CN115522184B - YSZ coating, ferronickel-based superalloy and preparation method thereof - Google Patents
YSZ coating, ferronickel-based superalloy and preparation method thereof Download PDFInfo
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- CN115522184B CN115522184B CN202211227161.5A CN202211227161A CN115522184B CN 115522184 B CN115522184 B CN 115522184B CN 202211227161 A CN202211227161 A CN 202211227161A CN 115522184 B CN115522184 B CN 115522184B
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- 238000000576 coating method Methods 0.000 title claims abstract description 116
- 239000011248 coating agent Substances 0.000 title claims abstract description 115
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 30
- 229910000863 Ferronickel Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 150000003754 zirconium Chemical class 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 150000003746 yttrium Chemical class 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 229910052727 yttrium Inorganic materials 0.000 claims description 36
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 30
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 18
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 16
- 229910052726 zirconium Inorganic materials 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 13
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical group CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- CVBUKMMMRLOKQR-UHFFFAOYSA-N 1-phenylbutane-1,3-dione Chemical compound CC(=O)CC(=O)C1=CC=CC=C1 CVBUKMMMRLOKQR-UHFFFAOYSA-N 0.000 claims description 8
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 claims description 8
- 235000019260 propionic acid Nutrition 0.000 claims description 8
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- YOBOXHGSEJBUPB-MTOQALJVSA-N (z)-4-hydroxypent-3-en-2-one;zirconium Chemical compound [Zr].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O YOBOXHGSEJBUPB-MTOQALJVSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 238000003723 Smelting Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000009993 protective function Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 23
- 229910045601 alloy Inorganic materials 0.000 description 19
- 239000000956 alloy Substances 0.000 description 19
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 10
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
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- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910017061 Fe Co Inorganic materials 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
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- 230000015572 biosynthetic process Effects 0.000 description 3
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- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
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- 239000002245 particle Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
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- 229920006395 saturated elastomer Polymers 0.000 description 2
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- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
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- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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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
- 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
Abstract
A YSZ coating, a ferronickel-based superalloy and a preparation method thereof belong to the technical field of superalloys, and overcome the defects of uniform and poor compactness of the YSZ coating and poor protective function of the coating in the prior art. The preparation method of the YSZ coating provided by the invention comprises the following steps: step 1, preparing YSZ sol by adopting precursor salt, additive and solvent; the precursor salts include yttrium salts and zirconium salts; step 2, coating YSZ sol into a layer; step 3, drying to remove the solvent to form a gel coating; and 4, performing heat treatment to form the YSZ coating. The invention can prepare compact and uniform coating.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloys, and particularly relates to a YSZ coating, a ferronickel-based high-temperature alloy and a preparation method thereof.
Background
In a coal-fired power generation unit, in order to improve the heat energy power generation efficiency and reduce pollutant emission, the steam temperature and pressure parameters of the unit are required to be continuously improved. The nickel-iron-based superalloy has a stable structure in a long-term aging process, and the nickel-iron-based superalloy generally adopts gamma' phase precipitation strengthening and grain boundary precipitation carbide phase with the volume fraction of not higher than 25% to strengthen the structure, has good welding performance, high-temperature strength and creep resistance, has high cost performance, and is considered as a better candidate material in a coal-fired generator set. Although nickel-iron based alloys have excellent mechanical properties, their inadequate oxidation resistance at higher service temperatures limits their large-scale use in higher parameter steam units.
When the nickel-iron-based alloy is in service in a high-temperature environment, surface oxidation is unavoidable, and the high-temperature oxidation not only can damage the surface quality of the alloy, but also can easily cause the mechanical property of the alloy to be damaged. The high-temperature oxidation of the surface of the substrate can be effectively reduced by adopting a coating protection technical means. At present, although the surface protection of nickel-based or nickel-iron-based alloy has advanced to some extent, most researches adopt a method of mixing powder into paint by means of a binder and sintering the paint on the alloy surface, in the process, the content of solid powder is higher, generally more than 50%, the mass fraction of solid powder is high, the content of solvent is low, the binder, the solvent and the solid paint cannot be chemically compatible, only ordinary physical mixing is difficult to form a uniform and stable paint system, so that the finally obtained coating is uniform and poor in compactness, and the protection function of the coating is further affected.
