CN105644058B - A kind of Y2O3/Cr2O3Complex gradient hydrogen resistance coating and preparation method thereof - Google Patents
A kind of Y2O3/Cr2O3Complex gradient hydrogen resistance coating and preparation method thereof Download PDFInfo
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- CN105644058B CN105644058B CN201410676340.6A CN201410676340A CN105644058B CN 105644058 B CN105644058 B CN 105644058B CN 201410676340 A CN201410676340 A CN 201410676340A CN 105644058 B CN105644058 B CN 105644058B
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- stainless steel
- hydrogen resistance
- complex gradient
- vacuum heat
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- 239000011248 coating agent Substances 0.000 title claims abstract description 113
- 238000000576 coating method Methods 0.000 title claims abstract description 113
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000001257 hydrogen Substances 0.000 title claims abstract description 65
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 65
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 34
- 239000010935 stainless steel Substances 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910001105 martensitic stainless steel Inorganic materials 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 abstract description 10
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 abstract description 9
- 229910000423 chromium oxide Inorganic materials 0.000 abstract description 9
- 230000008595 infiltration Effects 0.000 abstract description 4
- 238000001764 infiltration Methods 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 239000011651 chromium Substances 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000010653 organometallic reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The present invention relates to a kind of Y2O3/Cr2O3Complex gradient hydrogen resistance coating and preparation method thereof, the coating can be applied to the hydrogen infiltration-resistant of high-temperature vacuum heat-collecting tube.The Y2O3/Cr2O3Complex gradient hydrogen resistance coating is by stainless steel tube and the Y for being applied to stainless steel pipe inner surface2O3/Cr2O3Composite coating is formed.The composite coating is prepared by Metalorganic Chemical Vapor Deposition, and by repeated deposition chromium oxide and yttria coating, it is about 0.1~20 μm of multilayer Y to obtain thickness2O3And Cr2O3Complex gradient hydrogen resistance coating；The multilayer alternating structure that the coating is chromium oxide by innermost layer and yittrium oxide outermost layer is forms.The hydrogen resistance coating and substrate combinating strength are high, preparation technology is simple and cost is cheap, and NdFeB permanent magnets improve more than 150 times.
Description
Technical field
The present invention relates to a kind of Y2O3/Cr2O3Complex gradient hydrogen resistance coating and preparation method thereof, the coating can be applied to height
The hydrogen infiltration-resistant of warm vacuum heat collection pipe.
Background technology
The aging of heat transport fluid can produce free hydrogen in solar energy heat collection pipe, and hydrogen passes through mesotube by osmosis,
The vacuum annular space between mesotube and sleeve pipe is reached, causes the rise of annular space pressure, and then cause heat collecting pipe heat waste
The increase of mistake.The vacuum of annular gap between guarantee pipe, it is necessary to which taking appropriate measures reduces the amounts of hydrogen of vacuum annular space.For
This, researcher proposes prevents hydrogen from permeating using hydrogen resistance coating, so that the pressure of efficient dominating set heat-tube vacuum annular space,
Reduce the thermal losses of thermal-collecting tube.
The hydrogen resistance coating occurred earliest, which is that CN1971168 is disclosed, uses Y2O3, can be significantly as resistance hydrogen material
The infiltration of hydrogen is prevented, makes absorption tube that there is less heat loss.But such resistance its thermal coefficient of expansion of hydrogen material and matrix exist compared with
Big mismatch, larger thermal stress is produced after certain thermal shock, between coating and matrix, causes coating to be separated with matrix, serious shadow
Ring coating NdFeB permanent magnets, for solve the above problems researcher find it is other be well combined with matrix, thermal coefficient of expansion is adapted to
Small hydrogen resistance coating is as transition zone.
The content of the invention
In view of the foregoing, the present invention uses chromium oxide coating as tie coat, Cr2O3Thermal coefficient of expansion and stainless steel
Body more matches, and structure is more stable, and NdFeB permanent magnets are preferable, and yttria coating prepares MULTILAYER COMPOSITE gradient as hydrogen resistance coating
Hydrogen resistance coating, so as to improve NdFeB permanent magnets, there is provided it is a kind of with that matrix is well combined, preparation technology is simple, cost is cheap is more
Layer complex gradient hydrogen resistance coating material.
A kind of Y2O3/Cr2O3Complex gradient hydrogen resistance coating, the complex gradient hydrogen resistance coating is by stainless steel tube and is applied to not
The Y of rust steel pipe internal-surface2O3/Cr2O3Composite coating is formed.
