CN117587389A - Preparation method of aluminum oxide-based anti-corrosion coating on surface of 310S stainless steel - Google Patents
Preparation method of aluminum oxide-based anti-corrosion coating on surface of 310S stainless steel Download PDFInfo
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- CN117587389A CN117587389A CN202311627819.6A CN202311627819A CN117587389A CN 117587389 A CN117587389 A CN 117587389A CN 202311627819 A CN202311627819 A CN 202311627819A CN 117587389 A CN117587389 A CN 117587389A
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- 239000010935 stainless steel Substances 0.000 title claims abstract description 71
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 71
- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000005260 corrosion Methods 0.000 title claims description 19
- 238000002360 preparation method Methods 0.000 title claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 50
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000004411 aluminium Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract 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 27
- 230000007797 corrosion Effects 0.000 claims description 17
- 150000003839 salts Chemical class 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 description 7
- 229910000951 Aluminide Inorganic materials 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000010248 power generation Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001935 peptisation Methods 0.000 description 3
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 2
- 229910000943 NiAl Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 150000001398 aluminium Chemical class 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 208000016261 weight loss Diseases 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 229910001119 inconels 625 Inorganic materials 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 208000020442 loss of weight Diseases 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
Classifications
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1225—Deposition of multilayers of inorganic material
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
Abstract
Preparing a pseudo-boehmite aqueous solution, performing ultrasonic dispersion, dropwise adding a nitric acid solution to form semitransparent aluminum sol, adding a preset amount of PEG, and continuously stirring to obtain stable aluminum sol; step (2) cleaning the 310S stainless steel with ethanol and deionized water, immersing the stainless steel in aluminum sol, carrying out chemical bath at 60-90 ℃ for 1-4 hours, washing with ethanol, and drying to obtain the 310S stainless steel with the surface modified aluminum sol; performing heat treatment on the obtained stainless steel in an air atmosphere, and cooling along with a furnace to obtain 310S stainless steel with a uniform and compact aluminum oxide coating on the surface; step (4) adding tetraethoxysilane, or nanometer ZrC or nanometer ZrB into the aluminum sol obtained in the step (1) respectively 2 The particles are stirred to obtain silicon doped aluminum sol, zrC-aluminum sol or ZrB 2 -an aluminium sol; and (3) repeating the step (3) to obtain the 310S stainless steel modified by the uniform and compact coating.
Description
Technical Field
The invention relates to a preparation technology of a functional coating, in particular to a preparation technology of an alumina-based anticorrosive coating on the surface of stainless steel.
Background
The solar thermal power generation technology uses more molten salt as nitrate, the working temperature of the system is usually 280-560 ℃, but the condensation temperature of the existing tower type photo-thermal power generation system can reach more than 800 ℃, and the nitrate can not completely meet the system requirement. The chloride molten salt is expected to become heat storage molten salt for the next generation photo-thermal power generation system due to the excellent characteristics, but the corrosion of the chloride molten salt is extremely strong, and the chloride molten salt has higher requirements on the corrosion resistance of metal parts for photo-thermal power generation in a high-temperature chloride molten salt environment.
With the development of alloy materials, the space for improving the high-temperature performance and corrosion resistance of the nickel-based alloy by a material modification method is very limited; while superalloys such as Inconel 625 have better molten salt corrosion resistance, the high cost limits their widespread use in CSP systems. Therefore, the high-temperature-resistant anticorrosive coating is deposited on the surface of the stainless steel as a key component material of the photo-thermal power station, the service life of the photo-thermal power station is prolonged, and corrosion and high-temperature oxidation of the surface in the chloride molten salt are prevented to become the most effective way. Aluminide coatings have low density, high melting point, excellent mechanical properties and high temperature corrosion resistance, and become one of the most potential coatings.
Currently, aluminide coating is prepared by various methods, mainly Physical Vapor Deposition (PVD), chemical Vapor Deposition (CVD), magnetron sputtering, thermal spraying, cold spraying, plasma spraying, laser cladding, hot dip aluminum, 3D printing, and the like. The above methods have respective advantages such as strong binding force between the coating and the substrate, compact coating, controllable composition, etc., but also have disadvantages such as high requirements on equipment, high preparation cost, limited thickness of the coating, etc. Thus, there is a need to develop a simple, convenient, low cost method of preparing coatings.