Disclosure of Invention
Therefore, the invention aims to overcome the defects of uniform and poor compactness of a YSZ coating and poor protective function of the coating in the prior art, thereby providing a YSZ coating, a ferronickel-based superalloy and a preparation method thereof.
For this purpose, the invention provides the following technical scheme:
in a first aspect, the invention provides a method for preparing a YSZ coating, comprising the steps of:
step 1, preparing YSZ sol by adopting precursor salt, additive and solvent; the precursor salts include yttrium salts and zirconium salts;
step 2, coating YSZ sol into a layer;
step 3, drying to remove the solvent to form a gel coating;
and 4, performing heat treatment to form the YSZ coating.
Further, the step 1 satisfies at least one of the conditions (1) to (4):
(1) The zirconium salt is organic zirconium salt;
specifically, the zirconium salt comprises at least one of zirconium n-butoxide and zirconium acetylacetonate;
(2) The yttrium salt is yttrium acetate;
(3) The additive comprises at least one of propionic acid, benzoyl acetone, acrylic acid and acetylacetone;
(4) The solvent is methanol.
Further, the step 1 includes: yttrium solution and zirconium solution were prepared separately, yttrium: zirconium atom mole ratio (1.5-2.0), mixing yttrium solution and zirconium solution (8.0-8.5), stirring for 4-6 h at room temperature to form YSZ sol.
Further, in the step 3, the drying conditions are as follows: and drying at 120-170 deg.c in air condition.
Further, in the step 4, the heat treatment conditions are as follows: preserving heat for 1.5-2 h at 750-900 ℃ in a reducing atmosphere;
specifically, the temperature rising rate is 150-200 ℃/s;
a reducing atmosphere of N 2 And H 2 The volume ratio is (8-12): 1.
Further, the step 2 and the step 3 are alternately repeated to control the thickness of the gel coating.
In a second aspect, the present invention provides a YSZ coating.
In a third aspect, the present invention provides a ferronickel-based superalloy comprising a substrate and a YSZ coating disposed on the substrate;
in the step 2, the YSZ sol is coated on the substrate.
In a fourth aspect, the invention provides a preparation method of a ferronickel-based superalloy, wherein before YSZ sol is coated on a substrate, the substrate is sequentially polished, polished and ultrasonically cleaned;
specifically, the polishing comprises: sequentially polishing the surface of the matrix by adopting 200# abrasive paper, 600# abrasive paper, 1000# abrasive paper, 1200# abrasive paper and 2000# abrasive paper;
the polishing is electrochemical polishing;
the ultrasonic cleaning is performed by adopting acetone and alcohol.
Further, the preparation method of the matrix comprises the following steps: smelting, homogenizing treatment, rolling and solution treatment.
Specifically, the preparation method of the matrix comprises the following steps: smelting ferronickel base alloy mother liquor by a vacuum induction arc furnace, wherein the homogenization treatment temperature is 1150-1200 ℃, the rolling temperature is not lower than 200 ℃ above the gamma' precipitation temperature, the deformation of each pass is not lower than 20%, and the total deformation is not lower than 50%. The solution treatment temperature of the rolled alloy is 1000-1100 ℃, and the solution time is 30-90 min.
The matrix composition is Cr: 15-20%, C:0.02 to 0.1 percent, B:0 to 0.01 percent, ti:0.5 to 2.0 percent, al:1.0 to 3.5 percent, si: less than or equal to 0.8 percent, co:0 to 3.0 percent, N:0 to 0.01 percent, fe: 15-40% and the balance of Ni.
The technical scheme of the invention has the following advantages:
1. the preparation method of the YSZ coating provided by the invention comprises the following steps: step 1, preparing YSZ sol by adopting precursor salt, additive and solvent; the precursor salts include yttrium salts and zirconium salts; step 2, coating YSZ sol into a layer; step 3, drying to remove the solvent to form a gel coating; and 4, performing heat treatment to form the YSZ coating.
