CN112981323A - Aluminum oxide/erbium oxide ceramic coating composite system and preparation method thereof - Google Patents

Aluminum oxide/erbium oxide ceramic coating composite system and preparation method thereof Download PDF

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CN112981323A
CN112981323A CN201911275055.2A CN201911275055A CN112981323A CN 112981323 A CN112981323 A CN 112981323A CN 201911275055 A CN201911275055 A CN 201911275055A CN 112981323 A CN112981323 A CN 112981323A
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ceramic coating
oxide ceramic
coating
erbium oxide
sputtering
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于庆河
王维静
米菁
郝雷
李世杰
李帅
杜淼
王吉宁
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GRIMN Engineering Technology Research Institute 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
    • 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
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
    • 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
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to a hydrogen-resistant coating system and a preparation method thereof, in particular to an aluminum oxide and erbium oxide ceramic coating composite system and a preparation method thereof. The coating composite system comprises a substrate, an aluminum oxide ceramic coating and an erbium oxide ceramic coating which are sequentially coated on the substrate, or comprises the substrate and an even number of composite coatings which are formed by the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are sequentially coated on the substrate in an alternating manner. The composite coating is prepared by a vapor deposition method. The composite coating is formed by compounding an aluminum oxide ceramic layer and a metal erbium oxide ceramic layer, the preparation process of the coating is simple, the cost is low, the bonding performance with a substrate is good, the hydrogen resistance of the double-layer composite coating can be improved by more than 500 times at the working temperature of 600 ℃, and the good hydrogen resistance is shown.

Description

Aluminum oxide/erbium oxide ceramic coating composite system and preparation method thereof
Technical Field
The invention relates to a hydrogen-resistant coating system and a preparation method thereof, in particular to an aluminum oxide and erbium oxide ceramic coating composite system and a preparation method thereof.
Background
In the nuclear fusion reaction, deuterium and tritium as hydrogen isotopes are used as fuels of nuclear fusion, and the hydrogen isotopes have extremely strong permeability in a fusion blanket metal structure material due to small atomic radius, so that in order to prevent tritium from permeating from a proliferation agent to a coolant or from a pipeline to the environment, hydrogen-resistant coatings are coated on the inner wall of the tritium value-added blanket metal structure material and the inner wall of the pipeline to ensure the safety level of tritium in the environment and the coolant in a liquid tritium value-added blanket system. Common hydrogen barrier coatings are oxide ceramic coatings, nitride ceramic coatings, titanium-based ceramic coatings, and the like.
The structure of the hydrogen barrier coating is generally composed of two parts, namely a substrate and a coating. At present, the commonly used base material is stainless steel such as low-activity martensite or austenite and the like, and the preparation of the hydrogen-resistant coating is carried out on the base material, wherein the oxide ceramic coating can meet the design requirements of the coating material in the field of nuclear fusion reaction due to good high-temperature stability and excellent hydrogen resistance, so that the oxide ceramic coating is widely applied as an ideal candidate coating. In the prior art, an oxide ceramic coating is usually directly prepared on a base material, but due to the large difference of thermal expansion coefficients between the base material and the coating material, thermal stress mismatch is easily generated at a high temperature state, so that the coating is cracked and even peeled off, the hydrogen resistance of the coating is reduced, and hydrogen or isotopes thereof permeate into a metal structure material, so that the structure material is damaged by hydrogen, the physical performance of the structure material is reduced, and the service life of the structure material is shortened to a certain extent.
Disclosure of Invention
In order to overcome the defects of the existing coating system, the invention provides a composite coating system with superposed alumina and erbium oxide ceramic coatings and a preparation method thereof, wherein the gradient coating with moderate thermal expansion coefficient is introduced to relieve the influence of thermal stress on the coating at high temperature, and the alumina coating has strong hydrogen permeation resistance.
The composite coating system comprises a substrate, an aluminum oxide ceramic coating and an erbium oxide ceramic coating which are sequentially coated on the substrate, or comprises the substrate and an even number of layers of composite coatings which are formed by the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are sequentially coated on the substrate in an alternating mode.
Preferably, the substrate is a stainless steel structural material such as martensite or austenite with low activity.
Preferably, the crystalline state of the aluminum oxide is an amorphous state, the atomic distribution of the aluminum oxide is an amorphous structure with short-range order and long-range disorder, and no gamma phase, theta phase or alpha phase equivalent exists in the coating.
Preferably, the erbium oxide has a crystal structure, particularly a cubic phase crystal structure.
Preferably, the total thickness of the alumina ceramic coating and the erbium oxide ceramic coating does not exceed 5 μm, more preferably ranges from 0.1 to 5 μm.
