CN103802385A - Stainless steel based hydrogen permeation prevention composite coating - Google Patents
Stainless steel based hydrogen permeation prevention composite coating Download PDFInfo
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- CN103802385A CN103802385A CN201210449522.0A CN201210449522A CN103802385A CN 103802385 A CN103802385 A CN 103802385A CN 201210449522 A CN201210449522 A CN 201210449522A CN 103802385 A CN103802385 A CN 103802385A
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- stainless steel
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- composite coating
- oxide layer
- resistant composite
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 64
- 239000001257 hydrogen Substances 0.000 title claims abstract description 64
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000011248 coating agent Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 33
- 239000010935 stainless steel Substances 0.000 title claims abstract description 32
- 230000002265 prevention Effects 0.000 title abstract 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 239000011029 spinel Substances 0.000 claims abstract description 5
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 5
- 230000008595 infiltration Effects 0.000 claims description 41
- 238000001764 infiltration Methods 0.000 claims description 41
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 31
- 239000011572 manganese Substances 0.000 claims description 25
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 23
- 229910052748 manganese Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 13
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000007750 plasma spraying Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 3
- QDLZHJXUBZCCAD-UHFFFAOYSA-N [Cr].[Mn] Chemical compound [Cr].[Mn] QDLZHJXUBZCCAD-UHFFFAOYSA-N 0.000 abstract 3
- 239000010410 layer Substances 0.000 description 52
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000010963 304 stainless steel Substances 0.000 description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052722 tritium Inorganic materials 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000003904 radioactive pollution Methods 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a stainless steel based hydrogen permeation prevention composite coating. A stainless steel base body is provided with a hydrogen permeation prevention composite coating which is composed of a chromic oxide layer, a manganese chromium spinel layer and an aluminium oxide layer on the surface of the stainless steel base body from inward to outward, wherein the chromic oxide layer and the manganese chromium spinel layer on the surface of the stainless steel base body is obtained by in-situ oxidation of the surface of the stainless steel base body; the aluminum oxide layer is directly deposited on the surfaces of the chromic oxide layer and the manganese chromium spinel layer. The hydrogen permeation prevention composite coating disclosed by the invention has excellent hydrogen permeation prevention performance and thermal shock performance, and can be widely applied to hydrogen permeation prevention coatings of structural materials and devices in the field with hydrogen involvement.
Description
Technical field
This method relates to a kind of stainless steel-based hydrogen infiltration-resistant composite coating, and this composite coating can be widely used in relating to the hydrogen permeation preventing coating of structural material and device in hydrogen field.
Background technology
Relate to the application of hydrogen as all there is the problem of hydrogen diffusion and infiltration in the storage of hydrogen, use procedure.At solar energy thermal-power-generating, with in thermal-collecting tube, the infiltration of hydrogen and separate out the increase that enrichment meeting causes heat collecting pipe heat waste to lose, reduces the generating efficiency of thermal-collecting tube.In fusion reactor, the stainless steel pipeline in tritium propagation covering is in compared with elevated operating temperature, and its tritium-permeation rate can significantly raise, and causes infiltration and the leakage of tritium fuel, reduces the commercial value of thermonuclear fusion heap and causes radioactive pollution.To relate to hydrogen in hydrogen application and permeate the problem of bringing in order to solve, can prepare the method raising material of permeation barrier coating or the hydrogen infiltration-resistant performance of device on structural material surface by adopting.In all kinds of coating materials, pottery possesses that hydrogen permeability is low, Heat stability is good, corrosion resistance are good and mechanical hardness advantages of higher, is the preferred material of hydrogen permeation preventing coating.
