CN116352248B - Method for preparing modified layer on surface of magnesium alloy and magnesium alloy - Google Patents
Method for preparing modified layer on surface of magnesium alloy and magnesium alloy Download PDFInfo
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- CN116352248B CN116352248B CN202310394116.7A CN202310394116A CN116352248B CN 116352248 B CN116352248 B CN 116352248B CN 202310394116 A CN202310394116 A CN 202310394116A CN 116352248 B CN116352248 B CN 116352248B
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 143
- 238000000034 method Methods 0.000 title claims abstract description 63
- 238000003756 stirring Methods 0.000 claims abstract description 131
- 239000000956 alloy Substances 0.000 claims abstract description 120
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 119
- 239000000758 substrate Substances 0.000 claims abstract description 57
- 238000003825 pressing Methods 0.000 claims abstract description 35
- 238000003466 welding Methods 0.000 claims abstract description 35
- 238000012545 processing Methods 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910000691 Re alloy Inorganic materials 0.000 claims description 3
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 18
- 230000004048 modification Effects 0.000 abstract description 18
- 239000010410 layer Substances 0.000 description 116
- 238000005260 corrosion Methods 0.000 description 36
- 230000007797 corrosion Effects 0.000 description 33
- 239000000463 material Substances 0.000 description 32
- 230000008569 process Effects 0.000 description 23
- 239000011248 coating agent Substances 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 11
- 238000005520 cutting process Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 9
- 238000005498 polishing Methods 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 244000137852 Petrea volubilis Species 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 229910000765 intermetallic Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000010288 cold spraying Methods 0.000 description 5
- 239000007769 metal material Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000003856 thermoforming Methods 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
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- 150000001875 compounds Chemical class 0.000 description 2
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- 238000004372 laser cladding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000013519 translation Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 238000005054 agglomeration Methods 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 239000006023 eutectic alloy Substances 0.000 description 1
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- 238000007542 hardness measurement Methods 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/129—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding specially adapted for particular articles or workpieces
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The application provides a method for preparing a modified layer on the surface of a magnesium alloy, which comprises the following steps: preparing an as-cast high-entropy alloy sheet; tightly attaching one surface of the high-entropy alloy sheet and the surface of the magnesium alloy substrate, and fixing the high-entropy alloy sheet and the surface of the magnesium alloy substrate on a friction stir welding machine by adopting a clamping tool of the friction stir welding machine; the stirring head is a needleless stirring head, and the needleless stirring head is adopted to carry out multi-pass friction stir processing along the surface of the high-entropy alloy sheet so as to connect the high-entropy alloy sheet with the magnesium alloy substrate; wherein the shaft shoulder pressing amount of the needleless stirring head is smaller than the thickness of the high-entropy alloy sheet, the rotating speed of the needleless stirring head is 5000-10000 rpm, and the advancing speed is 500-1000 mm/min. The thickness and uniformity of the modified layer obtained by the method are easier to control, and the thickness of the modified layer can be controlled. The application also provides a magnesium alloy with a surface modification layer.
Description
Technical Field
The application relates to the field of surface modification of metal materials, in particular to a method for preparing a modified layer on the surface of a magnesium alloy and the magnesium alloy with the surface modified layer obtained by adopting the method.
Background
Magnesium alloy is widely applied to the fields of rail transit, automobiles, aerospace equipment, electronic component shells, medical appliances and the like due to the performances of small density, good electromagnetic shielding property, high specific strength, good mechanical property and the like. However, magnesium alloy has strong electronegativity and high chemical activity, and the surface of the magnesium alloy is extremely easy to oxidize in a humid environment to form a loose and porous oxide film. Under alkaline or neutral environment, the oxide film has a certain corrosion-resistant protection effect on the magnesium alloy matrix, but in a humid environment containing chloride ions, the oxide film is quickly destroyed to form sodium chloride, the sodium chloride has no protection effect on the magnesium alloy matrix, and the matrix material can be corroded continuously; the poor corrosion resistance severely restricts the application of magnesium alloy as a structural material in various fields.
Compared with the traditional alloy, the high-entropy alloy has the advantages of high thermal stability, excellent impact toughness, high-temperature corrosion resistance, wear resistance and the like. The high-entropy alloy surface modification layer is prepared on the surface of the magnesium alloy, so that the advantage of light weight of the magnesium alloy matrix can be exerted, and the problem of poor wear resistance and corrosion resistance of the magnesium alloy matrix can be solved. In the prior art, the preparation method of the commonly used high-entropy alloy surface modification layer comprises two methods of hot forming and cold forming; the hot forming process mainly comprises laser cladding, hot spraying and the like. By adopting the thermoforming process, the substrate and the coating material can be melted, heat sources in the process are concentrated, the temperature is higher, air holes, cracks, brittle intermetallic compounds and the like are easily generated in the cladding layer due to chilling heat, the thermal influence on the substrate is large, and the brittle intermetallic compounds are easily generated. The cold forming process is to shoot high-entropy alloy powder onto a substrate to form a compact coating by supersonic gas, solid-phase gas flow and the like at normal temperature, and if a large-sheet or block coating material is adopted, the high-entropy alloy powder cannot be rapidly shot, so that the combination of a high-entropy alloy surface modified layer and a matrix is not firm.