The invention adopts the metal precursor salt of the initial raw material, and the metal precursor salt is dissolved in the solvent by means of the additive with dissolution assisting and chelating effects to generate hydrolysis and polycondensation reaction, so as to form a stable and transparent sol system with the Tyndall effect, the dispersion and uniformity of the precursor salt in the sol are greatly improved compared with that of the common coating, and after the sol is dried, the sol loses fluidity, so that the gel with a three-dimensional network structure is formed. And a compact and uniform coating can be finally formed through high-temperature treatment.
2. In the preparation method of the YSZ coating, the zirconium salt is organic zirconium salt, the stability is good, the hydrolysis is not easy, the organic alcohol (such as methanol) is adopted as a solvent, and the sol has long-term stability due to the use of the organic zirconium salt and the action of an additive.
The invention adopts yttrium acetate as raw material, acetate and other components can form intermolecular crosslinking structure, and after methanol solvent is deprotonated, the group OCH 3 - The orbital occupied by the lone pair of electrons of the medium oxygen atom can overlap with the empty orbital of the Y center ion to form a complex with alkoxy property [ Y (OAC) 3 (OCH 3 ) 2 ] 2+ . Between complexesThe macromolecular organic crosslinking structure can be formed through intermolecular interaction in a hydrogen bond form, so that the stability of the sol is improved.
3. In the preparation method of the YSZ coating, yttrium is used as the raw material: zirconium atom mole ratio (1.5-2.0), mixing yttrium solution and zirconium solution (8.0-8.5) to prepare sol. Pure ZrO 2 Structural instability at room temperature, at ZrO 2 Adding Y 3+ Ions, zrO which can generate oxygen vacancies to change into an advantageous structure to metastable phase 2 Stable to room temperature. In addition to that, Y 2 O 3 Can be combined with ZrO 2 Solid solution reaction occurs to form a solid solution, along with Y 2 O 3 The increase of the addition has more obvious effects on activating crystal lattices and promoting sintering, so that the crystal grain development is more complete, the reaction temperature is reduced, and the lower reaction temperature can avoid adverse effects on the structural performance of the ferronickel base alloy matrix material. And Y is 2 O 3 Can reduce the mean free path of phonons from both the introduction of strain fields and oxygen vacancies, yttrium in the present invention: the thermal diffusion coefficient of the coating structural phase obtained when the molar ratio of zirconium atoms is (1.5-2.0) to (8.0-8.5) is smaller, and is closer to that of the alloy matrix and more matched with the matrix.
4. In the preparation method of the YSZ coating, in the step 4, the heat treatment conditions are as follows: preserving heat for 1.5-2 h at 750-900 ℃ in a reducing atmosphere; specifically, the temperature rising rate is 150-200 ℃/s. The invention adopts rapid heating during heat treatment, so that the sample decomposition degree is small in the low-temperature stage, the thermal decomposition of precursor salt and the breaking of chemical bonds are concentrated in the high-temperature stage, more energy is released by the breaking of the bonds, the driving force of nucleation and growth of crystal nucleus is improved, and YSZ phase can be obtained at lower temperature.
5. The ferronickel-based superalloy provided by the invention comprises a substrate and a YSZ coating arranged on the substrate, wherein the YSZ coating is prepared by adopting the method; in the step 2, the YSZ sol is coated on the substrate.
In the invention, YSZ sol is directly coated on a substrate, and the sol has excellent interface wettability and can be coated on a smooth surface with any geometric shape in a dipping way. The gel formation and the chemical reaction process of the coating during the heat treatment directly occur on the substrate, heterogeneous nucleation is taken as the main nucleation process, the formation of crystal nuclei and the growth of the crystal nuclei occur at the interface of the alloy and the coating, chemical bonds are formed at the interface of the coating and the substrate, and the bonding force is good. The ferronickel-based superalloy provided by the invention can be used as an auxiliary bonding means without an intermediate bonding layer, the prepared coating is well bonded with a matrix interface, the coating is uniform and compact, diffusion channels of oxidation media can be reduced, and the antioxidation capability of the alloy surface is improved.