At present, the ceramic hydrogen permeation preventing coating material having conducted a research mainly contains TiN, TiN/TiC, SiC, Er
2o
3, ZrO
2, Al
2o
3, Cr
2o
3deng.Wherein, aluminium oxide has excellent hydrogen infiltration-resistant performance, chemical stability and decay resistance etc., and its hydrogen infiltration reduces the factor up to 10
3, be confirmed as one of most potential hydrogen permeation preventing coating material [J.Nucl.Mater.328 (2004) 103].In addition, CN101469409A, CN101265603A, CN101845645A have announced the hydrogen permeation preventing coating that adopts Al prepared by distinct methods or Fe/Al alloy-layer and alumina layer compound.This type of hydrogen infiltration-resistant composite coating has good binding ability to matrix, and composite coating also has the ability of self-regeneration to the alumina layer micro-crack that may form in use procedure, therefore becomes one of study hotspot of hydrogen permeation preventing coating in the last few years.Although Al or Fe/Al alloy-layer and aluminium oxide hydrogen infiltration-resistant composite coating have advantage as above, the preparation of Al or Fe/Al alloy-layer relates to metal level and applies and high-temperature post-treatment, complicated process of preparation, and cost is high.
Summary of the invention
The object of this invention is to provide a kind of stainless steel base hydrogen infiltration-resistant composite coating.This composite coating combines the hydrogen infiltration-resistant performance of chromium oxide layer and alumina layer, has that preparation technology of coating is simple, the feature of hydrogen infiltration-resistant excellent performance.
For achieving the above object, the present invention adopts following technical scheme:
A kind of stainless steel hydrogen infiltration-resistant composite coating has hydrogen infiltration-resistant composite coating on stainless steel base, and this hydrogen infiltration-resistant composite coating is made up of chromium oxide layer, manganese picotite layer and the alumina layer of stainless steel-based surface respectively from the inside to the outside.
Chromium oxide layer, the manganese picotite layer of described stainless steel-based surface are obtained by stainless steel in-situ oxidation.
Described manganese picotite is by the Mn with spinel structure
xcr
yo
4oxide forms, wherein 1≤x≤2,1≤y≤2, and 2≤x+y≤3.
The resistance hydrogen of chromium oxide layer is functional, and the preparation technology that stainless steel surfaces in-situ oxidation obtains chromium oxide layer is simple, ripe.Research shows, it is not single chromium oxide that the oxidation of stainless steel base surface in situ obtains chromium oxide layer composition, and oxide layer forms [Chinese Marine University's journal, 41 (2011) 267] by fine and close chromium oxide layer and manganese picotite layer respectively outside interior.The hydrogen infiltration-resistant performance of coating is provided by fine and close chromium oxide layer, and it is 10-10 that the hydrogen infiltration of chromium oxide layer reduces the factor
2.Therefore, the compound hydrogen permeation preventing coating of chromium oxide layer and alumina layer possesses more excellent hydrogen infiltration-resistant performance.In addition, the matched coefficients of thermal expansion of chromium oxide and aluminium oxide is good, is respectively 7.5 × 10
-6k
-1with 6.9 × 10
-6k
-1, be conducive to obtain the good composite coating of thermal shock performance.
Described alumina layer be by one or more and Direct precipitation in reaction magnetocontrol sputtering, plasma spraying, chemical vapour deposition (CVD), metal-organic chemical vapor deposition equipment and sol-gal process method on chromium oxide layer and manganese picotite layer surface.
The gross thickness of the chromium oxide layer of described stainless steel-based surface and manganese picotite layer is 0.5-5 μ m, and wherein the thickness of manganese picotite layer is 0-0.5 micron, and thickness ≠ 0.The thickness of described alumina layer is 0.1-50 μ m.
Compared with prior art, the advantage of hydrogen infiltration-resistant composite coating of the present invention is:
1. hydrogen infiltration-resistant composite coating combines chromium oxide layer and alumina layer hydrogen infiltration-resistant characteristic, and therefore the more independent chromium oxide layer of hydrogen infiltration-resistant performance or the alumina layer of coating are more excellent.
2. chromium oxide layer and manganese picotite layer can regulate the thermal expansion process of stainless steel base and outer oxide aluminized coating, improve the bond strength of outer oxide aluminized coating and stainless steel base.
Accompanying drawing explanation
Fig. 1 is the structural representation of hydrogen infiltration-resistant composite coating.
Fig. 2 is the chromium oxide layer of the stainless steel-based surface in embodiment 1 and the cross section electron scanning electromicroscopic photograph of manganese picotite layer.
Fig. 3 is the X ray diffracting spectrum of the hydrogen infiltration-resistant composite coating in embodiment 1.
Fig. 4 is the cross section electron scanning electromicroscopic photograph of the hydrogen infiltration-resistant composite coating in embodiment 2.