Preferably, the thickness of the aluminum oxide ceramic coating and the erbium oxide ceramic coating respectively accounts for 1/2 of the total thickness of the coating.
On the other hand, the invention also provides a preparation method of the aluminum oxide/erbium oxide ceramic coating composite system, and the composite coating is prepared by adopting a vapor deposition method.
A preparation method of an aluminum oxide and erbium oxide ceramic coating composite system comprises the following steps:
(1) polishing one side of the substrate until the roughness is 0.1-2 mu m;
(2) preparing an alumina ceramic coating on a substrate by a vapor deposition method;
(3) preparing an erbium oxide ceramic coating on the aluminum oxide ceramic coating by a vapor deposition method;
(4) finally obtaining the double-layer composite coating consisting of the aluminum oxide ceramic coating and the erbium oxide ceramic coating.
In the preparation method of the invention, the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method.
Preferably, the physical vapor deposition method is a magnetron sputtering method.
More preferably, the magnetron sputtering method is a radio frequency magnetron sputtering method.
Preferably, the thickness of the double-layer composite coating consisting of the aluminum oxide ceramic coating and the erbium oxide ceramic coating is about 0.1-5 μm.
Preferably, the method further comprises the steps of:
(5) preparing a second aluminum oxide ceramic coating on the erbium oxide ceramic coating by a vapor deposition method; preparing a second erbium oxide ceramic coating on the second aluminum oxide ceramic coating by a vapor deposition method;
and repeating the steps to finally obtain the even-number composite coating formed by the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are mutually alternated.
Preferably, a four-layer composite coating consisting of the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are mutually alternated is finally obtained.
In the preparation method, the alumina ceramic coating is prepared by adopting a radio frequency magnetron sputtering method, and the preparation method comprises the following steps: taking an alumina ceramic target material as a sputtering target material, and carrying out magnetron sputtering on an alumina ceramic coating on a substrate; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, and reaction gas O is introduced after sputtering glow is stable2To compensate for oxygen vacancies, Ar/O, during coating deposition2The ratio of air pressure is 1-50, the sputtering power is 50-500W, and the sputtering air pressure0.1-10 Pa, and a target base distance of 10-200 mm.
In the preparation method, the erbium oxide ceramic coating is prepared by adopting a radio frequency magnetron sputtering method, and the preparation method comprises the following steps: performing magnetron sputtering on the aluminum oxide ceramic coating by taking the erbium oxide ceramic target as a sputtering target; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, and reaction gas O is introduced after sputtering glow is stable2To compensate for oxygen vacancies, Ar/O, during coating deposition2The air pressure ratio is 1-50, the sputtering power is 50-500W, the sputtering air pressure is 0.1-10 Pa, and the target base distance is 10-200 mm.
The invention has the beneficial effects that: according to the invention, by designing the aluminum oxide and erbium oxide composite coating system, on one hand, the introduction of the aluminum oxide ceramic coating solves the problem that the thermal expansion coefficients of a single-layer aluminum oxide coating and an erbium oxide coating are not matched when the single-layer aluminum oxide coating and the erbium oxide coating are directly contacted with a substrate, the generation of thermal stress can be effectively relieved under a high-temperature environment, and the cracking and peeling of the coating are avoided; in addition, when the aluminum oxide and erbium oxide coatings are alternately compounded, the introduction of the interface in the composite coating system can increase the permeation and diffusion energy barrier of hydrogen in the coating system and effectively slow down the diffusion and permeation rate of hydrogen, thereby improving the hydrogen resistance of the coating.
The composite coating system consisting of the aluminum oxide and erbium oxide ceramic coating is used for preventing or slowing down the permeation and diffusion rate of hydrogen by preparing on the surface of a stainless steel structural material with low activity, such as martensite or austenite, and particularly on a nuclear fusion reactor value-added cladding material taking hydrogen isotope deuterium and tritium as fuel. The composite coating is formed by sequentially arranging a stainless steel substrate, an aluminum oxide ceramic coating and an erbium oxide ceramic coating. The composite hydrogen-resistant coating can be prepared by a vapor deposition method, and the total thickness of the obtained composite coating is about 0.1-5 mu m thick double-layer composite coating; the coating is formed by compounding aluminum oxide and metal erbium oxide ceramic layers, the preparation process of the coating is simple, the cost is low, the bonding performance with a substrate is good, the hydrogen resistance of the double-layer composite coating can be improved by more than 500 times at the working temperature of 600 ℃, and the good hydrogen resistance is shown.
Drawings
FIG. 1 is a layout diagram of a double-layer alumina/erbium oxide ceramic coating composite structure.
