CN114032437B - Novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating and preparation method thereof - Google Patents
Novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating and preparation method thereof Download PDFInfo
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- CN114032437B CN114032437B CN202111347065.XA CN202111347065A CN114032437B CN 114032437 B CN114032437 B CN 114032437B CN 202111347065 A CN202111347065 A CN 202111347065A CN 114032437 B CN114032437 B CN 114032437B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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Abstract
The invention provides a preparation method of a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating, which comprises the following steps: coating a powder coating on the surface of a substrate and then drying to obtain a coating; carrying out laser cladding on the coating to obtain a Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating; the powder coating comprises: mixing the powder and the solvent; the mixed powder comprises: fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder. Aiming at the lower surface hardness and the poorer wear resistance of the aluminum alloy, the invention prepares a novel composite high-entropy alloy coating by laser cladding so as to improve the adverse performance, change the metallographic structure, improve the surface strength and hardness and prolong the service life of aluminum and aluminum alloy parts. The invention also provides a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating and a preparation method thereof.
Background
The aluminum alloy has small specific gravity, low density, fast heat transfer, high ground crust medium content and simple mining, and is widely applied to various industries. However, aluminum alloys have low hardness and poor wear resistance, and are difficult to be hardened by conventional heat treatment methods, which limits their application to some extent. At present, two main methods for improving the surface wear resistance of the aluminum alloy are as follows: one is to improve the overall wear resistance of the aluminum alloy; the other is to improve the wear resistance of the aluminum alloy surface by surface modification. Commonly used aluminum alloy surface modification techniques include anodization, electroplating, electroless plating, chemical oxidation, Physical Vapor Deposition (PVD), Chemical Vapor Deposition (CVD), spray coating, ion implantation, micro-arc oxidation, and the like. However, the surface coating obtained on the aluminum alloy by these methods is thin or the adhesion strength of the coating to the substrate is not high, and is liable to crack and peel, which is a simple mechanical adhesion or diffusion adhesion.
Disclosure of Invention
In view of the above, the invention aims to provide a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating and a preparation method thereof.
The invention provides a preparation method of a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating, which comprises the following steps:
coating a powder coating on the surface of a substrate and then drying to obtain a coating;
carrying out laser cladding on the coating to obtain a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating;
the powder coating comprises: mixing the powder and the solvent;
the mixed powder comprises: fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder.
Preferably, the substrate is an aluminum alloy.
Preferably, the molar ratio of the Fe powder, the Co powder, the Cr powder, the Cu powder, the Ti powder and the Y powder is (56-84): (59-118): (52-78): (64-96): (48-57): 13.35-22.25).
Preferably, the particle size of the mixed powder is 300-500 meshes.
Preferably, the solvent is alcohol.
Preferably, the thickness of the coating is 250-450 microns.
Preferably, the drying temperature is 80-120 ℃.
Preferably, the laser cladding is performed under the protection of an argon atmosphere.
Preferably, the current in the laser cladding process is 80-120A, the scanning speed is 100-400 mm/min, the pulse width is 2-5 ms, the frequency is 5-20 Hz, and the defocusing amount is 1-5 mm.
The invention provides a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating prepared by the method in the technical scheme.
Aiming at the lower surface hardness and the poorer wear resistance of the aluminum alloy, the invention prepares a novel composite high-entropy alloy coating by laser cladding so as to improve the poor performance of the aluminum alloy. The novel high-entropy alloy coating prepared by laser cladding can improve the poor performance, change the metallographic structure, improve the surface strength and hardness and prolong the service life of aluminum and aluminum alloy parts.
The invention improves the surface performance of the aluminum alloy by preparing the multi-principal-element alloy coating on the surface of the aluminum alloy through laser cladding, and the selected element powder comprises the following components: pure Fe powder, pure Cr powder (chromium), pure Co powder (cobalt), pure Cu powder, pure Ti powder and Y powder (yttrium), wherein the powder adopts analytically pure (AR) and has the granularity of about 300-500 meshes. Fe can increase the mixing entropy; cr can obviously improve the strength and hardness of the alloy, simultaneously enables the alloy to have stronger corrosion resistance, and can also react with Al to improve the oxidation resistance of the alloy; co has excellent high temperature resistance and corrosion resistance, and can also obviously improve the strength; the addition of Ti element makes the alloy easier to form BCC structure, and Y element can enhance the integral shaping and toughness. In order to generate a sufficient amount of toughness phase and prevent cracking in the selection of an alloy system, elements with small mixing enthalpy among the elements are selected as much as possible from the perspective of the mixing enthalpy, and the elements are generally between-40 and +15 kJ/mol; the surface is formed beautifully; a uniform cladding layer can be formed.