The specific embodiment
Hydrogen infiltration-resistant composite coating structure schematic diagram as shown in Figure 1, has hydrogen infiltration-resistant composite coating on stainless steel base 1, and this hydrogen infiltration-resistant composite coating is by from the inside to the outside by chromium oxide layer 2, and manganese picotite layer 3 and aluminum oxide coating layer 4 are composited.
The present invention further illustrates in conjunction with the following example and accompanying drawing, but the present invention is not limited to embodiment below.
1) 304 stainless steel substrates polishings, ultrasonic cleaning are processed and are dried up;
2) sample cleaning being dried up is placed in quartz tube type atmosphere furnace, carries 827 ℃ of oxidation 5h under aqueous vapor atmosphere obtain chromium oxide layer and manganese picotite layer at argon gas.Fig. 2 is the Cross Section Morphology of 304 stainless steel surfaces chromium oxide layers and manganese picotite layer, and wherein 1 is 304 stainless steels, and 2 is chromium oxide layer, and 3 is manganese picotite layer.Fig. 3 is the X ray diffracting spectrum of 304 stainless steel surfaces chromium oxide layers and manganese picotite layer, and coating is made up of chromium oxide and manganese picotite.
3) sample is placed in to quartz tube type atmosphere furnace and adopts metal-organic chemical vapor deposition equipment method deposition of aluminium oxide coatings, 400 ℃ of depositing temperatures, sedimentation time 4h.The composite coating style obtaining has been carried out to hydrogen penetrating quality test, and result shows that at 600 ℃, this composite coating is 113-126 to the 304 stainless hydrogen infiltration reduction factors, and its hydrogen permeation barrier performance is obviously better than aluminum oxide coating layer style and chromium oxide coating.
1) 316 stainless steel substrates polishings, ultrasonic cleaning are processed and are dried up;
2) sample cleaning being dried up is placed in quartz tube type atmosphere furnace, carries 877 ℃ of oxidation 5h under aqueous vapor atmosphere obtain chromium oxide layer and manganese picotite layer at argon gas.
3) sample is placed in to quartz tube type atmosphere furnace and adopts metal-organic chemical vapor deposition equipment method deposition of aluminium oxide coatings, 400 ℃ of depositing temperatures, sedimentation time 4h.Fig. 4 is the Cross Section Morphology of this hydrogen infiltration-resistant composite coating, is respectively 316 stainless steel bases 1 from the inside to the outside, chromium oxide layer 2, manganese picotite layer 3 and alumina layer 4.The composite coating style obtaining has been carried out to the hydrogen penetrating quality test after 700 ℃ of 30 thermal cycles, at 600 ℃, composite coating is 107-132 to the 316 stainless hydrogen infiltration reduction factors, it is 110-127 that the hydrogen infiltration of the composite coating after thermal cycle reduces the factor, this result is better than aluminum oxide coating layer, and therefore composite coating has excellent thermal shock resistance.
Claims (6)
1. a stainless steel-based hydrogen infiltration-resistant composite coating, is characterized in that, has hydrogen infiltration-resistant composite coating on stainless steel base, and this hydrogen infiltration-resistant composite coating is made up of chromium oxide layer, manganese picotite layer and the alumina layer of stainless steel-based surface from the inside to the outside.
2. stainless steel-based hydrogen infiltration-resistant composite coating according to claim 1, is characterized in that, chromium oxide layer, the manganese picotite layer of described stainless steel-based surface are obtained by stainless steel in-situ oxidation.
3. according to the hydrogen infiltration-resistant composite coating described in claim 1 and 2, it is characterized in that, described manganese picotite is by the Mn with spinel structure
xcr
yo
4oxide forms, wherein 1≤x≤2,1≤y≤2, and 2≤x+y≤3.
4. stainless steel-based hydrogen infiltration-resistant composite coating according to claim 1, it is characterized in that, described alumina layer be by one or more and Direct precipitation in reaction magnetocontrol sputtering, plasma spraying, chemical vapour deposition (CVD), metal-organic chemical vapor deposition equipment and sol-gal process method on chromium oxide layer and manganese picotite layer surface.