6. According to the preparation method of the ferronickel-based superalloy, a YSZ coating is prepared on a substrate by adopting a sol-gel method, and the prepared coating has high purity, uniform components, small granularity and narrow particle size distribution; the reaction temperature is lower; the gel formation and the chemical reaction process of the coating are directly carried out on the alloy matrix, the coating preparation flow is simpler, the equipment requirement is low, the preparation can be completed only by simple dip-and-pull equipment and a tubular heat treatment furnace, and the cost is low; compared with the existing coating preparation technology such as chemical vapor deposition, pulse laser deposition, magnetron sputtering and the like, the sol preparation process is simple, the cost is low, and the operability is strong; the invention can adopt a mode of dipping the alloy into the sol, so that the invention has no requirement on the shape of the alloy, can finish the coating of the workpiece in a very short time, has high efficiency and is suitable for industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is an X-ray diffraction pattern of the YSZ coating of example 1.
Fig. 2 is an SEM morphology of YSZ coating in example 1.
Fig. 3 is EDS spectra of YSZ coating in example 1.
Fig. 4 is an SEM morphology of YSZ coating in example 2.
Fig. 5 is an EDS spectrum of YSZ coating in example 2.
FIG. 6 is an EDS spectrum of the YSZ coating of example 3;
FIG. 7 is an EDS spectrum of the YSZ coating of example 4;
FIG. 8 is an SEM topography of the YSZ coating of example 6;
FIG. 9 is an EDS spectrum of the YSZ coating of example 6;
FIG. 10 is an SEM topography of the YSZ coating of comparative example 1;
FIG. 11 is weight gain data for ferronickel-based superalloys prepared in examples and comparative examples in a saturated steam environment at 650℃ for 1000 hours.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, by anyone who in the light of the present invention or combines the present invention with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
The preparation methods of the matrixes adopted in the embodiment and the comparative example of the invention comprise the following steps: the ferronickel base alloy mother solution is smelted by a vacuum induction arc furnace, the homogenization treatment temperature is 1200 ℃, the rolling temperature is 1150 ℃, the deformation per pass is 20%, and the total deformation is 60%. The solution treatment temperature of the rolled alloy is 1100 ℃, and the solution time is 30min. Sequentially polishing the surface of the substrate by using 200# sand paper, 600# sand paper, 1000# sand paper, 1200# sand paper and 2000# sand paper, performing electrochemical polishing, and sequentially ultrasonically cleaning by using acetone and alcohol.
The matrix composition is Cr: 15-20%, C:0.02 to 0.1 percent, B:0 to 0.01 percent, ti:0.5 to 2.0 percent, al:1.0 to 3.5 percent, si: less than or equal to 0.8 percent, co:0 to 3.0 percent, N:0 to 0.01 percent, fe: 15-40% and the balance of Ni.
Example 1
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.20g of yttrium acetate, 1.0g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 9.78g of zirconium n-butoxide, 4.13g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 1.5:8.5 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 at 150 ℃ in air to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within 800 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. And (3) extremely fast heating the sample, wherein the heating speed reaches 150 ℃/s, namely the sample at room temperature is quickly moved to a 800 ℃ temperature zone of the tube furnace by a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 2h. After the incubation time is over, the sample is removed from the 800 ℃ temperature zone by means of sliding rails and cooled to room temperature.
Fig. 1 is an X-ray diffraction pattern of a YSZ coating, and it can be seen from fig. 1 that, in addition to the diffraction peak of the matrix, a characteristic diffraction peak of YSZ phase can be observed, and no other impurity phase is generated, indicating that YSZ phase can be prepared on the ferronickel-based superalloy.
Fig. 2 is an SEM morphology of the YSZ coating, and the YSZ coating of fig. 2 has a dense surface, without cracks and holes.