Chinese patent CN113445041B discloses a method for preparing a low-cost light high-entropy alloy/alumina composite coating on the surface of magnesium alloy, mixing alumina particles with high-entropy alloy powder, mixing by a mixer to obtain high-entropy alloy/alumina composite powder, spraying the high-entropy alloy/alumina composite coating on the surface of magnesium alloy by using supersonic cold spraying technology, and finally preparing the coating with a thickness of 0.05-1 mm. However, the surface cold spraying process has the problems of poor interface combination with a substrate, difficult realization of a coating with large thickness, and the like. Furthermore, the prior art adopts powdery high-entropy alloy materials, and the thickness, the flatness and the uniformity of the prepared coating are difficult to control.
Disclosure of Invention
The application aims to solve the problems that the high-entropy alloy coating is prepared on the surface of the magnesium alloy in the prior art, a large-thickness coating cannot be formed by a surface cold spraying method, and the thickness, the flatness and the uniformity of the coating are difficult to control by a laser cladding method.
In order to solve the technical problems, the application provides a method for preparing a thickness-controllable modified layer on the surface of a magnesium alloy, which comprises the following steps.
S1: preparing as-cast high-entropy alloy sheet with thickness of 0.2-1.5 mm.
S2: one surface of the high-entropy alloy sheet is tightly attached to the surface of the magnesium alloy substrate, and a clamping tool of a friction stir welding machine is adopted to fix the high-entropy alloy sheet to the friction stir welding machine.
S3: the stirring head is a needleless stirring head, and the needleless stirring head is adopted to carry out multi-pass friction stir processing along the surface of the high-entropy alloy sheet so as to connect the high-entropy alloy sheet with the magnesium alloy substrate; wherein the shaft shoulder pressing amount of the needleless stirring head is smaller than the thickness of the high-entropy alloy sheet, the rotating speed of the needleless stirring head is 5000-10000 rpm, and the advancing speed is 500-1000 mm/min.
According to the application, the high-entropy alloy sheet is used for preparing the magnesium alloy surface modified layer in a friction stir processing mode, and the material is locally plasticized through friction heat and plastic deformation heat, so that the high-entropy alloy sheet forms the modified layer on the magnesium alloy substrate, the material flow in the processing process can be effectively controlled, the processing defect caused by adopting a thermoforming mode is avoided, and the thickness and uniformity of the modified layer are easier to control. Furthermore, the application adopts the needleless stirring head, and the technology of high rotation speed and high welding speed is matched to accelerate the preparation efficiency, simultaneously reduce the heat input, avoid the problem of increasing brittle intermetallic compounds, avoid the quality problem of the prepared modified layer, and ensure that the prepared modified layer is smoother and more uniform. In addition, in the preparation process, the thickness of the modified layer can be controlled by controlling the thickness of the high-entropy alloy sheet and matching with the shaft shoulder pressing amount of the stirring head.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application is characterized in that a plurality of spiral grooves extending from the edge to the center are uniformly formed on the surface of the shaft shoulder of the needleless stirring head.
By adopting the scheme, the spiral groove structure is designed on the surface of the shaft shoulder, so that the heat input can be reduced, the material flow is promoted, the formation of holes and compounds is reduced, and the compactness of the modified layer is enhanced. In addition, the spiral groove is designed to extend from the edge to the center, so that the spiral groove has the function of feeding back, the metal at the edge of the stirring head is received at the center of the welding seam, plastic deformation metal materials can be effectively reduced from escaping in the high-speed stirring process, and the problem of uneven material mixing caused by needleless stirring is avoided.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application has 3 spiral grooves; the 3 spiral grooves are uniformly arranged on the shaft shoulder, one ends extending towards the center are not connected, and a blank is formed in the center.
By adopting the scheme, the plastic deformation metal material is ensured to flow, and meanwhile, the heat input is realized as low as possible, so that the obtained modified layer is ensured to be uniform and flat.
According to another specific embodiment of the application, the diameter of the shaft shoulder is 10-14 mm; preferably, the stirring head has a diameter of 12mm relative to the shoulder.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application comprises at least one group of clamping tools, wherein each group of clamping tools is respectively arranged at two sides of a needleless stirring head, and the distance between each group of clamping tools is 14-18 mm; preferably, the distance between each set of gripping tools is 16mm relative to a stirring head having a shoulder diameter of 12mm.