The patent CN201910026394.0 proposes a preparation method of a high-frequency induction assisted self-propagating NiAl intermetallic compound coating, which has relatively complex preparation process, needs mixing, compacting, high-frequency induction heating, drying for 15 h, generates high vacuum environment, generates high pressure of 20-40 MPa and the like, and has certain danger. Patent CN202011410297.0 proposes a reactive element Hf modifiedβ-NiAl coating and process for its preparation, the method: composite plating a Ni-Hf layer on the substrate; depositing an Al layer on the obtained Ni-Hf layer using arc ion plating; annealing the obtained electroplated Ni-Hf+ arc ion plating deposited Al layer in a vacuum annealing furnace to obtain Hf modified AlβThe whole process flow is complicated, and the equipment requirement is high. Chemical bath is a simple technique for preparing films by combining dip-pull-coating, which is simple to operate and has low equipment requirements, and the application of the chemical bath to the preparation of aluminide coatings on stainless steel surfaces is a very effective means. On the premise of preparing aluminide coating chemical bath of aluminium sol, patent 202310444877.9 proposes a modified aluminium sol and a preparation method thereof, wherein the method utilizes aluminium chloride to prepare an aluminium trichloride solution, then adds concentrated ammonia water for precipitation, suction filtration and washing, then adds the aluminium trichloride solution, heats to 60 ℃ for peptizing to obtain the aluminium sol, adds auxiliary components under stirring condition, and carries out heat preservation reaction for 3 h to finally obtain the modified aluminium sol. The preparation of the traditional aluminum sol requires the steps of precipitation, filtration, washing, re-acidification, peptization, aging and the like, and the stable aluminum sol is obtained in one step by directly utilizing pseudo-boehmite (SB powder) nitrate to acidify peptization and then adding a PEG stabilizer. And then the 310S stainless steel is immersed in the aluminum sol by means of a chemical bath, and the 310S stainless steel with excellent corrosion resistance and modified aluminum oxide coating can be obtained after drying and calcining. In addition, by adding Si, nano ZrC and ZrB into the aluminum sol 2 And the nano ceramic powder further enhances the corrosion resistance of the coating.
Disclosure of Invention
The invention aims to provide a preparation method of an alumina-based anticorrosive coating on the surface of 310S stainless steel.
The invention relates to a preparation method of an alumina-based anticorrosive coating on the surface of 310S stainless steel, which comprises the following steps:
step (1) preparing pseudo-boehmite aqueous solution with the concentration of 0.1-10 mol/L; after ultrasonic dispersion, dropwise adding a nitric acid solution, wherein the nitric acid concentration is 0.01-0.5 mol/L, continuously stirring for 2-4 hours at 85 ℃ to form semitransparent aluminum sol, adding a preset amount of PEG, and continuously stirring to obtain stable aluminum sol, wherein the molecular weight of the PEG is 2000 and the mass fraction of the PEG is 0.1-1 wt%;
step (2) cleaning the cleaned 310S stainless steel with ethanol and deionized water, immersing the cleaned 310S stainless steel in the aluminum sol obtained in the step, carrying out chemical bath at 60-90 ℃ for 1-4 hours, and washing and drying the aluminum sol with ethanol to obtain the 310S stainless steel with the surface modified aluminum sol;
performing heat treatment on the obtained stainless steel in an air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating to 800-1100 ℃ for 2 h, and cooling with a furnace at a heating rate of 5 ℃ per minute to obtain 310S stainless steel with a uniformly dense aluminum oxide coating modified surface;
step (4) adding a preset amount of tetraethoxysilane, or nano ZrC or nano ZrB into the aluminum sol obtained in the step (1) respectively 2 The particles are 1 wt to 5 wt percent of doped/compounded amount, and the silicon doped aluminum sol, or ZrC-aluminum sol, or ZrB can be obtained after stirring for a preset time 2 -an aluminium sol; repeating the step (3) to obtain uniform and compact silicon-alumina, zrC-alumina and ZrB 2 Aluminum oxide coating modified 310S stainless steel.
The beneficial effects of the invention are as follows: the stable aluminum sol can be obtained through one-step acidification peptization, and the aluminide coating can be modified on the surface of the 310S stainless steel through a chemical bath and heat treatment mode. In addition, tetraethoxysilane, zrC and ZrB are added into the aluminum sol 2 The nano ceramic powder can be used for obtaining the Si doped alumina, zrC and ZrB 2 A nano ceramic phase reinforced alumina corrosion resistant coating. The method is simple, quick and low in cost, and has the industrialization of preparing the corrosion-resistant coating on the stainless steel surfaceAnd popularization prospect.