FIG. 2 is a layout diagram of a four-layer alumina/erbium oxide ceramic coating composite structure.
Detailed description of the invention
As shown in figure 1, the aluminum oxide/erbium oxide ceramic coating composite system comprises a stainless steel substrate, an aluminum oxide ceramic coating and an erbium oxide ceramic coating which are sequentially arranged. Wherein the substrate material is low-activity austenite or martensite or other stainless steel materials, the aluminum oxide coating state is an amorphous state, and the erbium oxide coating state is a crystal structure. The total thickness of the alumina and erbium oxide ceramic coating is not more than 5 μm.
Because the difference of the thermal expansion coefficients of the base material and the oxide ceramic coating is large, the coating material prepared on the base material is easy to influence the cracking or peeling of the coating and the reliability of the coating due to large interlayer thermal stress. By introducing the alumina coating with moderate thermal expansion coefficient, on one hand, the generation of high-temperature thermal stress can be reduced, in addition, the alumina also has certain hydrogen resistance, the permeation and diffusion energy barrier of hydrogen is increased at the composite interface of the alumina and the erbium oxide ceramic coating, and the diffusion rate of hydrogen can be effectively slowed down, thereby improving the hydrogen resistance.
In the preparation process of the coating, a radio frequency magnetron sputtering method is selected, and the method comprises the following steps:
(1) polishing one surface of a stainless steel substrate until the roughness is 0.1-2 mu m;
(2) preparing an alumina ceramic coating on a substrate by a radio frequency magnetron sputtering method;
(3) preparing an erbium oxide ceramic coating on the aluminum oxide ceramic coating by a radio frequency magnetron sputtering method;
(4) finally, the double-layer composite coating consisting of the aluminum oxide and erbium oxide ceramic coating with the thickness of about 0.1-5 mu m is obtained.
The preparation method of the alumina ceramic coating comprises the following steps: taking an alumina ceramic target as a sputtering target; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, after the sputtering glow is stable,introducing reaction gas O2To compensate for oxygen vacancies, Ar/O, during coating deposition2The air pressure ratio is 5-50, the sputtering power is 100-500W, the sputtering air pressure is 0.1-10 Pa, and the target base distance is 10-200 mm.
The preparation method of the erbium oxide ceramic coating comprises the following steps: taking an erbium oxide ceramic target material as a sputtering target material; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, and reaction gas O is introduced after sputtering glow is stable2To compensate for oxygen vacancies, Ar/O, during coating deposition2The air pressure ratio is 5-50, the sputtering power is 100-500W, the sputtering air pressure is 0.1-10 Pa, and the target base distance is 10-200 mm.
Example 1: preparation of Al by radio frequency magnetron sputtering method2O3/Er2O3Ceramic coating composite system
(1) Selecting 316L stainless steel as a substrate, polishing one side of the substrate to the roughness of 0.1-2 mu m, and sputtering by adopting an alumina target material with the diameter of 100 mm;
(2) a mechanical pump and a molecular pump are adopted to carry out vacuum pumping operation on the magnetron sputtering chamber in sequence until the vacuum degree reaches 2.0 multiplied by 10-3Pa；
(3) Introducing working gas Ar gas, controlling the gas inflow rate to be 20sccm, and performing pre-sputtering to clean the surface of the target material;
(4) introducing reaction gas O2Regulating sputtering power to 250W, sputtering pressure to 0.5Pa, target base distance to 80mm during sputtering, and sputtering for 200min to obtain 187nm Al2O3A ceramic coating;
(5) replacing erbium oxide ceramic target, adopting the same technological parameters as alumina, sputtering for 240min, and performing sputtering on Al2O3Preparation of Er with thickness of 152nm on surface of ceramic coating2O3Ceramic coating to obtain double-layer Al with total thickness of 339nm2O3/Er2O3The structural layout of the composite coating is shown in figure 1.
The hydrogen resistance of the composite coating prepared in example 1 was tested, and the double-layer Al was formed at a penetration temperature of 600 deg.C2O3/Er2O3The hydrogen resistance of the composite coating is more than 500 times of that of a 316L austenitic stainless steel matrix, which shows that the double-layer Al2O3/Er2O3The composite coating has good hydrogen resistance, the coating prepared in example 1 is subjected to a high-temperature thermal shock cycle test, and after the same test sample is subjected to three times of cycle repeated tests from room temperature → 600 ℃ high temperature → room temperature → 600 ℃ high temperature, permeation blocking factors are 498, 512 and 509 in sequence, and the hydrogen resistance is similar.
