CN116288123A - ODS steel with aluminum alloying coating and preparation method thereof - Google Patents
ODS steel with aluminum alloying coating and preparation method thereof Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 103
- 239000010959 steel Substances 0.000 title claims abstract description 103
- 239000011248 coating agent Substances 0.000 title claims abstract description 64
- 238000000576 coating method Methods 0.000 title claims abstract description 64
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 47
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005275 alloying Methods 0.000 title claims abstract description 16
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- 239000000956 alloy Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 32
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005507 spraying Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 19
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- 238000009792 diffusion process Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 10
- 239000010410 layer Substances 0.000 claims description 39
- 229910000838 Al alloy Inorganic materials 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000005488 sandblasting Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000004519 grease Substances 0.000 claims description 7
- 230000003746 surface roughness Effects 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000011247 coating layer Substances 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007790 scraping Methods 0.000 claims description 3
- 238000005422 blasting Methods 0.000 claims 2
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 17
- 239000010935 stainless steel Substances 0.000 abstract description 17
- 239000011159 matrix material Substances 0.000 abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- 238000001816 cooling Methods 0.000 abstract description 6
- 238000010891 electric arc Methods 0.000 abstract description 5
- 238000005098 hot rolling Methods 0.000 abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 239000011651 chromium Substances 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 230000007797 corrosion Effects 0.000 description 14
- 238000005260 corrosion Methods 0.000 description 14
- 239000000306 component Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000004506 ultrasonic cleaning Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000007581 slurry coating method Methods 0.000 description 6
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- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 229910000616 Ferromanganese Inorganic materials 0.000 description 3
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
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- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
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- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910000909 Lead-bismuth eutectic Inorganic materials 0.000 description 1
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/131—Wire arc spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
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Abstract
The invention discloses ODS steel with an aluminum alloying coating and a preparation method thereof, wherein high-purity iron, high-purity chromium, high-purity titanium, nanometer yttrium oxide powder and high-purity aluminum wires are used as raw materials, pure and defect-free 436 stainless steel is obtained through vacuum arc melting, water-cooling copper mold suction casting and hot rolling, nanometer yttrium oxide is introduced by a surface stirring friction treatment process, and the ODS steel with the aluminum alloying coating is prepared through arc spraying and vacuum diffusion annealing. The aluminum-alloyed ODS steel layer is prepared by combining surface stirring friction treatment and an electric arc spraying process, so that fine matrix grains and nano-scale dispersion particles uniformly distributed on the matrix are obtained, and the aluminum-alloyed ODS steel layer can be used for preparing an ODS aluminum-containing alloy coating.
Description
Technical Field
The invention belongs to the technical field of corrosion-resistant metal structural materials in extreme service environments, and particularly relates to ODS steel with an aluminum alloy coating and a preparation method thereof.
Background
As global climate warming increases, there is a need for people to seek energy modes for reducing carbon emissions to suppress the greenhouse effect, and the reduction of the use of renewable energy sources instead of fossil energy sources has become a broad consensus for people to reduce carbon emissions. The nuclear energy is highly focused by people because of the advantages of no carbon emission, stability, high efficiency and the like in the use process. The fourth generation nuclear reactor reference reactor type represented by the lead cold fast reactor is the first choice of the next generation green energy source of human beings. The lead-cooled fast reactor adopts lead/lead bismuth alloy as a coolant, has the characteristics of high safety, high economy, high sustainability and the like, and has great application potential; however, the problem of corrosion of the structural material by the liquid alloy is in need of solution.