Drawings
FIG. 1 is an alumina sol prepared in example 1, FIG. 2 is a Si-doped alumina sol prepared in example 2, FIG. 3 is a ZrC-alumina sol prepared in example 3, and FIG. 4 is a ZrB prepared in example 4 2 -an aluminium sol, fig. 1-4 being comparative samples of a set of experiments; FIG. 5 is an alumina coating modified 310S stainless steel obtained in example 1, FIG. 6 is Si-Al obtained in example 2 2 O 3 Coating-modified 310S stainless steel, FIG. 7 shows ZrC-Al obtained in example 3 2 O 3 Coating-modified 310S stainless steel, FIG. 8 is ZrB obtained in example 4 2 -Al 2 O 3 Coating-modified 310S stainless steel, fig. 5-8 are comparative samples of a set of experiments; FIG. 9 is a graph of the loss of weight of a coating-modified stainless steel at 800℃in high temperature chloride molten salt corrosion.
Description of the embodiments
The invention relates to a preparation method of an alumina-based anticorrosive coating on the surface of 310S stainless steel, which comprises the following steps:
step (1) preparing pseudo-boehmite aqueous solution with the concentration of 0.1-10 mol/L; after ultrasonic dispersion, dropwise adding a nitric acid solution, wherein the nitric acid concentration is 0.01-0.5 mol/L, continuously stirring for 2-4 hours at 85 ℃ to form semitransparent aluminum sol, adding a preset amount of PEG, and continuously stirring to obtain stable aluminum sol, wherein the molecular weight of the PEG is 2000 and the mass fraction of the PEG is 0.1-1 wt%;
step (2) cleaning the cleaned 310S stainless steel with ethanol and deionized water, immersing the cleaned 310S stainless steel in the aluminum sol obtained in the step, carrying out chemical bath at 60-90 ℃ for 1-4 hours, and washing and drying the aluminum sol with ethanol to obtain the 310S stainless steel with the surface modified aluminum sol;
performing heat treatment on the obtained stainless steel in an air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating to 800-1100 ℃ for 2 h, and cooling with a furnace at a heating rate of 5 ℃ per minute to obtain 310S stainless steel with a uniformly dense aluminum oxide coating modified surface;
step (4) adding a preset amount of tetraethoxysilane, or nano ZrC or nano ZrB into the aluminum sol obtained in the step (1) respectively 2 The particle, the doping/compounding amount is 1 wt-5 wt%, and the mixture is stirred for presettingAfter the time, the silicon doped aluminum sol, or ZrC-aluminum sol, or ZrB can be obtained 2 -an aluminium sol; repeating the step (3) to obtain uniform and compact silicon-alumina, zrC-alumina and ZrB 2 Aluminum oxide coating modified 310S stainless steel.
The preparation method has the advantages that the nanometer ZrC is 30 nm particles, and the nanometer ZrB 2 20 nm granules.
According to the preparation method, when the obtained 310S stainless steel modified by the alumina-based coating is subjected to a 800 ℃ high-temperature chloride molten salt corrosion test, compared with unmodified stainless steel, the modified stainless steel has excellent chloride high-temperature resistance.
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the embodiments, but the present invention is not limited to these embodiments.
Example 1: in this example, the concentration of SB powder was 1 mol/L and the concentration of nitric acid was 0.5 mol/L, stirring was continued at 85deg.C for 4. 4 h to form a semitransparent alumina sol, and a certain amount of PEG (molecular weight: 2000) was added with a mass fraction of 0.1. 0.1 wt% to obtain a stable alumina sol (Al) by continuing stirring, as shown in FIG. 1. Placing the cleaned 310S stainless steel in the aluminum sol, soaking the stainless steel in the aluminum sol at the temperature of 85 ℃ for 4 h, washing the stainless steel with ethanol and deionized water, then performing heat treatment in an air atmosphere, preserving heat at the temperature of 550 ℃ for 4 h, continuously heating the stainless steel to the temperature of 1000 ℃ for 2 h, and cooling the stainless steel with a furnace at the temperature rate of 5 ℃ per minute to obtain the 310S stainless steel with the surface being uniformly and densely coated with the aluminum oxide coating, as shown in fig. 5.
Example 2: in this example, the concentration of SB powder was 5 mol/L, the concentration of ethyl orthosilicate was 0.25 mol/L, the concentration of nitric acid was 1 mol/L, stirring was continued at 85deg.C for 4. 4 h to form a semitransparent alumina sol, a certain amount of PEG (molecular weight 2000) was added, the mass fraction of PEG was 0.5. 0.5 wt%, and stirring was continued to obtain a stable silica-doped alumina sol (Si-Al), as shown in FIG. 2. Placing the cleaned 310S stainless steel in the aluminum sol, soaking the stainless steel in the aluminum sol at 90 ℃ for 4 h, washing the stainless steel with ethanol and deionized water, then performing heat treatment in an air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating the stainless steel to 1100 ℃ for 2 h, and cooling the stainless steel with a furnace at a heating rate of 5 ℃ per minute to obtain the 310S stainless steel modified by the Si-doped aluminum oxide coating, as shown in fig. 6.