Example 2: preparation of Al by radio frequency magnetron sputtering method2O3/Er2O3Ceramic coating composite system
(1) Selecting 316L stainless steel as a substrate, polishing one side of the substrate to the roughness of 0.1-2 mu m, and sputtering by adopting an alumina target material with the diameter of 100 mm;
(2) a mechanical pump and a molecular pump are adopted to carry out vacuum pumping operation on the magnetron sputtering chamber in sequence until the vacuum degree reaches 2.0 multiplied by 10-3Pa；
(3) Introducing working gas Ar gas, controlling the gas inflow rate to be 20sccm, and performing pre-sputtering to clean the surface of the target material;
(4) introducing reaction gas O2Regulating sputtering power to 250W, sputtering pressure to 0.5Pa, target base distance to 80mm during sputtering, and sputtering for 500min to obtain 467nm Al2O3A ceramic coating;
(5) replacing erbium oxide ceramic target, adopting the same technological parameters as alumina, sputtering for 700min, and performing sputtering on Al2O3Er with the thickness of 448nm prepared on the surface of the ceramic coating2O3Ceramic coating to obtain final double-layer Al with total thickness of 905nm2O3/Er2O3And (4) composite coating.
The hydrogen resistance of the composite coating prepared in example 2 was tested, and the double-layer Al was formed at a penetration temperature of 600 deg.C2O3/Er2O3The hydrogen barrier properties of the composite coating were 900 times that of the 316L austenitic stainless steel substrate, which was about 2 times that of the composite coating in example 1, indicating a double layer of Al2O3/Er2O3Hydrogen resistance of composite coating and coatingThe thickness increases in a direct proportion.
Example 3: preparation of Al by radio frequency magnetron sputtering method2O3/Er2O3/Al2O3/Er2O3Ceramic coating composite system
(1) Selecting 316L stainless steel as a substrate, polishing one side of the substrate to the roughness of 0.1-2 mu m, and sputtering by adopting an alumina target material with the diameter of 100 mm;
(2) a mechanical pump and a molecular pump are adopted to carry out vacuum pumping operation on the magnetron sputtering chamber in sequence until the vacuum degree reaches 2.0 multiplied by 10-3Pa；
(3) Introducing working gas Ar gas, controlling the gas inflow rate to be 20sccm, and performing pre-sputtering to clean the surface of the target material;
(4) introducing reaction gas O2Regulating sputtering power to 250W, sputtering pressure to 0.5Pa, target base distance to 80mm during sputtering, and sputtering for 200min to obtain 187nm Al2O3A ceramic coating;
(5) replacing erbium oxide ceramic target, adopting the same technological parameters as alumina, sputtering for 240min, and performing sputtering on Al2O3Preparation of Er with thickness of 152nm on surface of ceramic coating2O3A ceramic coating is coated on the surface of the ceramic substrate,
(6) repeating the steps (4) and (5) to finally obtain four layers of Al with the total thickness of 678nm2O3/Er2O3/Al2O3/Er2O3The structural layout of the composite coating is shown in FIG. 2.
The hydrogen resistance of the composite coating prepared in example 3 was tested, and four layers of Al were applied at a penetration temperature of 600 deg.C2O3/Er2O3/Al2O3/Er2O3The hydrogen resistance of the composite coating is more than 800 times that of a 316L austenitic stainless steel matrix, and the composite coating shows good hydrogen resistance.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.

Claims (10)

1. An aluminum oxide and erbium oxide ceramic coating composite system is characterized in that: the coating comprises a substrate, and an aluminum oxide ceramic coating and an erbium oxide ceramic coating which are sequentially coated on the substrate, or comprises the substrate and an even number of composite coatings which are formed by the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are sequentially coated on the substrate and alternate with each other.
2. The alumina and erbium oxide ceramic coating composite system according to claim 1, characterized in that: the matrix is martensitic or austenitic stainless steel.
3. The alumina and erbium oxide ceramic coating composite system according to claim 1, characterized in that: the atomic distribution of the aluminum oxide is an amorphous structure with short-range order and long-range disorder; the erbium oxide has a cubic phase crystal structure.
4. The alumina and erbium oxide ceramic coating composite system according to claim 1, characterized in that: the total thickness of the aluminum oxide ceramic coating and the erbium oxide ceramic coating is not more than 5 mu m.
5. A method of preparing an alumina and erbium oxide ceramic coating composite system according to any of claims 1-4, characterized in that: the composite coating is prepared by a vapor deposition method.