The EDS spectra of the YSZ coating of fig. 3, in which, in addition to the matrix elements, absorption peaks of Y and Zr elements are observed, further indicates that the YSZ coating can be prepared on the nickel-iron-based superalloy, wherein the atomic percentages of the respective elements are shown in table 1, and the atomic percentages of the Y and Zr elements are respectively 0.27% and 1.56%, which is close to the stoichiometric ratio of 1.5 of metal atoms in the coating: 8.5, the above data illustrate that a pure phase YSZ coating can be prepared on a nickel-iron based superalloy using the method of this example.
TABLE 1 elemental content of YSZ coating
Element(s) | C | O | Al | Si | Ti | Cr | Fe | Co | Ni | Y | Zr |
Wt% | 25.83 | 10.66 | 1.95 | 0.18 | 1.36 | 14.68 | 15.18 | 0.23 | 21.96 | 2.13 | 5.84 |
At% | 56.55 | 16.26 | 1.78 | 0.15 | 0.69 | 6.89 | 6.63 | 0.09 | 9.13 | 0.27 | 1.56 |
Example 2
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.20g of yttrium acetate, 1.0g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 9.78g of zirconium n-butoxide, 4.13g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 1.5:8.5 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 under the air condition at 120 ℃ to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within 850 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. And (3) extremely fast heating the sample, wherein the heating speed reaches 200 ℃/s, namely the sample at room temperature is quickly moved to a 850 ℃ temperature zone of the tube furnace by a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 2h. After the incubation time is over, the sample is removed from the 850 ℃ temperature zone by means of movement of the slide rail and cooled to room temperature.
Fig. 4 is an SEM morphology of the YSZ coating, and from fig. 4 it can be seen that the YSZ coating surface is dense, free of cracks and holes.
Fig. 5 is an EDS spectrum of the YSZ coating, and the elemental content of the YSZ coating can be obtained by fig. 5, as shown in table 2. Wherein the atomic percentages of the Y and Zr elements are respectively 0.26 percent and 1.52 percent, which is close to the ideal proportion of metal atoms in the coating of 1.5:8.5, illustrating that a pure phase YSZ coating can be prepared on a nickel-iron based superalloy using the protocol shown in this example.
TABLE 2 elemental content of YSZ coating
Element(s) | C | O | Al | Si | Ti | Cr | Fe | Co | Ni | Y | Zr |
Wt% | 23.56 | 9.52 | 1.95 | 0.18 | 1.38 | 15.15 | 17.07 | 0.09 | 23.64 | 2.05 | 5.41 |
At% | 54.49 | 15.27 | 1.86 | 0.16 | 0.74 | 7.48 | 7.84 | 0.04 | 10.34 | 0.26 | 1.52 |
Example 3
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.20g of yttrium acetate, 1.0g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 9.78g of zirconium n-butoxide, 4.13g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 1.5:8.5 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 at 170 ℃ in air to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within the temperature range of 900 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. And (3) extremely fast heating the sample, wherein the heating speed reaches 150 ℃/s, namely the sample at room temperature is quickly moved to a 900 ℃ temperature zone of the tube furnace in a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 1.5h. After the incubation time is over, the sample is removed from the 900 ℃ temperature zone by means of sliding rails and cooled to room temperature.
Fig. 6 is an EDS spectrum of the YSZ coating, and the elemental content of the YSZ coating can be obtained by fig. 6, as shown in table 3. From Table 3, it is clear that the atomic percentages of the Y and Zr elements are respectively 0.21% and 1.19%, which are close to the stoichiometric ratio of 1.5 of the metal atoms in the coating: 8.5, illustrating that a pure phase YSZ coating can be prepared on a nickel-iron based superalloy using the protocol shown in this example.
TABLE 3 elemental content of YSZ coating
Element(s) | C | O | Al | Si | Ti | Cr | Fe | Co | Ni | Y | Zr |
Wt% | 12.96 | 9.37 | 2.36 | 0.03 | 1.72 | 17.47 | 20.46 | 0.09 | 28.97 | 1.93 | 4.64 |
At% | 36.12 | 19.19 | 2.87 | 0.04 | 1.17 | 11 | 12 | 0.05 | 16.16 | 0.21 | 1.19 |
Example 4
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.60g of yttrium acetate, 1.33g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 9.20g of zirconium n-butoxide, 3.89g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atomic molar ratio 2:8 yttrium solution and zirconium solution were mixed and stirred at room temperature for 6h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 at 150 ℃ in air to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within a temperature range of 750 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. Sample feedingAnd (3) carrying out extremely rapid heating, wherein the heating speed reaches 150 ℃/s, namely, a sample at room temperature is rapidly moved to a 750 ℃ temperature zone of the tube furnace by a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 2h. After the incubation time is over, the sample is removed from the 750 ℃ temperature zone by way of movement of the slide rail and cooled to room temperature.
