CN116515326B - Al (aluminum) alloy 2 O 3 -TiO 2 -B 2 O 3 Preparation method of composite oxide hydrogen-resistant coating - Google Patents
Al (aluminum) alloy 2 O 3 -TiO 2 -B 2 O 3 Preparation method of composite oxide hydrogen-resistant coating Download PDFInfo
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- CN116515326B CN116515326B CN202211569199.0A CN202211569199A CN116515326B CN 116515326 B CN116515326 B CN 116515326B CN 202211569199 A CN202211569199 A CN 202211569199A CN 116515326 B CN116515326 B CN 116515326B
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- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 239000011248 coating agent Substances 0.000 title claims abstract description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000001257 hydrogen Substances 0.000 title claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 9
- 229910045601 alloy Inorganic materials 0.000 title claims description 4
- 239000000956 alloy Substances 0.000 title claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 4
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000003980 solgel method Methods 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000003570 air Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000004888 barrier function Effects 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 2
- 229940009827 aluminum acetate Drugs 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 238000009423 ventilation Methods 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 3
- 229910003077 Ti−O Inorganic materials 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- JWZCKIBZGMIRSW-UHFFFAOYSA-N lead lithium Chemical compound [Li].[Pb] JWZCKIBZGMIRSW-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Chemical Treatment Of Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses an Al 2 O 3 ‑TiO 2 ‑B 2 O 3 The preparation method of the composite oxide hydrogen-resistant coating comprises the steps of firstly preparing soluble salts of Al, ti and B into high-activity composite oxide precursor powder by combining a sol-gel method with low-temperature oxidation sintering, forming a coating with a certain thickness on the surface of a target sample piece by spray drying, and then carrying out low-temperature heat treatment by utilizing B 2 O 3 Low melting point property promoting Al 2 O 3 TiO (titanium dioxide) 2 Sintering to form the composite oxide hydrogen-resistant coating. The invention uses a precursor with high activity formed by sol-gel to add B 2 O 3 The low melting point characteristic of the aluminum alloy is that the sintering temperature of Al-Ti-O is effectively reduced, the preparation of a compact hydrogen-resistant coating is realized at a lower temperature, and the bonding effect between the coating and a matrix is improved; the method has the advantages of low cost, simple operation, excellent hydrogen resistance effect and the like.
Description
Technical Field
The invention belongs to the technical field of hydrogen-resistant coatings, and particularly relates to a preparation method of a composite oxide coating.
Background
Al 2 O 3 The method has the advantages of good hydrogen prevention and isotope permeability, high resistivity, high temperature resistance, good compatibility with lithium lead and the like, and becomes a research hot spot of the hydrogen-resistant coating. In order to achieve good hydrogen permeation resistance and corrosion resistance, the alpha-Al is prepared by sintering at high temperature 2 O 3 Realizing compact coating and good film/base combination. But the sintering temperature of the iron-based substrate is not higher than 800 ℃ in general, and thus the alpha-Al 2 O 3 Too high sintering temperature>1000 c) in turn can present challenges to the manufacturing process of the coating material and the suitability of the substrate material. Thus, low temperature preparation of α -Al was sought 2 O 3 The new process of the membrane is critical.
Disclosure of Invention
In order to solve the problems, the present invention provides an Al with a low densification sintering temperature 2 O 3 -TiO 2 -B 2 O 3 A preparation method of a composite oxide hydrogen-resistant coating.
The invention realizes the above purpose through the following technical scheme:
al (aluminum) alloy 2 O 3 -TiO 2 -B 2 O 3 The preparation method of the composite oxide hydrogen-resistant coating comprises the following steps:
step 1: mixing soluble salts of Al, ti and B through a sol-gel method to prepare xerogel, and performing presintering through heat treatment to form high-activity composite oxide precursor powder;
step 2: uniformly mixing the precursor powder obtained in the step 1 with a solvent and a thickener, spraying the mixture on the surface of a sample by a spraying method to form a coating, and drying;
step 3: performing low-temperature heat treatment on the sample in the step 2, and utilizing B 2 O 3 Low melting point property promoting Al 2 O 3 TiO (titanium dioxide) 2 Sintering, i.e. forming Al on the surface of the sample 2 O 3 -TiO 2 -B 2 O 3 A composite oxide hydrogen barrier coating.
Further, al in the formed hydrogen-resistant coating 2 O 3 40-70% of TiO 2 20-50% by mass of B 2 O 3 The mass percentage is 5-30%.
Further, the thickness of the hydrogen-resistant coating is 0.1-100 micrometers.
Further, the soluble salt of Al is aluminum nitrate or aluminum acetate, the soluble salt of Ti is n-butyl titanate, and the soluble salt of B is boric acid.
Further, the method for preparing xerogel in the step 1 comprises the following steps: mixing and dissolving soluble salts of Al, ti and B in deionized water or a mixed solution of deionized water and ethanol, adding a complexing agent, regulating the pH to 5-6.5 by using ammonia water or nitric acid, heating and stirring to form a viscous sol, and drying in an oven at 100-140 ℃ to form xerogel. Wherein the complexing agent is at least one of citric acid, ethylenediamine tetraacetic acid and polyvinyl alcohol.