Stainless steel has excellent mechanical properties and corrosion resistance, and is low in cost, so that the stainless steel is widely applied to aspects of production and life. The fuel cladding of the lead-cooled fast reactor has a bad service environment, is soaked in liquid lead-bismuth eutectic for a long time and is subjected to high-dose neutron irradiation, so the cladding material must have excellent corrosion resistance and irradiation resistance in service. Stainless steel has excellent corrosion resistance and lower production cost, and has the potential of being applied to core components of the lead-cooled fast reactor in a large scale. Limited by dissolution corrosion and severe irradiation damage, commercial austenitic stainless steel cannot be applied to the primary circuit of a lead cooled fast reactor; the aluminum alloying is carried out on the surface of the original ferrite stainless steel, so that the corrosion resistance of the ferrite stainless steel can be obviously improved, and the irradiation resistance and the high-temperature mechanical property of the material are obviously improved by introducing nano-scale oxide particles with high dispersity into an alloy matrix, so that the ferrite stainless steel becomes one of the most competitive cladding materials. At present, ODS steel has a plurality of preparation methods, but most of the ODS steel has the problems of high production cost, difficult mass production, easy introduction of impurity elements and the like, and the mass application of the ODS FeCrAl alloy in the nuclear industry is hindered.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the ODS steel with the aluminum alloy coating and the preparation method thereof, and the oxide dispersion strengthening steel with the aluminum alloy coating, which has fine grain structure and fine oxide dispersion particles distributed on a matrix, is obtained through surface treatment, improves the irradiation resistance and corrosion resistance of the alloy while improving the mechanical property of the alloy, is used for solving the technical problems of high production cost, difficult mass production and easy introduction of impurity elements of the ODS steel, and provides a new idea for the development of the Oxide Dispersion Strengthening (ODS) steel in nuclear reactors.
The invention adopts the following technical scheme:
a preparation method of ODS steel with an aluminum alloying coating comprises the following steps:
mixing nanometer yttrium oxide powder, deionized water and polyvinyl alcohol to prepare Y 2 O 3 The sizing agent is coated on the surface of the steel plate in a scraping way, and is dried in vacuum for standby;
carrying out surface stirring friction treatment on the coating surface of the steel plate after vacuum drying to obtain an ODS steel layer;
and sequentially carrying out sand blasting and cleaning on the ODS steel layer, carrying out surface spraying by taking 4N high-purity aluminum as a raw material, and carrying out vacuum diffusion annealing to obtain the aluminum alloy ODS steel layer with oxide dispersion particles.
Specifically, the steel plate is prepared by vacuum arc melting and water-cooling copper die vacuum suction casting, and the surface of the steel plate is polished and cleaned before blade coating.
Specifically, Y 2 O 3 In the slurry, the mass fraction of the nano yttrium oxide powder is 9-11%, the mass fraction of the polyvinyl alcohol is 19-21%, and the mass fraction of the deionized water is 69-71%.
Specifically, Y 2 O 3 The preparation process of the slurry is as follows:
adding polyvinyl alcohol into deionized water, carrying out electromagnetic stirring for 14-1 min at 900-1100 rmp, adding nano yttrium oxide powder, and carrying out electromagnetic stirring for 25-30 min at 1400-1600 rmp to obtain Y 2 O 3 And (3) sizing.
Specifically, the thickness of the knife coating is 50-100 mu m, the temperature of vacuum drying is 75-80 ℃ and the time is 50-60 min.
Specifically, grease is coated on the coating surface of the steel plate after vacuum drying, a cutter is pressed down for 150-200 mu m, the rotating speed of the cutter is 300-600 rmp, the feeding rate is 50-100 mm/min, and the surface stirring friction treatment is carried out.
Furthermore, the cutter adopts a GCr15 alloy hemispherical cutter with the radius of 6-8 mm.
Specifically, the sand blasting pressure is 0.4-0.6 MPa, the surface roughness Ra of the ODS steel layer after sand blasting treatment is 1.8-2.4 mu m, the sprayed arc voltage is 30-45V, the arc current is 300-400A, the spraying distance is 100-350 mm, and the surface thickness is 0.5-1.0 mm.
Specifically, the temperature of the vacuum diffusion annealing is 450-600 ℃ and the time is 4-16 h.
The other technical scheme of the invention is that the ODS steel with the aluminum alloying coating comprises the following components in percentage by weight: 4% -6%, Y 2 O 3 :0.50 to 1.50 percent, cr:12.00% -14.00%, ti:0.50% -1.00%, mn: 0.70-1.00%, and the balance of Fe and unavoidable trace impurities.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method of ODS steel with an aluminum alloying coating ensures that oxide dispersion particles are uniformly distributed in an alloy layer through friction stir treatment, and simultaneously, matrix grains of the alloy layer are obviously refined; the ODS steel layer is subjected to aluminum alloying treatment by adopting the arc spraying and vacuum diffusion annealing process, so that the corrosion resistance of the ODS steel layer is obviously improved. The core point of the invention is that the homogenization distribution of the dispersed particles is regulated and controlled, the matrix grains of the ODS steel layer are thinned, and the aluminum of the ODS steel layer is alloyed, so that the ODS steel layer is prepared by aluminum alloying.
