CN115044875B - Multilayer gradient composite hydrogen-resistant coating and preparation method thereof - Google Patents
Multilayer gradient composite hydrogen-resistant coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 101
- 239000011248 coating agent Substances 0.000 title claims abstract description 99
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000001257 hydrogen Substances 0.000 title claims abstract description 53
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 57
- 229910052574 oxide ceramic Inorganic materials 0.000 claims abstract description 41
- 239000011224 oxide ceramic Substances 0.000 claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 31
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000004544 sputter deposition Methods 0.000 claims description 42
- 238000000151 deposition Methods 0.000 claims description 30
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 14
- 238000009792 diffusion process Methods 0.000 claims description 13
- 230000004888 barrier function Effects 0.000 claims description 9
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- HKRXOWGILGJWPT-UHFFFAOYSA-N oxygen(2-) yttrium(3+) zirconium(4+) Chemical compound [O-2].[Y+3].[Zr+4] HKRXOWGILGJWPT-UHFFFAOYSA-N 0.000 claims description 3
- 239000010963 304 stainless steel Substances 0.000 claims description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 2
- 229910001067 superalloy steel Inorganic materials 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 138
- 230000000903 blocking effect Effects 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 5
- 230000007704 transition Effects 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 40
- 239000000919 ceramic Substances 0.000 description 15
- 239000013077 target material Substances 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- 229910018173 Al—Al Inorganic materials 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000005524 ceramic coating Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- HVXCTUSYKCFNMG-UHFFFAOYSA-N aluminum oxygen(2-) zirconium(4+) Chemical compound [O-2].[Zr+4].[Al+3] HVXCTUSYKCFNMG-UHFFFAOYSA-N 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- 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
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- 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
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- C23C14/083—Oxides of refractory metals or yttrium
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention discloses a multilayer gradient composite hydrogen-resistant coating, which comprises at least 3 layers of different oxide ceramic layers coated on a substrate, wherein different metal-oxide dispersion layers are arranged between the substrate and the oxide ceramic layers and between the adjacent oxide ceramic layers. According to the invention, the metal-oxide dispersion layer is introduced between layers to serve as an interlayer transition layer, so that the binding force between the coating and the substrate and between the coating and the coating is improved, the high-temperature stability of the coating is enhanced, and the cold and hot impact resistance of a coating system is improved; the dispersion layer in the composite coating system is present, so that the interlayer bonding mode is converted into metal-metal bonding, and even if the top layer is scratched to cause peeling in the use process of the coating, the metal dispersion layer can be oxidized in situ at high temperature to generate a corresponding oxide layer so as to compensate peeling damage, and the coating has certain self-repairing property and effectively prolongs the hydrogen permeation blocking service life of the coating.
Description
Technical Field
The invention relates to the technical field of hydrogen-resistant coatings, in particular to a multilayer gradient composite hydrogen-resistant coating and a preparation method thereof.
Background
Because hydrogen has extremely small atomic radius, the hydrogen has very strong infiltration and diffusion capacity in the metal material, and the infiltration of hydrogen can cause the metal material to generate phenomena of hydrogen embrittlement, hydrogen corrosion and the like, so that the service life of the metal material is greatly shortened. It is found that the permeation rate of hydrogen in the ceramic material is far lower than that of hydrogen in the metal structural material, so that the preparation of the hydrogen-resistant ceramic coating on the surface of the metal material becomes one of the main technical means for solving the hydrogen permeation problem.
In the prior art, the hydrogen-resistant coatings developed at present are mainly divided into four main categories: (1) With Al 2 O 3 、Cr 2 O 3 、YSZ、Er 2 O 3 Predominantly oxide ceramic coating, (2) Si-based 3 N 4 And SiC-based silicide ceramic coating, (3) titanium-based ceramic coating such as TiN and TiC, and (4) FeAl-based aluminide coating. However, the single-layer hydrogen-resistant coating has limited hydrogen-resistant effect, the coating is easy to damage, and the hydrogen-resistant effect is further weakened after the coating is damaged.
The method improves the hydrogen resistance and high temperature stability of the coating to a certain extent by introducing a transition layer with moderate thermal expansion coefficient, however, the phenomenon of interlayer peeling and falling still exists in the high temperature service environment (T >900 ℃) of the coating, so that the coating is seriously invalid and the service life of the coating is greatly reduced.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a multilayer gradient composite hydrogen-resistant coating and a preparation method thereof, and the preparation method specifically comprises the following steps:
the multilayer gradient composite hydrogen-resistant coating comprises at least 3 layers of different oxide ceramic layers coated on a substrate, wherein different metal-oxide dispersion layers are arranged between the substrate and the oxide ceramic layers and between the adjacent oxide ceramic layers.