By adopting the scheme, the distance between each group of clamping tools is reduced as much as possible, so that the unstable welding process caused by the deformation of the high-entropy alloy sheet in the friction stir welding process is prevented, the high-entropy alloy modified layer material and the magnesium alloy base material are tightly attached, and the prepared modified layer has better compactness.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application comprises the following components in percentage by mass, wherein the magnesium alloy base material is AZ31B brand magnesium alloy: al:3.2%, zn:1.4%, mn:0.7%, si:0.07%, ca:0.04%, cu:0.01%, the balance Mg and unavoidable impurities.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application is characterized in that the needleless stirring head is made of tungsten-rhenium alloy.
By adopting the scheme, excessive abrasion of the stirring head in the processing process is avoided.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed in the embodiment of the application has the advantage that the high-entropy alloy sheet is AlCoCrFeNi 2.1 The composition comprises the following components in percentage by mass: 12.59% of Al, 17.24% of Co, 16.47% of Cr, 36.68% of Ni, and the balance of Fe and unavoidable impurities.
According to another specific embodiment of the application, the method for preparing the modified layer on the surface of the magnesium alloy disclosed by the embodiment of the application has the advantages that the shaft shoulder pressing amount of the needleless stirring head is 0.4-0.8 times of the thickness of the high-entropy alloy sheet; preferably, the shaft shoulder pressing amount is 0.6-0.8 times of the thickness of the high-entropy alloy sheet.
The application also provides a magnesium alloy, and the method for preparing the modified layer on the surface of the magnesium alloy is adopted to prepare the modified layer on the surface of the magnesium alloy.
By adopting the scheme, the comprehensive performance of the surface of the magnesium alloy can be obviously improved, the high-entropy alloy modified layer material and the magnesium alloy base material are tightly attached, and the prepared modified layer has good compactness; is flat and uniform.
The application has the beneficial effects that:
the application provides a method for preparing a modified layer on the surface of a magnesium alloy and the magnesium alloy with the surface modified layer obtained by the method. In addition, the magnesium alloy surface modification layer is prepared by using the high-entropy alloy sheet through a friction stir processing mode, so that the material flow in the processing process can be effectively controlled, and the thickness and uniformity of the modification layer are easier to control. Furthermore, the application adopts the needleless stirring head, and the technology of high rotation speed and high welding speed is matched to accelerate the preparation efficiency, simultaneously reduce the heat input, avoid the problem of increasing brittle intermetallic compounds, avoid the quality problem of the prepared modified layer, and ensure that the prepared modified layer is smoother and more uniform. In the preparation process, the thickness of the modified layer can be controlled by controlling the thickness of the high-entropy alloy sheet and matching with the shaft shoulder pressing amount of the stirring head.
The high-entropy alloy modified layer is prepared on the surface of the magnesium alloy by adopting a three-spiral groove-shaped needleless stirring head through a high-speed friction stir processing technology, so that the comprehensive performance of the surface of the magnesium alloy can be greatly improved. Compared with the magnesium alloy substrate, the self-corrosion potential of the prepared modified layer can be improved by 16.5%, the surface corrosion products are obviously reduced, the hardness value can be improved by 610% compared with the magnesium alloy substrate, and compared with AlCoCrFeNi 2.1 The high-entropy alloy can be lifted to 73.7%.
Drawings
FIG. 1 is a schematic diagram of multi-pass friction stir processing in a method for preparing a modified layer on a magnesium alloy surface provided by the application;
FIG. 2 is a schematic structural view of a triple helix groove-shaped needleless stirring head in the method for preparing a modified layer on the surface of the magnesium alloy;
FIGS. 3a-3c are photomicrographs of the interface between the modified layer and the substrate prepared in examples 1-3, respectively, of the present application;
FIGS. 3d-3f are SEM photographs of interfaces between the modified layers and the substrate prepared in examples 1-3, respectively;
FIG. 4 is a plot of the potentiodynamic polarization of the modified layers and substrates prepared according to examples 1-3 of the present application at different pressing amounts;
FIG. 5 shows hardness values of the modified layer, the magnesium alloy substrate, and the high-entropy alloy prepared in example 1 of the present application;
FIG. 6 is an SEM photograph obtained by observing the corrosion morphology of a magnesium alloy substrate;
FIG. 7 is an SEM photograph of the modified layer of example 1 of the present application obtained by observing the corrosion morphology.