Preferably, Y2O3/Cr2O3Composite coating material is Y2O3And Cr2O3；Y2O3/Cr2O3Composite coating is Y2O3Coating and
Cr2O3Coating alternating structure, total number of plies are more than or equal to 4 layers.
Y2O3/Cr2O3The innermost layer of composite coating is Cr2O3Coating, outermost layer Y2O3Coating.
Preferably, Y2O3/Cr2O3The thickness of composite coating is between 0.1~20 μm.
Preferably, the stainless steel tube is austenitic stainless steel or martensitic stain less steel.
Y2O3Coating and Cr2O3The thickness of coating can be mainly relevant with the preparation technology of each coating with identical or different.It is excellent
Choosing, multiple Y2O3The thickness of coating is identical or close, multiple Cr2O3The thickness of coating is identical or close.
Present invention also offers above-mentioned Y2O3/Cr2O3Application of the complex gradient hydrogen resistance coating in high-temperature vacuum heat-collecting tube,
I.e. above-mentioned stainless steel tube is the stainless steel mesotube of high-temperature vacuum heat-collecting tube；In the stainless steel mesotube of high-temperature vacuum heat-collecting tube
Inner surface applies Y2O3/Cr2O3Composite coating.The high-temperature vacuum heat-collecting tube has spectral selective absorbing coating by outer wall
Stainless steel mesotube and glass outer sleeve pipe composition.
The present invention is difficult to preparation high-performance for current high-temperature vacuum heat-collecting tube inner surface, uniform and stable hydrogen resistance coating carries
For a kind of fairly simple Y2O3And Cr2O3Complex gradient hydrogen resistance coating and preparation method thereof, i.e., the table in high-temperature vacuum heat-collecting tube
Kept man of a noblewoman time prepares Y using double evaporation source layerings2O3/Cr2O3MULTILAYER COMPOSITE gradient hydrogen resistance coating.
The present invention prepares Y using metal-organic chemical vapor deposition technology in high-temperature vacuum heat-collecting tube inner surface2O3/
Cr2O3MULTILAYER COMPOSITE gradient hydrogen resistance coating, the complex gradient coating can effectively reduce H2In the permeability of stainless steel, so that very well
The purpose for reaching hydrogen infiltration-resistant.
A kind of Y2O3/Cr2O3The preparation method of complex gradient hydrogen resistance coating, comprises the following steps：
(1) high-temperature vacuum heat-collecting tube stainless steel pipe inner surface is polished to 0.1~2 μm of roughness；
(2) Cr is prepared in stainless steel pipe inner surface using metal-organic chemical vapor deposition technology2O3Coating；
(3) Y is prepared in stainless steel pipe inner surface using metal-organic chemical vapor deposition technology2O3Coating；
(4) repeat the above steps (2)；
(5) repeat the above steps (3)；
It is final to obtain the multilayer Y that thickness is about 0.1-20 μm2O3/Cr2O3Complex gradient hydrogen resistance coating.
Prepare Cr2O3Coating specific process parameter is：React 50-200 DEG C of source temperature；Carrier gas flux 40-500ml/min；Carry
Gas is hydrogen.
Prepare Y2O3Coating specific process parameter is：React 50-200 DEG C of source temperature；Carrier gas flux 10-300ml/min；Carry
Gas is hydrogen.
, will during mainly by current-carrying gas by the container in organometallic reaction source when the principle of the present invention is growth film
The saturated vapor of reaction source is brought into reaction chamber to be mixed with other reacting gas, and chemistry then occurs in heated thereon
The growth of film is facilitated in reaction.
The present invention compares with existing technological achievements, has advantages below and high-lighting achievement：First in high-temperature vacuum thermal-arrest
Inside pipe wall realizes the preparation of yittrium oxide and chromium oxide mixing gradient hydrogen resistance coating, and the Y that this method is formed2O3And Cr2O3It is compound
Gradient hydrogen resistance coating has the characteristics of thickness is controllable, and compactness is high, and the more uniform NdFeB permanent magnets of composition are excellent.
The Y of the present invention2O3/Cr2O3Composite coating is prepared by metal-organic chemical vapor deposition method, passes through repeated deposition oxygen
Change chromium and yttria coating, it is about 0.1~20 μm of multilayer Y to obtain thickness2O3And Cr2O3Complex gradient hydrogen resistance coating；The coating by
The multilayer alternating structure composition that innermost layer is chromium oxide and yittrium oxide outermost layer is.The hydrogen resistance coating can be used for stainless steel structure part
Hydrogen permeation barrier, particularly solar high-temperature vacuum heat-collecting tube inner tube stainless steel tube hydrogen permeation barrier.And the resistance hydrogen applies
Layer with substrate combinating strength is high, preparation technology is simple and cost is cheap, more than 150 times of NdFeB permanent magnets raising.