Specifically, the coating comprises the following components in sequence from the inner layer to the outer layer: zr-yttrium oxide stabilized zirconia dispersion layer, yttrium oxide stabilized zirconia layer, zr-Y 2 O 3 A dispersion layer, a yttrium oxide layer and Y-Al 2 O 3 A dispersion layer and an alumina layer; in the present application, the YSZ is yttria-stabilized zirconiaIs abbreviated as (1).
Specifically, the matrix is low-activity martensite or austenite of stainless steel or high-temperature alloy.
Specifically, the atomic proportion of the metal phase in the dispersion layer is in the range of 30% -80%.
In particular, the total thickness of the hydrogen-resistant coating system is not more than 10 mu m.
Specifically, the thickness of the dispersion layer is 1/5-1/2 of the thickness of the oxide ceramic layer arranged on the outer layer.
In particular, the total thickness of the hydrogen barrier coating system is from 0.1 μm to 1 μm.
The invention discloses a preparation method of a multilayer gradient composite hydrogen-resistant coating, which comprises the following steps:
(1) Polishing one side of the substrate to a roughness of 0.1-2 mu m;
(2) Co-sputter depositing a first metal-oxide diffusion layer on a substrate;
(3) Sputtering and depositing a first oxide ceramic layer on the coating prepared in the previous step;
(4) Coating different metal-oxide dispersion layers and oxide ceramic layers on the coating prepared in the previous step by alternately adopting a co-sputtering deposition method and a sputtering deposition method to obtain a composite coating with alternately overlapped metal-oxide dispersion layers and oxide ceramic layers, wherein the number of layers of the composite coating is not less than 6, and the outermost layer is an oxide ceramic layer;
(5) And (3) carrying out Ar atmosphere high-temperature heat treatment on the composite coating obtained in the step (4) and alternately overlapped with the metal-oxide dispersion layer and the oxide ceramic layer, and finally obtaining the multilayer gradient composite hydrogen-resistant coating.
Specifically, the number of layers of the composite coating obtained in the step (4) is 6, and the composite coating sequentially comprises a first metal-oxide dispersion layer, a first oxide ceramic layer, a second metal-oxide dispersion layer, a second oxide ceramic layer, a third metal-oxide dispersion layer and a third oxide ceramic layer from inside to outside.
Specifically, the first metal-oxide dispersion layer is a Zr-yttria stabilized zirconia dispersion layer, the first oxide ceramic layer is a yttria stabilized zirconia layer, the second metal-oxide dispersion layer is a Zr-Y2O 3 dispersion layer, the second oxide ceramic layer is a yttria layer, the third metal-oxide dispersion layer is a Y-Al 2O3 dispersion layer, and the third oxide ceramic layer is an alumina layer.
The invention has the beneficial effects that:
1. according to the invention, the metal-oxide dispersion layer is introduced between layers to serve as an interlayer transition layer, so that the binding force between the coating and the substrate and between the coating and the coating is improved, the high-temperature stability of the coating is enhanced, and the cold and hot impact resistance of a coating system is improved;
2. the dispersion layer in the composite coating system disclosed by the invention is present, so that the interlayer bonding mode is converted into metal-metal bonding, and even if the top layer of the coating is scratched to cause peeling in the use process, the metal dispersion layer can be oxidized in situ at high temperature to generate a corresponding oxide layer so as to compensate the peeling damage, thereby having certain self-repairing property and effectively prolonging the hydrogen permeation blocking life of the coating.
Drawings
FIG. 1 is a schematic diagram of the structure of a multilayer gradient composite hydrogen barrier coating of the present disclosure.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description. The embodiments shown below do not limit the inventive content described in the claims in any way. The whole contents of the constitution shown in the following examples are not limited to the solution of the invention described in the claims.
The multilayer gradient composite hydrogen-resistant coating comprises at least 3 layers of different oxide ceramic layers coated on a substrate, wherein different metal-oxide dispersion layers are arranged between the substrate and the oxide ceramic layers and between the adjacent oxide ceramic layers.