Reference numerals:
1: a magnesium alloy substrate; 2: high entropy alloy sheet; 3: a stirring head; 31: a shaft shoulder; 32: a spiral groove.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present application more apparent, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
In order to improve the wear resistance and corrosion resistance of the magnesium alloy matrix, a coating needs to be prepared on the surface of the magnesium alloy. The application discloses a method for preparing a modified layer on the surface of magnesium alloy, wherein the surface modified layer is equivalent to a coating. The method comprises the following steps:
s1: and (5) polishing, cleaning and other pretreatment are carried out on the surface of the magnesium alloy substrate.
The surface of the magnesium alloy substrate can be polished by sand paper and the like, and specifically, the surface of the magnesium alloy can be polished by 400# sand paper, 800# sand paper, 1200# sand paper and 2000# sand paper in sequence; and then cleaning with alcohol, drying with cold air, and removing surface oxide films and impurities. Wherein, the length, width and thickness of the magnesium alloy base material are selected according to actual needs.
Further, the magnesium alloy is a conventional magnesium alloy in the art, for example, it may be AZ31B, AZ91D, ZK M, AZ31B, AZ31S, AZ31T, AZ40M, AZ a, or the like. In one embodiment of the application, the magnesium alloy substrate is AZ31B brand magnesium alloy, and comprises the following components in percentage by mass: 3.2% of Al, 1.4% of Zn, 0.7% of Mn, 0.07% of Si, 0.04% of Ca, 0.01% of Cu, and the balance of Mg and unavoidable impurities.
S1: preparing as-cast high-entropy alloy sheet with thickness of 0.2-1.5 mm.
The high-entropy alloy sheet is mainly used as a material of a modified layer on the surface of the magnesium alloy to increase the comprehensive performance of the surface of the magnesium alloy, so that the composition of the surface modified layer can be determined according to engineering requirements, and the high-entropy alloy such as AlCoCrFeNi, coCr Mo5, feMnCoCrSiCu, alCoCrFeNi2.1 and the like can be specifically selected. The high-entropy alloy sheet can be cast into cast ingots in a vacuum induction melting furnace; and then polishing, cleaning and other pretreatment are carried out on the as-cast high-entropy alloy sheet, specifically, 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 2000# abrasive paper can be sequentially adopted to polish the cut high-entropy alloy sheet so as to remove surface oxide films and impurities, and the bonding surface of the high-entropy alloy sheet and the magnesium alloy can be tightly bonded.
In one embodiment of the present application AlCoCrFeNi is selected 2.1 ，AlCoCrFeNi 2.1 The dual-phase high-entropy alloy is a dual-phase high-entropy alloy of a Face-Centered Cubic unit cell (Face Center Cubic/Face-Centered Cubic unit cell (FCC) and a body-Centered Cubic unit cell (Body Center Cubic, BCC), has excellent casting, corrosion resistance and forming properties of a eutectic alloy, has good strong plasticity matching and excellent high-temperature tensile strength at room temperature, is favorable for being coated on the surface of a magnesium alloy substrate through friction stir welding, can ensure that a surface modification layer is closely matched with the magnesium alloy substrate, and can effectively improve the wear resistance and corrosion resistance of the magnesium alloy; and AlCoCrFeNi 2.1 The price is relatively low, and the cost can be reduced. Further, alCoCrFeNi 2.1 The high-entropy alloy sheet comprises the following components in percentage by mass: 12.59% of Al, 17.24% of Co, 16.47% of Cr, 36.68% of Ni, and the balance of Fe and unavoidable impurities.
Further, the thickness of the high-entropy alloy sheet is flexibly adjusted according to the thickness of the surface modification layer prepared as required, if a surface modification layer with larger thickness is required, a thicker high-entropy alloy sheet can be adopted, and if a surface modification layer with smaller thickness is required, a thinner high-entropy alloy sheet can be adopted, and the thickness of the surface modification layer is controllable by matching with adjustment of the pressing amount, the rotating speed, the advancing speed and the like of the stirring head. The thickness of the high-entropy alloy sheet is 0.2 to 1.5mm, and specifically, the thickness of the high-entropy alloy sheet may be 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.8mm, 1mm, 1.2mm, 1.5mm, or the like. Preferably, the thickness of the high-entropy alloy sheet is 0.3 to 1mm, more preferably, the thickness of the high-entropy alloy sheet is 0.4 to 0.6mm, and still more preferably, the thickness of the high-entropy alloy sheet is 0.5mm. The high-entropy alloy sheet with the thickness of 0.5mm is adopted, so that the material flow in the processing process can be more effectively controlled, and the thickness and uniformity of the modified layer can be more easily controlled.
The length and width dimensions of the high-entropy alloy sheet are matched with the surface dimensions of the magnesium alloy substrate to be coated with the modified layer, so that the surface of the magnesium alloy substrate is uniformly coated with the modified layer.