Fig. 7 is an EDS spectrum of the YSZ coating, and the elemental content of the YSZ coating can be obtained by fig. 7, as shown in table 4. From Table 4, it can be seen that the atomic percentages of the Y and Zr elements are 0.41% and 1.6%, respectively, which are close to the stoichiometric ratio 2 of the metal atoms in the coating: 8, illustrating that pure phase YSZ coatings can be prepared on ferronickel-based superalloys using the protocol shown in this example.
TABLE 4 elemental content of YSZ coating
Element(s) | C | O | Al | Si | Ti | Cr | Fe | Co | Ni | Y | Zr |
Wt% | 21.86 | 9.55 | 1.91 | 0.16 | 1.55 | 13.62 | 16.37 | 0.11 | 23.23 | 5.76 | 5.88 |
At% | 56.82 | 14.81 | 1.76 | 0.14 | 0.8 | 6.5 | 7.28 | 0.06 | 9.82 | 0.41 | 1.6 |
Example 5
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.20g of yttrium acetate, 0.97g of acrylic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60 minutes to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 12.43g of zirconium acetylacetonate, 2.55g of acetylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 1.5:8.5 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 at 150 ℃ in air to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within 850 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. And (3) extremely fast heating the sample, wherein the heating speed reaches 150 ℃/s, namely the sample at room temperature is quickly moved to a 850 ℃ temperature zone of the tube furnace by a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 2h. After the incubation time is over, the sample is removed from the 850 ℃ temperature zone by means of movement of the slide rail and cooled to room temperature.
Example 6
The embodiment provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
2.40g of yttrium acetate, 2.0g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 8.06g of zirconium n-butoxide, 3.40g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 3:7 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, coating the YSZ sol on the surface of the substrate by using an immersion pulling method.
And step 3, drying the product in the step 2 at 150 ℃ in air to form a gel coating.
Step 4, carrying out heat treatment on the sample prepared in the step 3 in a slide rail type tube furnace:
heating the heating end of the tube furnace to a stable state within 800 ℃ and introducing N 2 And H 2 And mixing the materials according to the volume ratio of 10:1 to form a reducing atmosphere. And (3) extremely fast heating the sample, wherein the heating speed reaches 150 ℃/s, namely the sample at room temperature is quickly moved to a 800 ℃ temperature zone of the tube furnace by a sliding rail moving mode under the protection of atmosphere, and the temperature is kept for 2h. After the incubation time is over, the sample is removed from the 800 ℃ temperature zone by means of sliding rails and cooled to room temperature.
Fig. 8 is an SEM morphology of the YSZ coating of this example, fig. 9 is EDS spectra of the YSZ coating, and the elemental content of the YSZ coating can be obtained from fig. 9, as shown in table 5. As can be seen from Table 5, the atomic percentages of the elements Y and Zr are respectively 0.58% and 1.37%, which are close to the ratio 3: and 7, the preparation proportion of the coating is consistent with that of the sol, but the SEM morphology shows that the surface is provided with more porous particles, the morphology nonuniformity is increased, and the uniformity and the compactness of the coating are reduced when the atomic ratio of the Y element to the Zr element is overlarge.