Further, the stainless steel plate base material is prepared by adopting vacuum arc melting, so that the introduction of impurity elements is effectively avoided, the burning loss of raw materials is avoided, the utilization rate of the raw materials and the purity of the steel plate are obviously improved, the raw materials are cleaned and dried, the introduction of the impurity elements can be avoided, the defects and the inclusions of a sample are avoided to the greatest extent, the burning loss of the raw materials in the melting process can be effectively reduced, and the utilization rate of the raw materials is improved.
Further, the surface friction stir processing is adopted to introduce the nano-scale Y 2 O 3 Particles, effectively avoid Y 2 O 3 Coarsening and agglomerating of (C) to facilitate Y 2 O 3 Uniform distribution of particles in the matrix and refinement of the matrix structure.
Further, prepare Y 2 O 3 Uniformly dispersed sizing agent and is coated, dried and solidified on the surface of the stainless steel plate to obtain Y 2 O 3 Uniformly distributed coating layer, help Y 2 O 3 Is introduced uniformly.
Further, the cutter is pressed down in the surface friction stir processing, and the alloy layer is subjected to severe plastic deformation and simultaneously is subjected to Y 2 O 3 Is ground and mixed to promote Y 2 O 3 The coating layer is coated with lubricating grease on the dry coating layer, so that friction is reduced, and the service life of the cutter is prolonged.
Further, the spherical high alloy steel cutter is adopted to stir and rub the surface of the steel plate, so that the matrix grains of the alloy layer are obviously refined while the oxide dispersed particles are uniformly distributed in the alloy layer.
Furthermore, the oxide film and oil stains on the surface of the alloy can be removed by carrying out sand blasting treatment on the surface of the alloy before electric arc spraying, so that the introduction of impurities and defects is reduced, and the electric arc spraying of high-purity aluminum on the sand blasted surface is beneficial to reducing the introduction of impurities and providing a diffusion source for aluminum alloying on the surface of the alloy.
Further, after arc spraying and vacuum diffusion annealing, the mass fraction content of the matrix aluminum of the ODS steel layer is 4% -6%, and the average grain diameter of the grains is 20 μm.
In summary, the alloy layer is prepared by adopting the process of combining the surface stirring friction treatment and the electric arc spraying, so that the alloy layer has fine crystal grains and fine and uniform oxide dispersion particle distribution, and the material is well used for preparing the ODS aluminum-containing alloy.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the present invention, all embodiments and preferred methods of implementation mentioned herein may be combined with each other to form new solutions, unless otherwise specified.
In the present invention, all technical features mentioned herein and preferred features may be combined with each other to form new technical solutions, unless otherwise specified.
In the present invention, the percentage (%) or parts refer to weight percentage or parts by weight relative to the composition unless otherwise specified.
In the present invention, the components or preferred components thereof may be combined with each other to form a new technical solution, unless otherwise specified.
In the present invention, unless otherwise indicated, the numerical ranges "a-b" represent shorthand representations of any combination of real numbers between a and b, where a and b are both real numbers. For example, the numerical range "6-22" means that all real numbers between "6-22" have been listed throughout, and "6-22" is only a shorthand representation of a combination of these values.
The "range" disclosed herein may take the form of a lower limit and an upper limit, which may be one or more lower limits and one or more upper limits, respectively.
In the present invention, the term "and/or" as used herein refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
In the present invention, each reaction or operation step may be performed sequentially or sequentially unless otherwise indicated. Preferably, the reaction processes herein are performed sequentially.
Unless otherwise defined, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any method or material similar or equivalent to those described may be used in the present invention.
The invention provides ODS steel with an aluminum alloying coating and a preparation method thereof, which are prepared by combining surface stirring friction treatment and an electric arc spraying process, so that a structure with fine grains and uniformly distributed oxide dispersion particles is obtained, and a steel layer with fine grain structure and finely distributed matrix with fine dispersion particles is obtained, so that the ODS steel is used for preparing ODS aluminum alloy and provides a new thought for developing the material in a nuclear reactor.
The invention relates to ODS steel with an aluminum alloying coating, which comprises the following components in percentage by weight: 4% -6%, Y 2 O 3 :0.50 to 1.50 percent, cr:12.00% -14.00%, ti:0.50% -1.00%, mn: 0.70-1.00%, and the balance of Fe and unavoidable trace impurities.