S2: and tightly attaching one surface of the high-entropy alloy sheet to the surface of the magnesium alloy substrate, fixing the high-entropy alloy sheet to the friction stir welding machine by adopting a clamping tool of the friction stir welding machine, and enabling the other surface of the high-entropy alloy sheet to be positioned at one side close to the stirring head.
The surface of the magnesium alloy substrate subjected to polishing and cleaning is tightly attached to one surface of the high-entropy alloy sheet subjected to polishing and cleaning, and the attached magnesium alloy substrate and high-entropy alloy sheet are fixed on a workbench of the friction stir welding machine by using a clamping tool of the friction stir welding machine, so that the magnesium alloy substrate and the high-entropy alloy sheet are prevented from being displaced together or relatively displaced in the processing process, and the stable welding process is ensured. And the other side of the high-entropy alloy sheet is positioned above the friction stir welding machine, namely, near one side of the stirring head.
S3: the stirring head is a needleless stirring head, the needleless stirring head is adopted to carry out multi-pass stirring friction processing along the surface of the fixed high-entropy alloy sheet, so that the high-entropy alloy sheet is connected with the magnesium alloy base material, the shaft shoulder pressing amount of the needleless stirring head is smaller than the thickness of the high-entropy alloy sheet, the rotating speed of the needleless stirring head is 5000-10000 rpm, and the advancing speed is 500-1000 mm/min.
Specifically, in order to make the prepared modified layer more compact and uniform and reduce the warp deformation in the processing process, firstly, in the process of fixing a workpiece, as shown in fig. 1, a magnesium alloy base material 1 and a high-entropy alloy sheet 2 are tightly attached, a needleless stirring head 3 carries out single-pass friction stir welding along the same direction (F1 direction in the figure) from one side to the opposite side, and the F2 direction in the figure is the rotation direction of the stirring head 3; more specifically, the first weld may be started at the center, and then the second weld may be completed at a position overlapping the first weld by a certain distance (for example, about 1 mm) along the same rotation direction and processing direction, and multiple passes may be sequentially performed until the weld fills the entire magnesium alloy surface layer, wherein the imprint of the completed multiple pass friction stir processing on the left side of the high-entropy alloy sheet 2 is shown in fig. 1.
The traditional friction stir processing efficiency is lower, and in order to improve the processing efficiency, the friction stir welding is carried out at high rotating speed and high welding speed, but only the rotating speed is singly improved, so that the heat input is increased, and the brittle intermetallic compound is increased; to prevent this problem, the present application selects a needleless stirring head to reduce heat input; the needleless stirring head is adopted to rotate at a high speed, so that the heat input is reduced, and meanwhile, the preparation efficiency is improved; and the modified layer prepared by adopting the needleless stirring head is smoother and more uniform. Because of the high hardness of the high-entropy alloy, in one embodiment of the application, the needleless stirring head is made of tungsten-rhenium alloy, so that excessive abrasion of the stirring head in the processing process is avoided.
The shaft shoulder pressing amount of the stirring head is smaller than the thickness of the high-entropy alloy sheet, so that plastic deformation high-entropy alloy around the stirring head can be extruded out of a welding seam area during stirring, and the high-entropy alloy at the lower part of the stirring head is tightly attached to a magnesium alloy matrix through extrusion and thermal action of the stirring head, so that the problem of poor compactness of a prepared modified layer is avoided. When the stirring head rotates at a high speed, part of metal which is subjected to plastic deformation is extruded out of a welding seam area, and when a larger pressing amount is adopted, more metal is extruded out, so that the thickness change of the high-entropy alloy sheet is larger, and the thickness of a finally formed modified layer is thinner; when a smaller amount of pressing is used, less metal is extruded, so that the thickness variation of the high-entropy alloy sheet is smaller, and the thickness of the finally formed modified layer is thicker. Therefore, the thickness of the modified layer can be controlled by controlling the thickness of the high-entropy alloy sheet and matching with the pressing amount of the stirring head. In one embodiment of the application, the shaft shoulder pressing amount of the needleless stirring head is 0.4-0.8 times of the thickness of the high-entropy alloy sheet; preferably, the shaft shoulder pressing amount is 0.6-0.8 times of the thickness of the high-entropy alloy sheet; taking a high-entropy alloy sheet with a thickness of 0.5mm as an example, the shoulder pressing amount is 0.2-0.4 mm, preferably 0.3-0.4 mm. The rotational speed and the advancing speed of the stirring head are determined according to the high-entropy alloy sheet material, thickness and the like, and the rotational speed of the specific needleless stirring head can be 5000rpm, 600rpm, 7000rpm, 8000rpm, 9000rpm, 10000rpm and the like, and the advancing speed can be 500mm/min, 600mm/min, 700mm/min, 800mm/min, 900mm/min, 1000mm/min and the like.