Preferably, the multilayer gradient composite hydrogen-resistant coating comprises 3 oxide ceramic layers and 3 metal-oxide dispersion layers, and specifically, the coating sequentially comprises, from inner layer to outer layer: zr-yttria stabilized zirconia dispersion layer, zr-YSZ for Zr-oxideYttrium-stabilized zirconia, yttria-stabilized zirconia layers, yttria-stabilized zirconia, zirconium-yttrium-yttria dispersion layers expressed by YSZ, zr-Y 2 O 3 Represents zirconium-yttrium oxide, yttrium oxide (Y) 2 O 3 ) Layer, zirconium-aluminum oxide dispersion layer, using Y-Al 2 O 3 Represents zirconium-aluminum oxide, aluminum oxide (Al 2 O 3 ) A layer.
Preferably, the matrix is low-activity martensite or austenite of stainless steel or high-temperature alloy.
Preferably, the metal phase in the dispersion layer accounts for 30-80% of the atomic proportion. In particular, the metal phase in the dispersed layer may be 30%, 40%, 50%, 60%, 70%, or 80% by atomic ratio.
Preferably, the total thickness of the hydrogen barrier coating system is not more than 10 μm, more preferably, the total thickness of the hydrogen barrier coating system is from 0.1 μm to 1 μm, and may be specifically 0.1 μm, 0.2 μm, 0.5 μm, 0.8 μm, 0.9 μm, or 1 μm.
Preferably, the thickness of the dispersion layer is 1/5-1/2 of the thickness of the oxide ceramic layer arranged on the outer layer, and can be 1/5, 1/4, 1/3 or 1/2.
The invention discloses a preparation method of a multilayer gradient composite hydrogen-resistant coating, which comprises the following steps:
(1) Polishing the substrate to a roughness of 0.1 μm to 2 μm, specifically 0.1 μm, 0.5 μm, 0.8 μm, 1 μm, 1.5 μm, 1.8 μm, or 2 μm;
(2) Co-sputter depositing a first metal-oxide diffusion layer on a substrate;
(3) Sputtering and depositing a first oxide ceramic layer on the coating prepared in the previous step;
(4) Coating different metal-oxide dispersion layers and oxide ceramic layers on the coating prepared in the previous step by alternately adopting a co-sputtering deposition method and a sputtering deposition method to obtain a composite coating with alternately overlapped metal-oxide dispersion layers and oxide ceramic layers, wherein the number of layers of the composite coating is not less than 6, and the outermost layer is an oxide ceramic layer;
(5) And (3) carrying out Ar atmosphere high-temperature heat treatment on the composite coating obtained in the step (4) and alternately overlapped with the metal-oxide dispersion layer and the oxide ceramic layer, and finally obtaining the multilayer gradient composite hydrogen-resistant coating.
Preferably, the number of layers of the composite coating obtained in the step (4) is 6, and the composite coating sequentially comprises a first metal-oxide dispersion layer, a first oxide ceramic layer, a second metal-oxide dispersion layer, a second oxide ceramic layer, a third metal-oxide dispersion layer and a third oxide ceramic layer from inside to outside.
Preferably, the first metal-oxide dispersion layer is a Zr-Yttria Stabilized Zirconia (YSZ) dispersion layer, the first oxide ceramic layer is a Yttria Stabilized Zirconia (YSZ) layer, and the second metal-oxide dispersion layer is a Zr-Y 2 O 3 A dispersion layer of yttrium oxide (Y) 2 O 3 ) A third metal-oxide dispersion layer of Y-Al 2 O 3 A dispersion layer of aluminum oxide (Al 2 O 3 ) A layer.
Example 1
316L Zr-YSZ/YSZ/Zr-Y-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 Preparing a composite hydrogen-resistant coating:
(1) Selecting 316L stainless steel as a matrix, polishing one side of the matrix to a roughness of 1.5 mu m, cleaning and drying for later use;
(2) Zr-YSZ dispersion layer is prepared by magnetron co-sputtering, both targets are powered by a radio frequency power supply, ar is used as glow starting gas. When the back vacuum is better than 2.0X10 -4 After Pa, cleaning a target material in a sputtering chamber by adopting Ar plasma for 10min, wherein the deposition pressure of the coating is 0.5Pa, the sputtering power of a Zr target is 100W, the sputtering power of a YSZ target is 200W, the target base distance is 100mm, simultaneously, sputtering the Zr target and the YSZ target material to deposit a Zr-YSZ diffusion layer together, after 30min of deposition, turning off a radio frequency power supply corresponding to the Zr target, and depositing a YSZ ceramic layer by using a single target for 1.5h;
(3) Co-depositing Zr-Y on the basis of step (2) 2 O 3 Dispersive layer, zr target sputtering power 100W, Y 2 O 3 Sputtering power of the targets is 200W, and Zr-Y is generated after three targets are sputtered for 30min 2 O 3 Diffusion layer, radio frequency power supply of Zr target and Y target is closed, single target sputtering deposition Y 2 O 3 A ceramic layer is deposited for 2 hours;
(4) Changing the target material into a Y target, an Al target and Al based on the sample obtained in the step (3) 2 O 3 Ceramic target, regulating Y target sputtering power to 100W, al 2 O 3 The sputtering power of the ceramic target is 250W, the other parameters are kept unchanged, and firstly three targets are sputtered for 30min to deposit Y-Al 2 O 3 Diffusion layer, then closing Y target and Al target, single target sputtering deposition Al 2 O 3 A ceramic layer is deposited for 2 hours;
(5) Carrying out Ar atmosphere heat treatment at 700 ℃ on the composite coating sample, and keeping the temperature for 2 hours to obtain Zr-YSZ/YSZ/Zr-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 The structure of the composite hydrogen-resistant coating is shown in figure 1.