ODS steel with aluminum alloyed coating comprises ferrite matrix and oxide dispersion particles distributed on the matrix, Y 2 O 3 Can form uniformly distributed nano-scale dispersion particles, and can be used for preparing ODS aluminum-containing alloy.
The thickness of the ODS steel with the aluminum alloy coating is 150-200 mu m, the average particle diameter of the oxide dispersion particles is 20 mu m, and the average particle diameter of the dispersion oxide particles is 60nm.
Referring to FIG. 1, the ODS steel with the aluminum alloy coating and the preparation method thereof of the invention comprise the following steps:
s1, preparing 436 stainless steel by adopting vacuum arc melting and water-cooling copper mold vacuum suction casting, hot rolling into a 20mm thick steel plate, and annealing for later use;
s2, polishing and cleaning the surface of the 436 stainless steel plate prepared in the step S1, mixing nano yttrium oxide powder, deionized water and polyvinyl alcohol to form slurry, scraping the slurry on the surface of the steel plate by using a scraper, and drying in vacuum for later use;
sequentially polishing the steel plate by adopting 1000, 1500 and 2000-mesh sand paper, and sequentially carrying out ultrasonic cleaning by adopting absolute ethyl alcohol and acetone; the slurry preparation steps specifically comprise: nanometer yttrium oxide powder, polyvinyl alcohol and deionized water are respectively weighed according to the mass fractions of 9% -11%, 19% -21% and 69% -71%, one ten thousandth of high-precision day bisection is adopted, firstly polyvinyl alcohol is added into the deionized water, electromagnetic stirring is carried out for 14-16 min at the rotating speed of 900-1100 rmp, then nanometer yttrium oxide powder is added, and electromagnetic stirring is carried out for 25-30 min at the rotating speed of 1400-1600 rmp, thus obtaining Y 2 O 3 A slurry;
the slurry of 50-100 μm was knife coated using a doctor blade, and then dried in a vacuum oven at 80℃for 60 minutes.
S3, coating Y prepared in the step S2 2 O 3 Performing surface friction stir treatment on the coating surface of the steel plate coated with the slurry by using a GCr15 alloy hemispherical cutter to obtain an ODS steel layer;
the radius of the GCr15 alloy hemispherical cutter is 6-8 mm;
during the surface friction stir treatment, the surface of the steel plate is coated with lubricating grease, the cutter is pressed down for 150-200 mu m, the rotating speed of the cutter is 300-600 rmp, and the feeding rate is 100mm/min.
And S4, sequentially carrying out sand blasting and cleaning on the ODS steel layer prepared in the step S3, spraying 4N high-purity aluminum serving as a raw material on the surface of the ODS steel layer by using an arc spraying gun, and carrying out vacuum diffusion annealing to obtain the aluminum alloy ODS steel layer with fine grains and uniformly distributed oxide dispersion particles.
The sand blasting pressure is 0.4-0.6 MPa, brown corundum is adopted as sand grains, the sand blasting treatment leads the surface roughness Ra of the ODS steel layer to be 1.8-2.4 mu m, and absolute ethyl alcohol and acetone are sequentially adopted for ultrasonic cleaning;
the mass percentage of each component of the 4N high-purity aluminum wire is 99.996 percent of Al, the balance is unavoidable impurities, the diameter is 2mm, and the arc spraying process parameters are as follows: arc voltage is 30-45V, arc current is 300-400A, spraying distance is 100-350 mm, and surface thickness is 0.5-1.0 mm;
the temperature of the vacuum diffusion annealing process is 450-600 ℃ and the time is 4-16 h.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of tough ODS steel with aluminum alloying coating
The invention selects pure iron, pure chromium, ferromanganese, ferrotitanium, 4N6 grade pure aluminum wire, nanometer yttrium oxide powder and the like as raw materials. Obtaining a nuclear 436 steel substrate through vacuum arc melting, vacuum copper mold suction casting and a thermal deformation process; introducing nano yttrium oxide powder into a substrate through stirring friction treatment to obtain an ODS steel layer; an ODS steel coating containing aluminum is obtained through arc spraying and vacuum heat treatment annealing.