It should be noted that, in order to prevent that the laminating of high entropy alloy piece and magnesium alloy substrate is not inseparable, friction stir welding machine includes at least a set of centre gripping instrument, and every group centre gripping instrument sets up respectively in needleless stirring head's both sides, guarantees that the high entropy alloy piece and the magnesium alloy substrate of the processing position of needs closely laminate and do not take place relative displacement in the friction stir process. And, in order to prevent the welding process from being unstable due to the deformation of the high-entropy alloy sheet during friction stir welding, the distance between each group of clamping tools is reduced as much as possible. The distance between each group of clamping tools is determined according to the diameter of the shaft shoulder of the stirring head, and the smaller the distance is, the closer the distance is, so that the high-entropy alloy modified layer material and the magnesium alloy base material are attached, and the compactness of the prepared modified layer is better.
In one embodiment of the application, the diameter of the shaft shoulder of the needleless stirring head is 10-14 mm; preferably, the shoulder diameter is 12mm. Further, in one embodiment of the present application, the distance between each set of gripping tools is 14-18 mm; preferably, the distance between each set of gripping tools is 16mm relative to a stirring head having a shoulder diameter of 12mm. Wherein, the technological parameters for preparing the surface modified layer of the magnesium alloy substrate with the thickness of 5mm are preferably as follows: the diameter of the shaft shoulder is 12mm, the pressing amount of the shaft shoulder is 0.3mm, the rotating speed of the stirring head is 8000rpm, and the translation speed of the stirring head is 600mm/min.
According to one embodiment of the present application, as shown in fig. 2, the surface of the shoulder 31 of the pin-less stirring head 3 is uniformly provided with a plurality of spiral grooves 32 extending from the edge toward the center.
The application selects the needleless stirring head, but in the high-speed stirring process of the needleless stirring head, part of plastic deformation metal is screwed out of a welding line, so that the flowing capability of the plastic deformation metal is weakened, and the risks of holes, accumulation and poor compactness are caused. Therefore, the surface of the shaft shoulder of the needleless stirring head is provided with the spiral groove, so that the heat input is reduced, the material flow is promoted, the formation of holes and compounds is reduced, and the compactness of a modified layer is enhanced. Besides the needleless stirring head with the spiral groove, other needleless stirring heads with other designs can be selected, so long as the material flow can be promoted without improving the heat input. In addition, the spiral groove is designed to extend from the edge to the center and has the function of feeding back, so that the metal at the edge of the stirring head is received at the center of the welding seam, the escape of plastic deformation metal materials in the high-speed stirring process can be effectively reduced, and the problem of uneven material mixing caused by needleless is avoided.
According to one embodiment of the present application, as shown in FIG. 2, there are 3 spiral grooves 32, forming a triple spiral groove needleless stirring head. The 3 spiral grooves 32 are uniformly arranged on the shaft shoulder 31, one ends extending towards the center are not connected, and a blank is formed in the center. The three spiral groove-shaped needleless stirring head shaft shoulders are adopted, except for three spiral grooves with the same shape, the interfaces of the other shaft shoulders are kept flat, the plastic deformation metal material flow is promoted, and meanwhile, the heat input is realized as low as possible, so that the obtained modified layer is uniform and flat.
According to the application, friction stir welding is adopted, and the material is locally plasticized through friction heat and plastic deformation heat, so that the high-entropy alloy sheet forms a modified layer on the magnesium alloy substrate, and the processing defect caused by adopting a thermoforming mode is avoided. Further, in the process of preparing the modified layer by friction stir processing, if a powder modified layer prefabricating method is used, the modified layer powder is required to be sprayed on the surface of the magnesium alloy substrate in a cold spraying mode, then friction stir welding is performed, and the thickness of the modified layer cannot be controlled due to the limitation of the cold spraying mode, and the modified layer with large thickness cannot be prepared. Or prefabricating the powdery material on the surface of the matrix by means of punching, slotting and the like, and then carrying out surface modification by friction stir processing, so that the processing technology is complicated, the agglomeration phenomenon of reinforced particles is easy to occur, and the material performance is influenced. Therefore, the magnesium alloy surface modified layer is prepared by using the high-entropy alloy sheet through a friction stir processing mode, so that the material flow in the processing process can be effectively controlled, and the thickness and uniformity of the modified layer are easier to control.
The needleless stirring head is adopted, the preparation efficiency is improved by matching with a high-rotation-speed and high-welding-speed process, the heat input is reduced, the problem of increasing brittle intermetallic compounds is avoided, the quality problem of a prepared modified layer is avoided, and the prepared modified layer is smoother and more uniform. Further, in the preparation process, the thickness of the modified layer can be controlled by controlling the thickness of the high-entropy alloy sheet and matching with the shaft shoulder pressing amount of the stirring head. The three-spiral groove-shaped needleless stirring head is adopted to prepare the high-entropy alloy modified layer on the surface of the magnesium alloy by a high-speed friction stir processing technology, so that the comprehensive performance of the surface of the magnesium alloy can be greatly improved.