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings.
Brief description of the drawings
Fig. 1 is to scribble multilayer Y2O3/Cr2O3The high-temperature vacuum heat-collecting tube structural representation of complex gradient hydrogen resistance coating.
Embodiment
As shown in figure 1, to scribble Y2O3/Cr2O3The high-temperature vacuum heat-collecting tube structural representation of complex gradient hydrogen resistance coating,
It is from inside to outside yttria coating 1, chromium oxide coating 2, yttria coating 1, chromium oxide coating 2, stainless steel tube 3, heat absorbing coating
4th, vacuum area 5 and outer glass tube 6.Wherein, Y2O3/Cr2O3Complex gradient hydrogen resistance coating by high-temperature vacuum heat-collecting tube stainless steel tube
3rd, chromium oxide coating 2, yttria coating 1, chromium oxide coating 2 and yttria coating 1 are combined.High-temperature vacuum heat-collecting tube is main
By outer wall there is the stainless steel mesotube of spectral selective absorbing coating and glass outer sleeve pipe to form, stainless steel tube and outer glass tube
Between form ring vaccum.Stainless steel tube is austenitic stainless steel or martensitic stain less steel.
Embodiment 1
Prepare the high-temperature vacuum heat-collecting tube Y that thickness is 0.5 μm2O3/Cr2O3Complex gradient hydrogen resistance coating：
(1) stainless steel pipe inner surface is polished to 1 μm of roughness；
(2) Cr is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 150 DEG C of source temperature；Reaction time 30min；Carrier gas flux 200ml/min.
(3) Y is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 100 DEG C of source temperature；Reaction time 30min；Carrier gas flux is 100ml/min.
(4) repeat the above steps (2)；
(5) repeat the above steps (3).
It is final to obtain the multilayer Y that thickness is about 0.5 μm2O3And Cr2O3Complex gradient hydrogen resistance coating.
Determine multilayer Y2O3And Cr2O3H of the complex gradient hydrogen resistance coating at 400 DEG C2Permeability, NdFeB permanent magnets improve 230 times.
Embodiment 2
Prepare the high-temperature vacuum heat-collecting tube Y that thickness is 1 μm2O3/Cr2O3Complex gradient hydrogen resistance coating：
(1) stainless steel pipe inner surface is polished to 0.5 μm of roughness；
(2) Cr is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 180 DEG C of source temperature；Reaction time 60min；Carrier gas flux 200ml/min.
(3) Y is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 120 DEG C of source temperature；Reaction time 60min；Carrier gas flux 150ml/min.
(4) repeat the above steps (2)；
(5) repeat the above steps (3).
It is final to obtain the multilayer Y that thickness is about 1 μm2O3And Cr2O3Complex gradient hydrogen resistance coating.
Determine multilayer Y2O3And Cr2O3H of the complex gradient hydrogen resistance coating at 400 DEG C2Permeability, NdFeB permanent magnets improve 290 times.
Embodiment 3
Prepare the high-temperature vacuum heat-collecting tube Y that thickness is 0.8 μm2O3/Cr2O3Complex gradient hydrogen resistance coating：
(1) stainless steel pipe inner surface is polished to 0.3 μm of roughness；
(2) Cr is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 200 DEG C of source temperature；Reaction time 45min；Carrier gas flux 200ml/min.
(3) Y is prepared in high-temperature vacuum heat-collecting tube inner surface using metal-organic chemical vapor deposition technology2O3Coating；Tool
Body technology parameter is：React 160 DEG C of source temperature；Reaction time 45min；Carrier gas flux 80ml/min.
(4) repeat the above steps (2)；
(5) repeat the above steps (3).
It is final to obtain the multilayer Y that thickness is about 0.8 μm2O3And Cr2O3Complex gradient hydrogen resistance coating.
Determine multilayer Y2O3And Cr2O3H of the complex gradient hydrogen resistance coating at 400 DEG C2Permeability, NdFeB permanent magnets improve 360 times.
The multilayer Y of the present invention2O3And Cr2O3Complex gradient hydrogen resistance coating can be used for the hydrogen permeation barrier of stainless steel structure part,
The particularly hydrogen permeation barrier of solar high-temperature vacuum heat-collecting tube inner tube stainless steel tube.And the hydrogen resistance coating is combined by force with matrix
Degree is high, and NdFeB permanent magnets improve more than 230 times.