The total thickness of the prepared composite coating is about 500nm, and the hydrogen permeation blocking factor of the coating is 600 at the permeation temperature of 700 ℃. The coating prepared in example 1 was subjected to a high temperature thermal shock cycle test from room temperature to 700 ℃ and Wen room temperature to one cycle, and after 50 cycles, the coating remained intact without cracking and flaking.
Example 2
GH4099 Zr-YSZ/YSZ/Zr-Y-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 Preparing a composite hydrogen-resistant coating:
(1) Selecting GH4099 nickel-based superalloy as a matrix, polishing one side of the matrix to a roughness of 1.5 mu m, cleaning and drying for later use;
(2) Zr-YSZ dispersion layer is prepared by magnetron co-sputtering, both targets are powered by a radio frequency power supply, ar is used as glow starting gas. When the back vacuum is better than 2.0X10 -4 After Pa, ar plasma is adopted to clean the target material in a sputtering chamber for 10min, the coating deposition pressure is 0.5Pa, the sputtering power of the Zr target is 100W, the sputtering power of the YSZ target is 250W, the target base distance is 100mm,simultaneously sputtering a Zr target and a YSZ target material to co-deposit a Zr-YSZ diffusion layer, closing a radio frequency power supply corresponding to the Zr target after 30min of deposition, and depositing a YSZ ceramic layer by a single target for 3h;
(3) Co-depositing Zr-Y on the basis of step (2) 2 O 3 Dispersive layer, zr target sputtering power 100W, Y 2 O 3 Sputtering power of the targets is 300W, and Zr-Y is generated after three targets are sputtered for 30min 2 O 3 Diffusion layer, radio frequency power supply of Zr target and Y target is closed, single target sputtering deposition Y 2 O 3 A ceramic layer is deposited for 3 hours;
(4) Changing the target material into a Y target, an Al target and Al based on the sample obtained in the step (3) 2 O 3 Ceramic target, regulating Y target sputtering power to 100W, al 2 O 3 The sputtering power of the ceramic target is 350W, the other parameters are kept unchanged, and firstly three targets are sputtered for 30min to deposit Y-Al 2 O 3 Diffusion layer, then closing Y target and Al target, single target sputtering deposition Al 2 O 3 A ceramic layer is deposited for 3 hours;
(5) Carrying out Ar atmosphere heat treatment at 1000 ℃ on the composite coating sample, and keeping the temperature for 2 hours to obtain Zr-YSZ/YSZ/Zr-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 The structure layout diagram of the composite hydrogen-resistant coating is shown in figure 1.
The total thickness of the prepared composite coating is about 800nm, and the hydrogen permeation blocking factor of the coating is 800 at the permeation temperature of 900 ℃. The coating prepared in example 2 was subjected to a high-temperature thermal shock cycle test, and after 50 cycles, the coating was free from cracking and flaking, and the hydrogen permeation barrier property was stabilized at 500h or more, from room temperature to 700 ℃ and Wen room temperature.