The high-entropy alloy is also called multi-principal-element alloy, is broadly defined as a solid solution consisting of 5 or more than 5 elements, and the atomic fraction of the main elements is in the range of 5-35%; the high-entropy alloy has the characteristics of higher entropy value and difficult diffusion of constituent element atoms, is easy to obtain a solid solution phase and a nano structure with high thermal stability, even an amorphous structure, and has better mechanical property.
In the invention, the laser beam has good coherence, strong directivity and high energy density, and the surface of the material can be modified by laser. Laser surface modification refers to the use of laser irradiation to produce a series of thin layers of physical and chemical changes to improve the overall properties of the material surface. The laser surface modification technology has the advantages of high cooling speed, short laser processing time, no special requirement on the size of a workpiece, easy obtainment of ideal surface modification layer structure, easy realization of selective alloying, automation and the like, can obtain a uniform and compact strengthening layer with fine grains on the surface of the aluminum alloy, and belongs to metallurgical bonding between the strengthening layer and a matrix.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a preparation method of a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating, which comprises the following steps:
coating a powder coating on the surface of a substrate and then drying to obtain a coating;
and carrying out laser cladding on the coating to obtain the novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating.
In the present invention, the substrate is preferably an aluminum alloy, more preferably 1050 aluminum alloy; the Al content in the 1050 aluminum alloy is preferably greater than or equal to 99.5 wt%, more preferably 99.5 wt% to 99.8 wt%, and most preferably 99.6 wt% to 99.7 wt%.
In the present invention, the substrate is preferably subjected to a treatment to apply a powder coating, the treatment preferably comprising:
and polishing, degreasing, cleaning and drying the substrate.
In the invention, the grinding is preferably performed by using sand paper, and more preferably, the base body is ground to be flat by using 120-800 meshes of sand paper respectively.
In the present invention, the degreasing method is preferably degreasing by using acetone.
In the present invention, the cleaning method is preferably cleaning with alcohol.
In the present invention, the drying is preferably blow drying.
In the present invention, the powder coating comprises: mixing the powder and the solvent.
In the present invention, the mixed powder includes: fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder.
In the present invention, the purity of the Fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder (mixed powder) is preferably analytically pure.
In the present invention, the particle size of the Fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder (mixed powder) is preferably 300 to 500 mesh, more preferably 350 to 450 mesh, and most preferably 400 mesh.
In the invention, the molar ratio of the Fe powder, the Co powder, the Cr powder, the Cu powder, the Ti powder and the Y powder is preferably (56-84): (59-118): (52-78): (64-96): (48-57): 13.35-22.25), more preferably (60-80): 70-110): 55-75): 70-90): 50-55): 15-20, most preferably (65-75): 80-100): 60-70): 75-85): 52-53): 16-18.
In the present invention, the solvent is preferably alcohol.
In the present invention, the mass ratio of the mixed powder to the solvent is preferably 1: (1-3), more preferably 1: (1.5-2.5), most preferably 1: 2.
in the present invention, the preparation method of the powder coating preferably includes:
and mixing the mixed powder with a solvent and grinding to obtain the powder coating.
In the present invention, the grinding is preferably carried out in a mortar; the grinding time is preferably 0.5-2 hours, more preferably 1-1.5 hours, and most preferably 1.2-1.3 hours; the grinding is preferably to a non-viscous paste.
In the invention, the thickness of the coating is preferably 250-450 micrometers, more preferably 300-400 micrometers, and most preferably 350 micrometers; a doctor blade is preferably used to control the coating thickness during the coating process.
In the present invention, the drying method is preferably drying, more preferably drying in a resistance furnace; the resistance furnace is preferably a KSL-1200X box type resistance furnace. In the invention, the drying temperature is preferably 80-120 ℃, more preferably 90-110 ℃, and most preferably 100 ℃; the drying heat preservation time is preferably 1-4 hours, more preferably 2-3 hours, and most preferably 2.5 hours; in the drying process, the temperature is preferably increased by 8-12 ℃ per minute to 80-120 ℃, more preferably increased by 9-11 ℃ per minute, and most preferably increased by 10 ℃ per minute.
In the present invention, the laser cladding is preferably performed under the protection of an argon atmosphere. In the invention, the laser cladding preferably adopts LWS-1000 type Nd: YAG laser welder; the LWS-1000 type Nd: the YAG laser welding machine adopts Nd: YAG, laser wavelength is 1.064 microns; the output power is 0-1000W, the pulse frequency is 0-100 Hz, the pulse width is 0.5-10 ms, the working current is 100-450A, the beam divergence angle is less than 15mrad, the power fluctuation is less than 3%, the spot diameter is 0.6-1.0 mm, and the stroke of the workbench is 400mm x 600mm x 300 mm.