Claims (7)
- A kind of 1. Y2O3/Cr2O3Complex gradient hydrogen resistance coating, it is characterised in that：By stainless steel tube and it is applied to table in stainless steel tube The Y in face2O3/Cr2O3Composite coating is formed；Described Y2O3/Cr2O3Composite coating is Y2O3Coating and Cr2O3Coating alternating structure, Total number of plies is more than or equal to 4 layers；Described Y2O3/Cr2O3The innermost layer of composite coating is Cr2O3Coating, outermost layer Y2O3Coating； Described Y2O3/Cr2O3The thickness of composite coating is 0.1~20 μm.
- 2. Y according to claim 12O3/Cr2O3Complex gradient hydrogen resistance coating, it is characterised in that：The stainless steel tube is Austria Family name's body stainless steel or martensitic stain less steel.
- 3. the Y described in claim 1 or 22O3/Cr2O3Application of the complex gradient hydrogen resistance coating in high-temperature vacuum heat-collecting tube.
- 4. Y according to claim 32O3/Cr2O3Application of the complex gradient hydrogen resistance coating in high-temperature vacuum heat-collecting tube, its It is characterised by：Apply Y in the inner surface of the stainless steel mesotube of high-temperature vacuum heat-collecting tube2O3/Cr2O3Composite coating.
- 5. Y according to claim 42O3/Cr2O3Application of the complex gradient hydrogen resistance coating in high-temperature vacuum heat-collecting tube, its It is characterised by：The high-temperature vacuum heat-collecting tube is had the stainless steel mesotube and outer layer glass of spectral selective absorbing coating by outer wall Glass sleeve pipe forms.
- A kind of 6. Y2O3/Cr2O3The preparation method of complex gradient hydrogen resistance coating, comprises the following steps：(1) high-temperature vacuum heat-collecting tube stainless steel pipe inner surface is polished to 0.1~2 μm of roughness；(2) Cr is prepared in stainless steel pipe inner surface using metal-organic chemical vapor deposition technology2O3Coating；(3) Y is prepared in stainless steel pipe inner surface using metal-organic chemical vapor deposition technology2O3Coating；(4) repeat the above steps (2)；(5) repeat the above steps (3)；It is final to obtain the multilayer Y that thickness is 0.1-20 μm2O3/Cr2O3Complex gradient hydrogen resistance coating.
- 7. Y according to claim 62O3/Cr2O3The preparation method of complex gradient hydrogen resistance coating, it is characterised in that：Prepare Cr2O350-200 DEG C of the reaction source temperature of coating, carrier gas flux 40-500ml/min；Prepare Y2O3The reaction source temperature 50- of coating 200 DEG C, carrier gas flux 10-300ml/min.
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| CN108239751B (en) * | 2016-12-27 | 2020-02-18 | 有研工程技术研究院有限公司 | Device for preparing hydrogen-resistant coating on inner wall of high-temperature vacuum heat-collecting tube |
| CN113046695A (en) * | 2019-12-27 | 2021-06-29 | 有研工程技术研究院有限公司 | Yttrium/yttrium oxide composite hydrogen resistant coating |
Citations (3)
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|---|---|---|---|---|
| GB2093073A (en) * | 1981-02-06 | 1982-08-25 | Maschf Augsburg Nuernberg Ag | A method of producing protective oxide layers |
| CN103160828A (en) * | 2011-12-09 | 2013-06-19 | 北京有色金属研究总院 | Steel-based hydrogen permeation-resistant composite coating and preparation method for same |
| CN103895282A (en) * | 2012-12-26 | 2014-07-02 | 北京有色金属研究总院 | Composite gradient hydrogen-resistant coating for high-temperature evacuated collector tube and preparation method thereof |
-
2014
- 2014-11-21 CN CN201410676340.6A patent/CN105644058B/en active Active
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 |
| CN103160828A (en) * | 2011-12-09 | 2013-06-19 | 北京有色金属研究总院 | Steel-based hydrogen permeation-resistant composite coating and preparation method for same |
| CN103895282A (en) * | 2012-12-26 | 2014-07-02 | 北京有色金属研究总院 | Composite gradient hydrogen-resistant coating for high-temperature evacuated collector tube and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| MOCVD工艺制备Y2O3涂层的研究;蒋文文;《中国硕士学位论文全文数据库 工程科技Ⅰ辑》;20111015;第2、11、22页 * |
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Effective date of registration: 20190627 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: No. 2, Xinjie street, Xicheng District, Beijing, Beijing Patentee before: General Research Institute for Nonferrous Metals |