Example 3
304Zr-YSZ/YSZ/Zr-Y-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 Preparing a composite hydrogen-resistant coating:
(1) Selecting 304 stainless steel as a matrix, polishing one side of the matrix to a roughness of 1.5 mu m, cleaning and drying for later use;
(2) Zr-YSZ dispersion layer is prepared by magnetron co-sputtering, both targets are powered by a radio frequency power supply, ar is used as glow starting gas. When the back vacuum is better than 2.0X10 -4 After Pa, cleaning a target material in a sputtering chamber by adopting Ar plasma for 10min, wherein the deposition pressure of the coating is 0.5Pa, the sputtering power of a Zr target is 50W, the sputtering power of a YSZ target is 150W, the target base distance is 100mm, simultaneously, the Zr target and the YSZ target material are sputtered to deposit a Zr-YSZ diffusion layer together, after 30min of deposition, a radio frequency power supply corresponding to the Zr target is turned off, a YSZ ceramic layer is deposited by a single target, and the deposition time is 1.5h;
(3) Co-depositing Zr-Y on the basis of step (2) 2 O 3 Dispersed layer, zr target sputtering power 50W, Y 2 O 3 The sputtering power of the targets is 250W, and Zr-Y is generated after 30min of co-sputtering of the three targets 2 O 3 Diffusion layer, radio frequency power supply of Zr target and Y target is closed, single target sputtering deposition Y 2 O 3 A ceramic layer is deposited for 2 hours;
(4) Changing the target material into a Y target, an Al target and Al based on the sample obtained in the step (3) 2 O 3 Ceramic target, regulating Y target sputtering power to 50W, al 2 O 3 The sputtering power of the ceramic target is 200W, the other parameters are kept unchanged, and firstly three targets are sputtered for 30min to deposit Y-Al 2 O 3 Diffusion layer, then closing Y target and Al target, single target sputtering deposition Al 2 O 3 A ceramic layer is deposited for 3 hours;
(5) Carrying out Ar atmosphere heat treatment at 700 ℃ on the composite coating sample, and keeping the temperature for 2 hours to obtain Zr-YSZ/YSZ/Zr-Y 2 O 3 /Y 2 O 3 /Y-Al-Al 2 O 3 /Al 2 O 3 The structure layout diagram of the composite hydrogen-resistant coating is shown in figure 1.
The total thickness of the prepared composite coating is about 350nm, and the hydrogen permeation blocking factor of the coating is 500 at the permeation temperature of 700 ℃. The coating prepared in example 3 was subjected to a high-temperature thermal shock cycle test, and after 50 cycles, the coating was free from cracking and flaking, and the hydrogen permeation barrier property was stabilized at 300h or more, from room temperature to 700 ℃ and up to Wen room temperature.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. The multilayer gradient composite hydrogen-resistant coating is characterized by comprising at least 3 different oxide ceramic layers coated on a substrate, wherein different metal-oxide dispersion layers are arranged between the substrate and the oxide ceramic layers and between the adjacent oxide ceramic layers; the coating comprises the following components in sequence from the inner layer to the outer layer: zirconium-yttrium oxide stabilized zirconium oxide dispersion layer, yttrium oxide stabilized zirconium oxide layer, zr-Y 2 O 3 A dispersion layer, a yttrium oxide layer and Y-Al 2 O 3 A dispersion layer and an alumina layer; the atomic proportion of the metal phase in the dispersion layer is 40% -80%, and the total thickness of the hydrogen-resistant coating system is not more than 10 mu m.
2. The multilayer gradient composite hydrogen barrier coating of claim 1, wherein the substrate is 316L stainless steel, GH4099 nickel-based superalloy, or 304 stainless steel.
3. The multilayer gradient composite hydrogen barrier coating of claim 1, wherein the total thickness of the hydrogen barrier coating system is 0.1 μm to 1 μm.
4. The multilayer gradient composite hydrogen-resistant coating according to claim 1, wherein the thickness of the dispersion layer is 1/5-1/2 of the thickness of the oxide ceramic layer arranged on the outer layer.
5. A method for preparing the multilayer gradient composite hydrogen-resistant coating as claimed in claim 1, comprising the steps of:
(1) Polishing one side of the substrate to a roughness of 0.1-2 mu m;
(2) Co-sputter depositing a first metal-oxide diffusion layer on a substrate;
(3) Sputtering and depositing a first oxide ceramic layer on the coating prepared in the previous step;
(4) Coating different metal-oxide dispersion layers and oxide ceramic layers on the coating prepared in the previous step by alternately adopting a co-sputtering deposition and sputtering deposition method to obtain a composite coating with alternately overlapped metal-oxide dispersion layers and oxide ceramic layers, wherein the coating sequentially comprises the following components from an inner layer to an outer layer: zirconium-yttrium oxide stabilized zirconium oxide dispersion layer, yttrium oxide stabilized zirconium oxide layer, zr-Y 2 O 3 A dispersion layer, a yttrium oxide layer and Y-Al 2 O 3 A dispersion layer and an alumina layer;
(5) And (3) carrying out Ar atmosphere high-temperature heat treatment on the composite coating obtained in the step (4) and alternately overlapped with the metal-oxide dispersion layer and the oxide ceramic layer, and finally obtaining the multilayer gradient composite hydrogen-resistant coating.
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