Example 3: in the embodiment, the concentration of SB powder is 5 mol/L, the concentration of ZrC nano-particles is 0.25 mol/L, the concentration of nitric acid is 1 mol/L, stirring is continued at 85 ℃ for 4 h to form semitransparent alumina sol, a certain amount of PEG (molecular weight is 2000) is added, the mass fraction of the PEG is 0.5 wt percent, and stirring is continued to obtain stable ZrC composite alumina sol (ZrC-Al) as shown in figure 3. Placing the cleaned 310S stainless steel in the aluminum sol, soaking the stainless steel in the aluminum sol at 90 ℃ for 4 h, washing the stainless steel with ethanol and deionized water, then performing heat treatment in an air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating the stainless steel to 1100 ℃ for 2 h, and cooling the stainless steel with a furnace at a heating rate of 5 ℃ per minute to obtain the 310S stainless steel modified by the ZrC composite aluminum oxide coating, as shown in FIG. 7.
Example 4: in this example, the concentration of SB powder is 5 mol/L, and nano ZrB is added 2 Stirring at 85deg.C with nitric acid concentration of 0.25 mol/L and nitric acid concentration of 1 mol/L continuously for 4 h to form semitransparent aluminum sol, adding a certain amount of PEG (molecular weight of 2000) with PEG mass fraction of 0.5 wt%, and stirring continuously to obtain stable ZrB 2 Composite aluminium sol (ZrB) 2 -Al), as shown in fig. 4. Placing the cleaned 310S stainless steel into the aluminum sol, soaking at 90 ℃ for 4 h, washing with ethanol and deionized water, performing heat treatment under air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating to 1100 ℃ for 2 h, heating at a rate of 5 ℃ per minute, and cooling with a furnace to obtain ZrB 2 Composite alumina coating decorated 310S stainless steel as shown in fig. 8.
The alumina-based coating modified 310S stainless steel obtained in examples 1-4 is used for a high-temperature chloride molten salt corrosion test, and the chloride molten salt comprises NaCl/MgCl 2 KCl (24.5:55.0:20.5, wt.%) at 800 deg.C for 10 h, the weight loss of the corroded sample is as shown in FIG. 9, and the weight loss of the coated stainless steel is less, indicating its excellent high temperature chloride molten salt corrosion resistance.
Claims (3)
1. The preparation method of the alumina-based anticorrosive coating on the surface of the 310S stainless steel is characterized by comprising the following steps:
step (1) preparing pseudo-boehmite aqueous solution with the concentration of 0.1-10 mol/L; after ultrasonic dispersion, dropwise adding a nitric acid solution, wherein the nitric acid concentration is 0.01-0.5 mol/L, continuously stirring for 2-4 hours at 85 ℃ to form semitransparent aluminum sol, adding a preset amount of PEG, and continuously stirring to obtain stable aluminum sol, wherein the molecular weight of the PEG is 2000 and the mass fraction of the PEG is 0.1-1 wt%;
step (2) cleaning the cleaned 310S stainless steel with ethanol and deionized water, immersing the cleaned 310S stainless steel in the aluminum sol obtained in the step, carrying out chemical bath at 60-90 ℃ for 1-4 hours, and washing and drying the aluminum sol with ethanol to obtain the 310S stainless steel with the surface modified aluminum sol;
performing heat treatment on the obtained stainless steel in an air atmosphere, preserving heat at 550 ℃ for 4 h, continuously heating to 800-1100 ℃ for 2 h, and cooling with a furnace at a heating rate of 5 ℃ per minute to obtain 310S stainless steel with a uniformly dense aluminum oxide coating modified surface;
step (4) adding a preset amount of tetraethoxysilane, or nano ZrC or nano ZrB into the aluminum sol obtained in the step (1) respectively 2 The particles are 1 wt to 5 wt percent of doped/compounded amount, and the silicon doped aluminum sol, or ZrC-aluminum sol, or ZrB can be obtained after stirring for a preset time 2 -an aluminium sol; repeating the step (3) to obtain uniform and compact silicon-alumina, zrC-alumina and ZrB 2 Aluminum oxide coating modified 310S stainless steel.
2. The method for preparing the aluminum oxide-based anticorrosive coating on the surface of 310S stainless steel according to claim 1, wherein the nanometer ZrC is 30 nm particles, and the nanometer ZrB is 2 20 nm granules.
3. The method for preparing the aluminum oxide-based corrosion-resistant coating on the surface of the 310S stainless steel according to claim 1, wherein when the 310S stainless steel modified by the aluminum oxide-based coating is subjected to a high-temperature chloride molten salt corrosion test at 800 ℃, the coating is modified to have excellent chloride high-temperature molten salt corrosion resistance compared with unmodified stainless steel.
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