The preparation process of the invention specifically comprises the following steps:
s1, preparing an as-cast alloy by adopting vacuum arc melting and water-cooling copper die vacuum suction casting according to the component proportioning requirements, and obtaining a 436 stainless steel substrate with the thickness of 20mm after hot rolling and annealing.
S2, sequentially polishing the surface of the 436 stainless steel plate prepared in the step S1 by using 1000, 1500 and 2000-mesh sand paper, sequentially ultrasonically cleaning the steel plate by using absolute ethyl alcohol and acetone, respectively weighing nano yttrium oxide powder, polyvinyl alcohol and deionized water according to mass fractions of 9%, 19% and 70%, respectively weighing the nano yttrium oxide powder, the polyvinyl alcohol and the deionized water uniformly in a high-precision way, firstly adding the polyvinyl alcohol into the deionized water, carrying out electromagnetic stirring at a rotating speed of 1100rmp for 14min, then adding the nano yttrium oxide powder, carrying out electromagnetic stirring at a rotating speed of 1600rmp for 30min to obtain slurry, carrying out blade coating by using a scraper to obtain a slurry coating with a thickness of 50 mu m, and then drying the slurry coating in a vacuum drying box at 80 ℃ for 60min;
s3, coating Y prepared in the step S2 2 O 3 Coating graphene grease on the surface of a steel plate coated with the slurry, pressing down 150 mu m by using a GCr15 alloy hemispherical cutter with the radius of 6mm, and carrying out surface friction stir treatment on the surface of the coating at the rotation speed of 600rmp and the feeding speed of 100mm/min to obtain an ODS steel layer;
s4, adopting brown corundum sand grains to carry out sand blasting on the ODS steel layer prepared in the step S3 at the pressure of 0.41MPa to enable the surface roughness Ra to be 1.9 mu m, sequentially adopting absolute ethyl alcohol and acetone for ultrasonic cleaning, taking 4N 6-grade high-purity aluminum wires with the diameter of 2mm as raw materials, spraying the aluminum wires at the arc voltage of 32V and the arc current of 320A for the distance of 100mm, spraying the aluminum alloy coating on the surface of the aluminum alloy steel layer by using an arc spray gun to obtain a coating with the thickness of 0.6mm, and carrying out vacuum diffusion annealing at the temperature of 450 ℃ for 16h to obtain the ODS steel with the aluminum alloy coating.
The ODS steel with the aluminum alloy coating, which is obtained by the embodiment, has fine crystal grains and oxide dispersion particles uniformly distributed, forms a composite alloy structure with an aluminum alloy solid solution strengthening matrix and an oxide dispersion phase with excellent high-temperature stability, obviously improves the mechanical properties of the alloy and simultaneously gives consideration to certain corrosion resistance and irradiation resistance.
Example 2
Preparation of corrosion resistant ODS steel with aluminum alloyed coating
The invention selects pure iron, pure chromium, ferromanganese, ferrotitanium, 4N6 grade pure aluminum wire, nanometer yttrium oxide powder and the like as raw materials. Obtaining a nuclear 436 steel substrate through vacuum arc melting, vacuum copper mold suction casting and a thermal deformation process; introducing nano yttrium oxide powder into a substrate through stirring friction treatment to obtain an ODS steel layer; an ODS steel coating containing aluminum is obtained through arc spraying and vacuum heat treatment annealing.
The preparation process of the invention specifically comprises the following steps:
s1, preparing an as-cast alloy by adopting vacuum arc melting and water-cooling copper die vacuum suction casting according to the component proportioning requirements, and obtaining a 436 stainless steel substrate with the thickness of 15mm after hot rolling and annealing.