Further, in the step 1, the heat treatment is sintering for 30-300 minutes at 200-600 ℃ under air or oxygen atmosphere.
Further, in the step 2, the solvent comprises at least one of deionized water, ethanol, acetone, ethylene glycol and monomethyl dipyrrolidone, and the thickener is at least one of triethanolamine, polyethylene glycol, dibutyl phthalate, polyvinyl butyral, polyvinylidene fluoride, polytetrafluoroethylene and sodium carboxymethyl cellulose.
Further, in step 2, the spraying method comprises the following steps: spraying the powder dispersed in the solvent on the surface of the sample at the temperature of 10-90 ℃ by high-pressure air, oxygen or nitrogen, and drying by ventilation at the temperature of 10-50 ℃.
Further, in the step 3, the low-temperature heat treatment is to sinter at 600-800 ℃ for 30-300 minutes under the atmosphere of air or oxygen.
The invention has the beneficial effects that:
the invention uses a precursor with high activity formed by sol-gel to add B 2 O 3 The low melting point characteristic of the aluminum alloy is that the sintering temperature of Al-Ti-O is effectively reduced, the preparation of a compact hydrogen-resistant coating is realized at a lower temperature, and the bonding effect between the coating and a matrix is improved; the method has the advantages of low cost, simple operation, excellent hydrogen resistance effect and the like.
Drawings
FIG. 1 is an Al alloy prepared in example 1 of the present invention 2 O 3 (70%)-TiO 2 (20%)-B 2 O 3 The appearance of the composite oxide hydrogen-resistant coating is (10%), and the coating is tightly combined with the matrix, has no obvious interface pores and is compact in the interior of the coating.
Detailed Description
The invention will now be described in further detail with reference to the following examples, it being necessary to note that the following detailed description is given for the purpose of illustration only and is not to be construed as limiting the scope of the invention, as numerous insubstantial modifications and adaptations of the invention are possible in light of the above disclosure by those skilled in the art.
Example 1
This example prepares an Al 2 O 3 (70%)-TiO 2 (20%)-B 2 O 3 (10%) a composite oxide hydrogen barrier coating comprising the steps of:
step 1: weighing Al (NO) according to the target mass ratio 3 ) 3 N-butyl titanate, boric acid and dissolving in deionized water according to the molar ratio of the total metal salt to citric acid of 1:1 adding citric acid and adding ammonia water to adjust the pH value to 6. The solution was heated and stirred at 80 ℃ until a viscous sol was formed, and then dried in a 100 ℃ oven to form a xerogel. And grinding and crushing the xerogel, and sintering for 1h at 500 ℃ in the atmosphere of air in a muffle furnace to obtain the precursor powder.
Step 2: the volume ratio of ethanol to glycol is 8:2, adding precursor powder into the mixed solution with the solid content of 20 percent, adding 5 weight percent of polyethylene glycol and 5 weight percent of polyvinyl butyral, fully stirring and mixing, uniformly spraying the mixture on the surface of an iron-based sample in an oven with the temperature of 50 ℃ by using a high-pressure air gun, and airing at room temperature.
Step 3: placing the sample in the step 2 into a muffle furnace, and sintering at 700 ℃ for 5 hours in an air atmosphere to form Al on the surface of the sample 2 O 3 (70%)-TiO 2 (20%)-B 2 O 3 And (10 percent) the composite oxide hydrogen-resistant coating is compact, has the thickness of about 1 micron, is tightly combined with the matrix, and has no obvious pores at the interface. The hydrogen permeation reduction factor of the coating was measured by a gas phase hydrogen permeation device at room temperature to result in about 2450.
Example 2
This example prepares an Al 2 O 3 (40%)-TiO 2 (30%)-B 2 O 3 (30%) a composite oxide hydrogen barrier coating comprising the steps of:
step 1: weighing Al (NO) according to the target mass ratio 3 ) 3 N-butyl titanate, boric acid and dissolved in deionized water and ethanol in a volume ratio of 8:2 in the mixed solution according to the mole ratio of the total metal salt to the citric acid of 1:1.3 adding citric acid and adding ammonia water to adjust the pH value to 5.5. The solution was heated to 90 ℃ with stirring until the solution formed a viscous sol and was dried in an oven at 140 ℃ to form a xerogel. Grinding and crushing the xerogel, and sintering for 2 hours at 450 ℃ in an atmosphere furnace under the oxygen atmosphere to obtain precursor powder.
Step 2: the volume ratio of the acetone to the glycol is 1:1, adding precursor powder into the mixed solution to make the solid content of the precursor powder be 10%, adding 10wt% of triethanolamine and 5wt% of polyethylene glycol, fully stirring and mixing, uniformly spraying the mixture on the surface of an iron-based sample at room temperature by using a high-pressure nitrogen spray gun, and airing the mixture in a baking oven at 40 ℃.
Step 3: placing the sample in the step 2 in a muffle furnace, and sintering at 800 ℃ for 1h in an oxygen atmosphere to form Al on the surface of the sample 2 O 3 (40%)-TiO 2 (30%)-B 2 O 3 (30%) of a composite oxide hydrogen-resistant coating. The hydrogen permeation reduction factor of the coating was measured by a gas phase hydrogen permeation device at room temperature and resulted in about 2100.