The method for preparing the modified layer on the surface of the magnesium alloy of the present application is described in further detail below with specific examples. Wherein the magnesium alloy base material is AZ31B brand magnesium alloy, and the high-entropy alloy sheet is AlCoCrFeNi 2.1 The needleless stirring head is a three-spiral groove-shaped needleless stirring head, and the diameter of the shaft shoulder is 12mm.
Example 1
The preparation method of the magnesium alloy surface modification layer comprises the following steps:
s1: and (3) cutting, polishing, cleaning and other pretreatment are carried out on the surface of the magnesium alloy substrate.
For the test, a wire cutting machine is adopted to cut the magnesium alloy substrate into blocks of 100mm multiplied by 5mm, 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 2000# abrasive paper are adopted to polish the cut magnesium alloy blocks in sequence, so that surface oxide films and impurities are removed, and the magnesium alloy blocks are cleaned by alcohol and dried by cold air.
S1: preparing an as-cast high-entropy alloy sheet, and performing pretreatment such as cutting, polishing, cleaning and the like on the as-cast high-entropy alloy sheet.
Cutting the high-entropy alloy into sheets with the thickness of 100mm multiplied by 0.5mm by adopting a wire cutting machine, polishing the cut high-entropy alloy sheets by adopting 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 2000# abrasive paper in sequence, removing surface oxide films and impurities, cleaning by using alcohol, and drying by using cold air.
S2: and tightly attaching one surface of the high-entropy alloy sheet to the surface of the magnesium alloy substrate, fixing the high-entropy alloy sheet to the friction stir welding machine by adopting a clamping tool of the friction stir welding machine, and enabling the other surface of the high-entropy alloy sheet to be positioned at one side close to the stirring head. And tightly attaching the pretreated high-entropy alloy sheet and the magnesium alloy square block, and fixing the high-entropy alloy sheet and the magnesium alloy square block by a clamping tool of a friction stir welding machine. Each group of clamping tools are respectively arranged at two sides of the needleless stirring head, and the distance between each group of clamping tools is 16mm.
S3: and (3) adopting a gantry type friction stir welding machine, and carrying out multi-pass friction stir processing along the surface of the fixed high-entropy alloy sheet by using a needleless stirring head. The stirring head is not inclined, the shaft shoulder pressing amount is 0.30mm, the rotating speed of the stirring head is 8000rpm, and the translation speed of the stirring head is 600mm/min.
After the processing is completed, a magnesium alloy having a surface-modified layer is obtained.
Example 2
A method for preparing a magnesium alloy surface modification layer is provided, and the method for preparing the magnesium alloy surface modification layer is provided in reference to the embodiment 1, except that in the step S3, the shaft shoulder pressing amount is 0.35mm.
Example 3
A method for preparing a magnesium alloy surface modification layer is provided, and the method for preparing the magnesium alloy surface modification layer is provided in reference to the embodiment 1, except that in the step S3, the shaft shoulder pressing amount is 0.40mm.
The samples prepared in the three examples above were subjected to tissue analysis and performance characterization:
(1) Comparison analysis of modified layer with substrate interface mirror and SEM (scanning electron microscope) under different shaft shoulder pressing amounts
Fig. 3a-3c show respective photographs of the interface between the modified layer prepared in examples 1-3 and the substrate, with respect to the press-down amounts d=0.30 mm, d=0.35 mm, and d=0.40 mm, and fig. 3d-3f show respective SEM photographs of the interface between the modified layer prepared in examples 1-3 and the substrate, with respect to the press-down amounts d=0.30 mm, d=0.35 mm, and d=0.40 mm. From the photograph, it can be seen that as the penetration depth gradually increases, the thickness of the modified layer gradually decreases from 0.237mm to 0.130mm, and the quality of the modified layer gradually deteriorates. At the pressing amount d=0.40 mm, micropores and cracks appear on the surface of the modified layer.
(2) The corrosion resistance of the modified layer prepared under different shaft shoulder pressing amounts is compared
Cutting an AZ31B magnesium alloy substrate and the magnesium alloy with the surface modification layer obtained in the embodiment 1-3 into corrosion samples of 20mm multiplied by 15mm multiplied by 5.5mm by a wire cutting machine, respectively polishing the corrosion samples by sand paper, connecting the samples with a metal conductor after surface polishing to expose the surface to be tested, sealing all the other surfaces by using a resin insulating adhesive, taking 3.5wt% sodium chloride solution as a corrosive liquid, taking the samples, a platinum sheet and a saturated hot wire electrode as working electrodes, electrodes and reference electrodes respectively, and extracting corrosion potential data in a special electrochemical workstation to obtain a potentiodynamic polarization curve; and obtaining the self-corrosion potentials of the different corrosion samples from the electrochemical workstation.