In the invention, the current in the laser cladding process is preferably 80-120A, more preferably 90-110A, and most preferably 100A; the scanning speed is preferably 100-400 mm/min, more preferably 150-350 mm/min, more preferably 200-300 mm/min, and most preferably 250 mm/min; the pulse width is preferably 2-5 ms, and more preferably 3-4 ms; the frequency is preferably 5-20 Hz, more preferably 10-15 Hz, and most preferably 12-13 Hz; the defocusing amount is preferably 1-5 mm, more preferably 2-4 mm, and most preferably 3 mm; the size of the cladding area is preferably (5-15) mm, more preferably (8-12) mm, and most preferably 10 mm-10 mm.
The invention provides a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating prepared by the method in the technical scheme; the component range of the novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating is consistent with that of the mixed powder in the technical scheme, and the thickness range is consistent with that of the coating in the technical scheme, so that the details are not repeated.
According to the invention, the novel coating is cladded under the optimized process parameters, the hardness of the cladding layer is obviously improved compared with that of the base material, the highest hardness is improved by 24 times, the average hardness of the middle part of the cladding layer is improved by 16 times compared with that of the base material, and the wear resistance is improved by 30% maximally compared with that of the base material.
The invention improves the surface performance of the aluminum alloy by preparing the multi-principal-element alloy coating on the surface of the aluminum alloy through laser cladding, and the selected element powder comprises the following components: pure Fe powder, pure Cr powder (chromium), pure Co powder (cobalt), pure Cu powder, pure Ti powder and Y powder (yttrium), wherein the powder adopts analytically pure (AR) and has the granularity of about 300-500 meshes. Fe can increase the mixing entropy; cr can obviously improve the strength and hardness of the alloy, simultaneously enables the alloy to have stronger corrosion resistance, and can also react with Al to improve the oxidation resistance of the alloy; co has excellent high temperature resistance and corrosion resistance, and can also obviously improve the strength; the addition of Ti element makes the alloy easier to form BCC structure, and Y element can enhance the integral shaping and toughness. In order to generate a sufficient amount of toughness phase and prevent cracking in the selection of an alloy system, elements with small mixing enthalpy among the elements are selected as much as possible from the perspective of the mixing enthalpy, and the elements are generally between-40 and +15 kJ/mol; the surface is formed to be beautiful; a uniform cladding layer can be formed.
The base material adopted in the following embodiment of the invention is an aluminum sheet product provided by Beijing Jiaming platinum industry nonferrous metal Co., Ltd, and the equipment adopted in the laser cladding process is LWS-1000 type Nd: YAG laser welder; LWS-1000 type Nd: the YAG laser welding machine adopts Nd: YAG, laser wavelength is 1.064 microns; the output power is 0-1000W, the pulse frequency is 0-100 Hz, the pulse width is 0.5-10 ms, the working current is 100-450A, the beam divergence angle is less than 15mrad, the power fluctuation is less than 3%, the spot diameter is 0.6-1.0 mm, and the stroke of the workbench is 400mm x 600mm x 300 mm.
Examples 1 to 5
And (3) polishing and flattening the aluminum sheet by using 120-800 meshes of abrasive paper respectively, washing oil stain by using acetone, then washing by using alcohol, and drying by blowing to obtain the base plate.
According to the use amount of each raw material in table 1, pure Cr powder, pure Co powder, pure Cu powder, pure Ti powder and Y powder (the particle size of each powder is 300-500 mesh) are mixed with alcohol, and ground in a mortar for about 1 hour to form non-viscous paste, so as to obtain the coating.
Presetting a coating on the substrate by the coating, and controlling the thickness of the coating to be 250 mu m by a scraper; and (3) drying the coated coating in a KSL-1200X box type resistance furnace, raising the temperature in the KSL-1200X box type resistance furnace by 10 ℃ per minute, raising the temperature to 100 ℃, and then preserving the heat for 4 hours to dry the coating.
Under the protection of argon atmosphere, adopting LWS-1000 type Nd: YAG laser welder carries out laser cladding and laser cladding on the coating, and the technological parameters are as follows: the current is 90A, the scanning speed is 200mm/min, the pulse width is 2ms, the frequency is 10Hz, and the defocusing amount is 1 mm; obtaining the Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating.