5. stainless steel-based hydrogen infiltration-resistant composite coating according to claim 1, it is characterized in that, the gross thickness of the lip-deep chromium oxide layer of described stainless steel base and manganese picotite layer is 0.5-5 micron, and wherein the thickness of manganese picotite layer is 0-0.5 micron, and thickness ≠ 0.
6. stainless steel-based hydrogen infiltration-resistant composite coating according to claim 1, is characterized in that the thickness of described alumina layer is 0.1-50 micron.
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|---|---|---|---|
| CN201210449522.0A CN103802385A (en) | 2012-11-12 | 2012-11-12 | Stainless steel based hydrogen permeation prevention composite coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210449522.0A CN103802385A (en) | 2012-11-12 | 2012-11-12 | Stainless steel based hydrogen permeation prevention composite coating |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561891A (en) * | 2015-01-30 | 2015-04-29 | 四川大学 | Double-component gradient hydrogen permeation barrier coating and preparation method thereof |
| CN105369205A (en) * | 2015-10-16 | 2016-03-02 | 常州大学 | Technological method for manufacturing multifunctional film on surface of stainless steel |
| 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 |
| CN106280039A (en) * | 2016-08-31 | 2017-01-04 | 广州双乳胶制品有限公司 | A kind of anti-tritium glove and preparation method thereof |
| CN108220961A (en) * | 2018-01-12 | 2018-06-29 | 清华大学 | A kind of compound hydrogen infiltration-resistant material of stainless base steel and preparation method thereof |
| CN112899733A (en) * | 2021-01-20 | 2021-06-04 | 华中科技大学 | Compact chromium oxynitride hydrogen permeation-resistant coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2093073A (en) * | 1981-02-06 | 1982-08-25 | Maschf Augsburg Nuernberg Ag | A method of producing protective oxide layers |
| CN101215709A (en) * | 2007-12-27 | 2008-07-09 | 南京航空航天大学 | Vitreous barrier layer for stainless steel with resistance to hydrogen or hydrogen isotope penetration and preparation method thereof |
| CN101265603A (en) * | 2008-01-29 | 2008-09-17 | 四川大学 | A kind of preparation method of multi-layer hydrogen permeation barrier composite membrane |
-
2012
- 2012-11-12 CN CN201210449522.0A patent/CN103802385A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2093073A (en) * | 1981-02-06 | 1982-08-25 | Maschf Augsburg Nuernberg Ag | A method of producing protective oxide layers |
| CN101215709A (en) * | 2007-12-27 | 2008-07-09 | 南京航空航天大学 | Vitreous barrier layer for stainless steel with resistance to hydrogen or hydrogen isotope penetration and preparation method thereof |
| CN101265603A (en) * | 2008-01-29 | 2008-09-17 | 四川大学 | A kind of preparation method of multi-layer hydrogen permeation barrier composite membrane |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561891A (en) * | 2015-01-30 | 2015-04-29 | 四川大学 | Double-component gradient hydrogen permeation barrier coating and preparation method thereof |
| CN105369205A (en) * | 2015-10-16 | 2016-03-02 | 常州大学 | Technological method for manufacturing multifunctional film on surface of stainless steel |
| CN105369205B (en) * | 2015-10-16 | 2018-06-12 | 常州大学 | A kind of stainless steel surface prepares the process of multi-function membrane |
| 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 two-dimensional material regulating silicon-carbon composite structure hydrogen barrier coating and preparation method thereof |
| CN106280039A (en) * | 2016-08-31 | 2017-01-04 | 广州双乳胶制品有限公司 | A kind of anti-tritium glove and preparation method thereof |
| CN108220961A (en) * | 2018-01-12 | 2018-06-29 | 清华大学 | A kind of compound hydrogen infiltration-resistant material of stainless base steel and preparation method thereof |
| CN108220961B (en) * | 2018-01-12 | 2020-08-14 | 清华大学 | Stainless steel-based composite hydrogen permeation resistant material and preparation method thereof |
| CN112899733A (en) * | 2021-01-20 | 2021-06-04 | 华中科技大学 | Compact chromium oxynitride hydrogen permeation-resistant coating and preparation method thereof |
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Application publication date: 20140521 |