6. The method of preparing an alumina and erbium oxide ceramic coating composite system according to claim 5, comprising the steps of:
(1) polishing one side of the substrate until the roughness is 0.1-2 mu m;
(2) preparing an alumina ceramic coating on a substrate by a vapor deposition method;
(3) preparing an erbium oxide ceramic coating on the aluminum oxide ceramic coating by a vapor deposition method;
(4) obtaining a double-layer composite coating consisting of an aluminum oxide ceramic coating and an erbium oxide ceramic coating with the thickness of 0.1-5 mu m.
7. The method of preparing an alumina and erbium oxide ceramic coating composite system according to claim 6, characterized in that: the method further comprises the following steps:
(5) preparing a second aluminum oxide ceramic coating on the erbium oxide ceramic coating by a vapor deposition method; preparing a second erbium oxide ceramic coating on the second aluminum oxide ceramic coating by a vapor deposition method;
and repeating the steps to finally obtain the even-number composite coating formed by the aluminum oxide ceramic coating and the erbium oxide ceramic coating which are mutually alternated.
8. The method of preparing an alumina and erbium oxide ceramic coating composite system according to claim 6, characterized in that: the vapor deposition method is a physical vapor deposition method or a chemical vapor deposition method; the physical vapor deposition method is a magnetron sputtering method; the magnetron sputtering method is a radio frequency magnetron sputtering method.
9. A method of preparing an alumina and erbium oxide ceramic coating composite system according to any of the claims 6, characterized in that: the method for preparing the alumina ceramic coating by adopting the radio frequency magnetron sputtering method comprises the following steps: taking an alumina ceramic target material as a sputtering target material, and carrying out magnetron sputtering on an alumina ceramic coating on a substrate; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, and reaction gas O is introduced after sputtering glow is stable2To compensate for oxygen vacancies, Ar/O, during coating deposition2The air pressure ratio is 1-50, the sputtering power is 50-500W, the sputtering air pressure is 0.1-10 Pa, and the target base distance is 10-200 mm.
10. The method of preparing an alumina and erbium oxide ceramic coating composite system according to claim 6, characterized in that:the erbium oxide ceramic coating is prepared by adopting a radio frequency magnetron sputtering method, and comprises the following steps: performing magnetron sputtering on the aluminum oxide ceramic coating by taking the erbium oxide ceramic target as a sputtering target; firstly, pre-vacuuming to 10-6～10-2Pa; then Ar gas is introduced for pre-sputtering, and reaction gas O is introduced after sputtering glow is stable2To compensate for oxygen vacancies, Ar/O, during coating deposition2The air pressure ratio is 1-50, the sputtering power is 50-500W, the sputtering air pressure is 0.1-10 Pa, and the target base distance is 10-200 mm.
CN201911275055.2A 2019-12-12 2019-12-12 Aluminum oxide/erbium oxide ceramic coating composite system and preparation method thereof Pending CN112981323A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
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US20080131711A1 (en) * 2006-12-01 2008-06-05 Siemens Power Generation, Inc. Bond coat compositions and arrangements of same capable of self healing
CN101469409A (en) * 2007-12-27 2009-07-01 北京有色金属研究总院 Composite aluminum oxide /erbium hydrogen resistance coating and preparation thereof
CN104070718A (en) * 2014-07-14 2014-10-01 四川材料与工艺研究所 Tritium-blocking plating and preparation method thereof
CN105729934A (en) * 2014-12-11 2016-07-06 北京有色金属研究总院 M/MOx composite hydrogen resistance coating and preparation method thereof
CN107043905A (en) * 2016-02-06 2017-08-15 北京有色金属研究总院 A kind of metal hydride surface recombination hydrogen permeation barrier and preparation method thereof
CN108531907A (en) * 2016-07-15 2018-09-14 应用材料公司 Has the laminated coating of diffused barrier layer and anti-erosion layer

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080131711A1 (en) * 2006-12-01 2008-06-05 Siemens Power Generation, Inc. Bond coat compositions and arrangements of same capable of self healing
CN101469409A (en) * 2007-12-27 2009-07-01 北京有色金属研究总院 Composite aluminum oxide /erbium hydrogen resistance coating and preparation thereof
CN104070718A (en) * 2014-07-14 2014-10-01 四川材料与工艺研究所 Tritium-blocking plating and preparation method thereof
CN105729934A (en) * 2014-12-11 2016-07-06 北京有色金属研究总院 M/MOx composite hydrogen resistance coating and preparation method thereof
CN107043905A (en) * 2016-02-06 2017-08-15 北京有色金属研究总院 A kind of metal hydride surface recombination hydrogen permeation barrier and preparation method thereof
CN108531907A (en) * 2016-07-15 2018-09-14 应用材料公司 Has the laminated coating of diffused barrier layer and anti-erosion layer

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Application publication date: 20210618