S2, sequentially polishing the surface of the 436 stainless steel plate prepared in the step S1 by adopting 1000, 1500 and 2000-mesh sand paper, sequentially carrying out ultrasonic cleaning by adopting absolute ethyl alcohol and acetone, respectively weighing 11%, 20% and 69% of nano yttrium oxide powder, polyvinyl alcohol and deionized water according to mass fractions of 11%, 20% and 69% of deionized water respectively, uniformly weighing the nano yttrium oxide powder in a high-precision way, firstly adding polyvinyl alcohol into the deionized water, carrying out electromagnetic stirring at a rotating speed of 1000rmp for 15min, then adding nano yttrium oxide powder, carrying out electromagnetic stirring at a rotating speed of 1500rmp for 27min to obtain slurry, carrying out blade coating by using a scraper to obtain a slurry coating with a thickness of 100 mu m, and then drying the slurry coating in a vacuum drying box at a temperature of 77 ℃ for 55min;
s3, coating Y prepared in the step S2 2 O 3 Coating graphene grease on the surface of a steel plate coated with the slurry, pressing down the steel plate by using a GCr15 alloy hemispherical cutter with the radius of 8mm by 200 mu m, and carrying out surface friction stir treatment on the surface of the coating at the rotating speed of 300rmp and the feeding speed of 50mm/min to obtain an ODS steel layer;
s4, adopting brown corundum sand grains to carry out sand blasting on the ODS steel layer prepared in the step S3 at the pressure of 0.50MPa to enable the surface roughness Ra to be 2.5 mu m, sequentially adopting absolute ethyl alcohol and acetone for ultrasonic cleaning, taking 4N 6-grade high-purity aluminum wires with the diameter of 2mm as raw materials, spraying the aluminum wires to the surface of the aluminum wires at the arc voltage of 40V and the arc current of 350A for the spraying distance of 150mm, spraying the aluminum wires to obtain a 1.0mm thick coating by using an arc spray gun, and carrying out vacuum diffusion annealing at 600 ℃ for 12h to obtain the ODS steel with the aluminum alloy coating.
ODS steel with aluminum alloying coating obtained in the embodiment has deeper thermite diffusion depth, excellent corrosion resistance and introduced nano Y 2 O 3 The dispersed particles improve the mechanical property of the alloy and compensate the softening phenomenon of ferritic steel with higher aluminum content.
Example 3
Preparation of ODS Steel coating sample
The invention selects pure iron, pure chromium, ferromanganese, ferrotitanium, 4N6 grade pure aluminum wire, nanometer yttrium oxide powder and the like as raw materials. Obtaining a nuclear 436 steel substrate through vacuum arc melting, vacuum copper mold suction casting and a thermal deformation process; introducing nano yttrium oxide powder into a substrate through stirring friction treatment to obtain an ODS steel layer; an ODS steel coating containing aluminum is obtained through arc spraying and vacuum heat treatment annealing.
The preparation process of the invention specifically comprises the following steps:
s1, preparing an as-cast alloy by adopting vacuum arc melting and water-cooling copper die vacuum suction casting according to the component proportioning requirements, and obtaining a 436 stainless steel substrate with the thickness of 20mm after hot rolling and annealing.
S2, polishing the surface of the 436 stainless steel plate prepared in the step S1 by sequentially adopting 1000, 1500 and 2000-mesh sand paper, sequentially adopting absolute ethyl alcohol and acetone for ultrasonic cleaning, respectively weighing 10%, 21% and 69% of nano yttrium oxide powder, polyvinyl alcohol and deionized water according to the mass fraction of 10%, 21% and 69% of the nano yttrium oxide powder, uniformly weighing the nano yttrium oxide powder in a high-precision way, firstly adding polyvinyl alcohol into the deionized water, carrying out electromagnetic stirring at 900rmp rotation speed for 16min, then adding nano yttrium oxide powder, carrying out electromagnetic stirring at 1400rmp rotation speed for 25min to obtain slurry, carrying out blade coating to obtain a slurry coating with the thickness of 90 mu m, and then putting the slurry coating into a vacuum drying box for drying at 80 ℃ for 60min;
s3, coating Y prepared in the step S2 2 O 3 Coating graphene grease on the surface of a steel plate coated with the slurry, pressing down 50 mu m by using a GCr15 alloy hemispherical cutter with the radius of 8mm, and carrying out surface friction stir treatment on the surface of the coating at the rotation speed of 500rmp and the feeding speed of 100mm/min to obtain an ODS steel layer;
s4, adopting brown corundum sand grains to carry out sand blasting on the ODS steel layer prepared in the step S3 at the pressure of 0.41MPa to enable the surface roughness Ra to be 2.1 mu m, sequentially adopting absolute ethyl alcohol and acetone for ultrasonic cleaning, taking 4N 6-grade high-purity aluminum wires with the diameter of 2mm as raw materials, spraying the aluminum wires at the arc voltage of 40V and the arc current of 375A for the distance of 250mm, spraying the aluminum alloy coating on the surface of the aluminum alloy steel layer by using an arc spray gun to obtain a 1.0mm thick coating, and carrying out vacuum diffusion annealing at the temperature of 530 ℃ for 8 hours to obtain the ODS steel with the aluminum alloy coating.