TABLE 5 elemental content of YSZ coating
Element(s) | C | O | Al | Si | Ti | Cr | Fe | Co | Ni | Y | Zr |
Wt% | 12.75 | 9.24 | 2.37 | 0.15 | 1.65 | 14.43 | 20.89 | 0.02 | 26.14 | 6.24 | 6.12 |
At% | 35.13 | 18.97 | 2.89 | 0.17 | 1.13 | 11.04 | 12.29 | 0.01 | 16.42 | 0.58 | 1.37 |
Comparative example 1
The comparative example provides a preparation method of a ferronickel-based superalloy, which comprises the following steps:
step 1, preparing YSZ sol;
1.20g of yttrium acetate, 1.0g of propionic acid and 15ml of methanol were mixed and magnetically stirred at 40℃for 60min to prepare a homogeneous yttrium solution. A homogeneous zirconium solution was prepared by mixing 9.78g of zirconium n-butoxide, 4.13g of benzoylacetone, and 15ml of methanol. According to yttrium: zirconium atom mole ratio of 1.5:8.5 yttrium solution and zirconium solution were mixed and stirred at room temperature for 4h to form YSZ sol.
And 2, atomizing the sol by using a pressure atomization method, preserving the temperature at 900 ℃ for 1h to prepare powder, and forming a coating on the substrate by plasma spraying. The appearance of the coating is shown in fig. 10, and it can be seen from the graph that the surface of the coating obtained by the conventional method has more cracks and does not meet the protection requirement of the coating.
Test examples
Weight gain data for the examples and comparative examples at 650 ℃ in a 1000h saturated steam environment are shown in fig. 11, and test results are shown in table 6.
Table 6 nickel-iron based superalloy properties
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (9)
1. A method for preparing a YSZ coating, comprising the steps of:
step 1, preparing YSZ sol by adopting precursor salt, additive and solvent; the precursor salts include yttrium salts and zirconium salts;
step 2, coating YSZ sol into a layer;
step 3, drying to remove the solvent to form a gel coating;
step 4, performing heat treatment to form a YSZ coating;
in the step 4, the heat treatment conditions are as follows: preserving heat for 1.5-2 h at 750-900 ℃ in a reducing atmosphere;
the temperature rising rate is 150-200 ℃/s; a reducing atmosphere of N 2 And H 2 The volume ratio is (8-12): 1.
2. The method of preparing a YSZ coating according to claim 1, characterized in that step 1 satisfies at least one of the conditions (1) - (4):
(1) The zirconium salt is organic zirconium salt;
specifically, the zirconium salt comprises at least one of zirconium n-butoxide and zirconium acetylacetonate;
(2) The yttrium salt is yttrium acetate;
(3) The additive comprises at least one of propionic acid, benzoyl acetone, acrylic acid and acetylacetone;
(4) The solvent is methanol.
3. The method of preparing a YSZ coating according to claim 1 or 2, characterized in that step 1 comprises: yttrium solution and zirconium solution were prepared separately, yttrium: zirconium atom mole ratio (1.5-2.0), mixing yttrium solution and zirconium solution (8.0-8.5), stirring for 4-6 h at room temperature to form YSZ sol.
4. The method for preparing YSZ coating according to claim 1 or 2, wherein in the step 3, the drying conditions are: and drying at 120-170 deg.c in air condition.
5. The method of preparing a YSZ coating according to claim 1 or 2, characterized in that step 2 and step 3 are alternately repeated to control the thickness of the gel coating.
6. YSZ coating obtainable by the method of any one of claims 1-5.
7. A ferronickel-based superalloy comprising a substrate and a YSZ coating disposed on the substrate, the YSZ coating made by the method of any of claims 1-5;
in the step 2, the YSZ sol is coated on the substrate.
8. A method for preparing the ferronickel-based superalloy as in claim 7, wherein the substrate is sequentially polished, polished and ultrasonically cleaned before the substrate is coated with YSZ sol;
the polishing comprises the following steps: sequentially polishing the surface of the matrix by adopting 200# abrasive paper, 600# abrasive paper, 1000# abrasive paper, 1200# abrasive paper and 2000# abrasive paper;
the polishing is electrochemical polishing;
the ultrasonic cleaning is performed by adopting acetone and alcohol.
9. The method for producing a ferronickel-based superalloy according to claim 8, wherein the method for producing a substrate comprises: smelting, homogenizing treatment, rolling and solution treatment.
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