The performance of the Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating prepared by the embodiment of the invention is detected, and the detection method of the surface hardness comprises the following steps: measuring the microhardness of the cross section of the laser cladding layer by using a VTD401 digital display microVickers hardness tester, wherein the load is 100gf, and the loading time is 10 s; the hardness testing direction is the horizontal direction, hardness measurement is carried out along the cladding layer in the horizontal direction, one point is made at an interval of 0.5mm, 5-6 points are measured on the cladding layer, 3-4 points are measured on the base material, and an average value is obtained.
The method for detecting the hardness of the joint of the coating and the base material comprises the following steps: measuring the microhardness of the cross section of the laser cladding layer by using a VTD401 digital display microVickers hardness tester, wherein the load is 100gf, and the loading time is 10 s; the hardness testing direction is a vertical direction, one point is measured at an interval of 0.25mm in the vertical direction, 5-6 points are measured on the cladding layer, 3-4 points are measured on the base material, and an average value is taken.
The friction coefficient detection method comprises the following steps: the wear test is carried out by adopting MMW-1A microcomputer controlled universal friction wear testing machine of Mexico-testing technology Limited company of Jinan Yihua, the load is 20N, the rotating speed is 100r/min, the testing time is 15min, and the precision of the wear quality is 10 -4 g, measuring by using an electronic scale; the sample is prepared as
The corresponding counter grinding ring uses the No. 45 steel counter grinding ring after heat treatment; the specific test conditions are as follows: the speed of rotation is 100rpm/min, the test force is maintained under a load of 20N, in the form of dry friction, and the test time is 20 min.
The results are shown in Table 1.
TABLE 1 test results of the amount of each metal powder and the properties of the prepared coatings in examples 1 to 5 of the present invention
According to the embodiment, the multi-principal-element alloy coating is prepared on the surface of the aluminum alloy through laser cladding so as to improve the surface performance of the aluminum alloy, and the selected element powder comprises the following components: pure Fe powder, pure Cr powder (chromium), pure Co powder (cobalt), pure Cu powder, pure Ti powder and Y powder (yttrium), wherein the powder adopts analytically pure (AR), and the particle size is about 300-500 meshes. Fe can increase the mixing entropy; cr can obviously improve the strength and hardness of the alloy, simultaneously enables the alloy to have stronger corrosion resistance, and can also react with Al to improve the oxidation resistance of the alloy; co has excellent high temperature resistance and corrosion resistance, and can also obviously improve the strength; the addition of Ti element makes the alloy easier to form BCC structure, and Y element can enhance the integral shaping and toughness. In order to generate a sufficient amount of toughness phase and prevent cracking in the selection of an alloy system, elements with small mixing enthalpy among the elements are selected as much as possible from the perspective of the mixing enthalpy, and the elements are generally between-40 and +15 kJ/mol; the surface is formed beautifully; a uniform cladding layer can be formed.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A preparation method of a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating comprises the following steps:
coating a powder coating on the surface of a substrate and then drying to obtain a coating;
carrying out laser cladding on the coating to obtain a novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating;
the powder coating comprises: mixing the powder and the solvent;
the mixed powder comprises: fe powder, Co powder, Cr powder, Cu powder, Ti powder and Y powder;
the mass ratio of the Fe powder to the Co powder to the Cr powder to the Cu powder to the Ti powder to the Y powder is 1.10:1.06:1.05:1.15:1.12: 0.20.
2. The method of claim 1, wherein the substrate is an aluminum alloy.
3. The method according to claim 1, wherein the particle size of the mixed powder is 300-500 mesh.
4. The method of claim 1, wherein the solvent is an alcohol.
5. The method of claim 1, wherein the coating has a thickness of 250 to 450 micrometers.
6. The method according to claim 1, wherein the drying temperature is 80 to 120 ℃.
7. The method of claim 1, wherein the laser cladding is performed under a protective argon atmosphere.
8. The method of claim 1, wherein the current in the laser cladding process is 80-120A, the scanning speed is 100-400 mm/min, the pulse width is 2-5 ms, the frequency is 5-20 Hz, and the defocusing amount is 1-5 mm.
9. A novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating prepared by the method of claim 1.
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| CN202111347065.XA CN114032437B (en) | 2021-11-15 | 2021-11-15 | Novel Fe-Cr-Co-Cu-Ti-Y multi-element high-entropy alloy coating and preparation method thereof |
| PCT/CN2021/135276 WO2023082386A1 (en) | 2021-11-15 | 2021-12-03 | New-type fe-cr-co-cu-ti-y multi-element high-entropy alloy coating layer and preparation method therefor |
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| CN104313572B (en) * | 2014-11-14 | 2017-10-03 | 重庆理工大学 | A kind of preparation method of aluminum alloy surface laser alloying Al Cr Ti Si Cu multi-principal elements alloy coatings |
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