The ODS steel with the aluminum alloy coating, which is obtained by the embodiment, has fine crystal grains, oxide dispersion particles are uniformly distributed, and the aluminum diffusion layer further improves the corrosion resistance of the alloy, and has good mechanical property, corrosion resistance and irradiation resistance.
In summary, the ODS steel with the aluminum alloy coating and the preparation method thereof enable the alloy to have fine crystal grains and uniform nano-scale dispersion particle distribution, and can be used for preparing the ODS aluminum-containing alloy.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The preparation method of the ODS steel with the aluminum alloying coating is characterized by comprising the following steps of:
mixing nanometer yttrium oxide powder, deionized water and polyvinyl alcohol to prepare Y 2 O 3 The sizing agent is coated on the surface of the steel plate in a scraping way, and is dried in vacuum for standby;
carrying out surface stirring friction treatment on the coating surface of the steel plate after vacuum drying to obtain an ODS steel layer;
and sequentially carrying out sand blasting and cleaning on the ODS steel layer, carrying out surface spraying by taking 4N high-purity aluminum as a raw material, and carrying out vacuum diffusion annealing to obtain the aluminum alloy ODS steel layer with oxide dispersion particles.
2. The method for manufacturing ODS steel having an aluminum alloy coating according to claim 1, wherein the steel sheet is manufactured by vacuum arc melting and water-cooled copper die vacuum suction casting, and the steel sheet is polished and cleaned on the surface of the steel sheet before blade coating.
3. According to claimThe method for producing ODS steel having an aluminum alloy coating according to claim 1, characterized in that Y 2 O 3 In the slurry, the mass fraction of the nano yttrium oxide powder is 9-11%, the mass fraction of the polyvinyl alcohol is 19-21%, and the mass fraction of the deionized water is 69-71%.
4. The method for producing an ODS steel having an aluminum alloy coating according to claim 1, characterized in that Y 2 O 3 The preparation process of the slurry is as follows:
adding polyvinyl alcohol into deionized water, carrying out electromagnetic stirring for 14-1 min at 900-1100 rmp, adding nano yttrium oxide powder, and carrying out electromagnetic stirring for 25-30 min at 1400-1600 rmp to obtain Y 2 O 3 And (3) sizing.
5. The method for manufacturing ODS steel having an aluminum alloy coating according to claim 1, wherein the thickness of the blade coating is 50-100 μm, the temperature of vacuum drying is 75-80 ℃, and the time is 50-60 min.
6. The method for manufacturing an ODS steel with an aluminum alloy coating according to claim 1, characterized in that grease is applied to a coating surface of a steel sheet after vacuum drying, a cutter is pressed down by 150 to 200 μm, the rotation speed of the cutter is 300 to 600rmp, and the feed rate is 50 to 100mm/min, and surface friction stir processing is performed.
7. The method for manufacturing ODS steel having an aluminum alloy coating according to claim 6, wherein the cutter is a GCr15 alloy hemispherical cutter having a radius of 6-8 mm.
8. The method for producing ODS steel having an aluminum-alloyed coating according to claim 1, wherein the blasting pressure is 0.4-0.6 MPa, the surface roughness Ra of the ODS steel layer after blasting is 1.8-2.4 μm, the arc voltage of the spraying is 30-45V, the arc current is 300-400A, the spraying distance is 100-350 mm, and the face thickness is 0.5-1.0 mm.
9. The method for manufacturing an ODS steel having an aluminum alloy coating according to claim 1, characterized in that the vacuum diffusion annealing is performed at a temperature of 450 to 600 ℃ for a time of 4 to 16 hours.
10. An ODS steel having an aluminum alloy coating layer, characterized in that it is prepared by the method for preparing an ODS steel having an aluminum alloy coating layer according to any one of claims 1 to 9, comprising, in weight percent, al:4% -6%, Y 2 O 3 :0.50 to 1.50 percent, cr:12.00% -14.00%, ti:0.50% -1.00%, mn: 0.70-1.00%, and the balance of Fe and unavoidable trace impurities.
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