Comparative example 1
Comparative example A is preparedl 2 O 3 (70%)-TiO 2 (30%) a composite oxide hydrogen barrier coating comprising the steps of:
step 1: weighing Al (NO) according to the target mass ratio 3 ) 3 N-butyl titanate is dissolved in deionized water according to the molar ratio of the total metal salt to citric acid of 1:1 adding citric acid and adding ammonia water to adjust the pH value to 6. The solution was heated and stirred at 80 ℃ until a viscous sol was formed, and then dried in a 100 ℃ oven to form a xerogel. And grinding and crushing the xerogel, and sintering for 1h at 500 ℃ in the atmosphere of air in a muffle furnace to obtain the precursor powder.
Step 2: the volume ratio of ethanol to glycol is 8:2, adding precursor powder into the mixed solution with the solid content of 20 percent, adding 5 weight percent of polyethylene glycol and 5 weight percent of polyvinyl butyral, fully stirring and mixing, uniformly spraying the mixture on the surface of an iron-based sample in an oven with the temperature of 50 ℃ by using a high-pressure air gun, and airing at room temperature.
Step 3: and (3) placing the sample piece in the step (2) in a muffle furnace, and sintering for 5 hours at 700 ℃ in an air atmosphere, wherein the surface of the sample piece only forms a pulverized and loose coating due to the fact that the sintering temperature is too low and no auxiliary flux exists.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (4)
1. Al (aluminum) alloy 2 O 3 -TiO 2 -B 2 O 3 The preparation method of the composite oxide hydrogen-resistant coating is characterized by comprising the following steps of:
step 1: mixing soluble salt of Al, n-butyl titanate and boric acid through a sol-gel method to prepare xerogel, and performing presintering through heat treatment to form high-activity composite oxide precursor powder; the soluble salt of Al is aluminum nitrate or aluminum acetate; wherein:
the method for preparing the xerogel comprises the following steps: mixing soluble salt of Al, n-butyl titanate and boric acid, dissolving in deionized water or a mixed solution of deionized water and ethanol, adding a complexing agent, regulating the pH to 5-6.5 by using ammonia water or nitric acid, heating and stirring to form a viscous sol, and drying in an oven at 100-140 ℃ to form xerogel;
the heat treatment is sintering for 30-300 minutes at 200-600 ℃ under air or oxygen atmosphere;
step 2: uniformly mixing the precursor powder obtained in the step 1 with a solvent and a thickener, spraying the mixture on the surface of a sample by a spraying method to form a coating, and drying;
the solvent comprises at least one of deionized water, ethanol, acetone and ethylene glycol, and the thickener comprises at least one of triethanolamine, polyethylene glycol, polyvinyl butyral and sodium carboxymethyl cellulose;
step 3: carrying out low-temperature heat treatment on the sample in the step 2, namely forming Al on the surface of the sample 2 O 3 -TiO 2 -B 2 O 3 A composite oxide hydrogen barrier coating; al in the formed hydrogen-resistant coating 2 O 3 40-70% of TiO 2 20-50% by mass of B 2 O 3 The mass percentage is 5-30%; the low-temperature heat treatment is sintering at 600-800 ℃ for 30-300 minutes under the atmosphere of air or oxygen.
2. The method of manufacturing according to claim 1, characterized in that: the thickness of the hydrogen-resistant coating is 0.1-100 micrometers.
3. The method of manufacturing according to claim 1, characterized in that: the complexing agent is at least one of citric acid, ethylenediamine tetraacetic acid and polyvinyl alcohol.
4. The method according to claim 1, wherein in step 2, the spraying method is as follows: spraying the powder dispersed in the solvent on the surface of the sample at the temperature of 10-90 ℃ by high-pressure air, oxygen or nitrogen, and drying by ventilation at the temperature of 10-50 ℃.
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CN113978056A (en) * | 2021-10-15 | 2022-01-28 | 北京科技大学 | Vanadium alloy |
CN114163850A (en) * | 2021-12-15 | 2022-03-11 | 河南爱邦科技有限公司 | Composite material metal high-temperature-resistant anti-oxidation coating and preparation method thereof |
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US9644273B2 (en) * | 2007-02-09 | 2017-05-09 | Honeywell International Inc. | Protective barrier coatings |
US9062564B2 (en) * | 2009-07-31 | 2015-06-23 | General Electric Company | Solvent based slurry compositions for making environmental barrier coatings and environmental barrier coatings comprising the same |
US8501840B2 (en) * | 2009-07-31 | 2013-08-06 | General Electric Company | Water based slurry compositions for making environmental barrier coatings and environmental barrier coatings comprising the same |
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CN113978056A (en) * | 2021-10-15 | 2022-01-28 | 北京科技大学 | Vanadium alloy |
CN114163850A (en) * | 2021-12-15 | 2022-03-11 | 河南爱邦科技有限公司 | Composite material metal high-temperature-resistant anti-oxidation coating and preparation method thereof |
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