pa, and Heating temperature is 300 ~ 600 DEG C, target-substrate distance 80 ~ 100mm.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106283052A (en) * 2016-08-23 2017-01-04 北京航空航天大学 A kind of two-dimensional material regulation and control silicon-carbon composite construction hydrogen resistance coating and preparation method thereof
CN107217281A (en) * 2017-05-26 2017-09-29 华中科技大学 A kind of NEW TYPE OF COMPOSITE resistance tritium coating and preparation method thereof
CN109699114A (en) * 2019-02-18 2019-04-30 中国科学院合肥物质科学研究院 A kind of MULTILAYER COMPOSITE neutron-producing target and preparation method thereof
CN112647055A (en) * 2020-11-13 2021-04-13 中国科学院金属研究所 Chemical vapor deposition method for preparing silicon carbide composite coating on monocrystalline silicon or polycrystalline silicon
CN114657509A (en) * 2022-03-25 2022-06-24 西安交通大学 Ceramic-metal multilayer composite coating resistant to corrosion of liquid lead-bismuth alloy and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002336665A (en) * 2001-05-14 2002-11-26 Japan Steel Works Ltd:The Hydrogen-permeable membrane
JP2005066427A (en) * 2003-08-21 2005-03-17 Ishikawajima Harima Heavy Ind Co Ltd Hydrogen separation sheet and method for producing the same
US20090191417A1 (en) * 2008-01-25 2009-07-30 Oerlikon Trading Ag, Truebbach Permeation barrier layer
WO2011119469A1 (en) * 2010-03-22 2011-09-29 T3 Scientific Llc Hydrogen selective protective coating, coated article and method
CN104004992A (en) * 2014-05-27 2014-08-27 江苏科技大学 Stainless steel hydrogen-permeation-barrier composite film and preparation method thereof
CN104561891A (en) * 2015-01-30 2015-04-29 四川大学 Double-component gradient hydrogen permeation barrier coating and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002336665A (en) * 2001-05-14 2002-11-26 Japan Steel Works Ltd:The Hydrogen-permeable membrane
JP2005066427A (en) * 2003-08-21 2005-03-17 Ishikawajima Harima Heavy Ind Co Ltd Hydrogen separation sheet and method for producing the same
US20090191417A1 (en) * 2008-01-25 2009-07-30 Oerlikon Trading Ag, Truebbach Permeation barrier layer
WO2011119469A1 (en) * 2010-03-22 2011-09-29 T3 Scientific Llc Hydrogen selective protective coating, coated article and method
CN104004992A (en) * 2014-05-27 2014-08-27 江苏科技大学 Stainless steel hydrogen-permeation-barrier composite film and preparation method thereof
CN104561891A (en) * 2015-01-30 2015-04-29 四川大学 Double-component gradient hydrogen permeation barrier coating and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106283052A (en) * 2016-08-23 2017-01-04 北京航空航天大学 A kind of two-dimensional material regulation and control silicon-carbon composite construction hydrogen resistance coating and preparation method thereof
CN106283052B (en) * 2016-08-23 2019-01-25 北京航空航天大学 A kind of two-dimensional material regulation silicon-carbon composite construction hydrogen resistance coating and preparation method thereof
CN107217281A (en) * 2017-05-26 2017-09-29 华中科技大学 A kind of NEW TYPE OF COMPOSITE resistance tritium coating and preparation method thereof
CN109699114A (en) * 2019-02-18 2019-04-30 中国科学院合肥物质科学研究院 A kind of MULTILAYER COMPOSITE neutron-producing target and preparation method thereof
CN112647055A (en) * 2020-11-13 2021-04-13 中国科学院金属研究所 Chemical vapor deposition method for preparing silicon carbide composite coating on monocrystalline silicon or polycrystalline silicon
CN112647055B (en) * 2020-11-13 2021-09-24 中国科学院金属研究所 Chemical vapor deposition method for preparing silicon carbide composite coating on monocrystalline silicon or polycrystalline silicon
CN114657509A (en) * 2022-03-25 2022-06-24 西安交通大学 Ceramic-metal multilayer composite coating resistant to corrosion of liquid lead-bismuth alloy and preparation method thereof

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