FIG. 4 shows the potentiodynamic polarization curves of the modified layers and substrates prepared in examples 1-3 at different amounts of pressing, and Table 1 shows the self-etching potentials of the modified layers and substrates prepared at different amounts of pressing. From the data in the table, it can be derived: the corrosion potential of the modified layer is increased compared to the magnesium alloy substrate. When the shoulder pressing amount of the stirring head is increased from d=0.30 mm to d=0.40 mm, the corrosion potential gradually decreases, which indicates that the corrosion resistance of the modified layer decreases with the increase of the shoulder pressing amount, which may be caused by the deterioration of the forming quality of the modified layer prepared with the pressing amount d=0.40 mm. Compared with a magnesium alloy substrate, the self-corrosion potential of the prepared modified layer is improved by 16.5% when the pressing amount d=0.30 mm, which shows that the preparation of the high-entropy alloy modified layer on the surface of the magnesium alloy can obviously improve the corrosion resistance of the surface of the magnesium alloy.
TABLE 1 self-etching potential of modified layers and substrates prepared at different pressing amounts
(3) Microhardness contrast under different materials and conditions
Cutting AZ31B magnesium alloy substrate into 20mm×20mm×5.5mm samples by using a wire cutting machine, and performing AlCoCrFeNi 2.1 The high-entropy alloy was cut into samples of 20mm×20mm×0.5mm, and the magnesium alloy with the surface-modified layer obtained in example 1 was cut into samples of 20mm×20mm in length and width; all samples were sanded separately, surface polished, and placed on a durometer sample stand for hardness testing, where a maximum load force of 200g was set, hold time of 15s, and an average of 6 points was taken as the final measurement, each point spaced 0.5mm apart.
FIG. 5 shows a magnesium alloy with a surface modified layer, AZ31B magnesium alloy substrate and AlCoCrFeNi according to example 1 2.1 Hard of high entropy alloysThe degree value can be seen from the graph: AZ31B magnesium alloy substrate and AlCoCrFeNi 2.1 The hardness of the high-entropy alloy (HEA) and the modified layer (Coating) were 67HV, 274HV and 476HV, respectively, indicating that the modified layer prepared by friction stir processing has a 610% increase in hardness value compared to the magnesium alloy substrate (caused by the combination of excellent comprehensive properties of the high-entropy alloy and grain refinement during friction stir processing), compared to AlCoCrFeNi 2.1 The high-entropy alloy is improved by 73.7%, which shows that the preparation of the high-entropy alloy modified layer on the surface of the magnesium alloy can obviously improve the hardness of the surface of the magnesium alloy.
(4) Comparison of corrosion morphology of magnesium alloy substrate and high-entropy alloy modified layer
The sample corrosion morphology was subjected to microscopic morphology observation analysis by SEM using the AZ31B magnesium alloy corrosion sample without the modified layer as a comparative example, and the magnesium alloy (shoulder pressing amount d=0.30 mm) corrosion sample with the modified layer obtained in example 1.
Fig. 6 shows SEM photographs obtained by observing the corrosion morphology of the magnesium alloy substrate. As can be seen from fig. 6: the etched surface of the magnesium alloy substrate forms a plurality of corrosion cracks and corrosion holes, which are probably formed by flocculent porous Mg (OH) 2 Phase exfoliation and local enrichment of beta-Mg 17 Al 12 Intergranular galvanic corrosion of the phases. Fig. 7 shows SEM photographs obtained by observing the corrosion morphology of the modified layer of example 1. As can be seen from fig. 7: when the pressing amount d=0.30 mm of the shaft shoulder of the stirring head, the surface of the prepared sample after the corrosion of the modified layer is smoother, and only a very small amount of granular corrosion products appear. As can be seen from the surface morphology comparison of the modified layer and the base material after corrosion, the modified layer has better corrosion resistance than the base material, and the high-entropy alloy modified layer prepared by friction stir processing has obvious effect of improving the corrosion resistance of the AZ31B magnesium alloy surface.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. As used herein, the singular forms "a," "an," and "the ()" are intended to include the plural forms as well, unless the context clearly indicates otherwise. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The expression "at least one (seed)" when before or after the list of elements modifies the entire list of elements without modifying individual elements of the list.
Further, the terms "comprises" or "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, regions, integers, steps, operations, elements, components, and/or groups thereof.
As used herein, "about" or "approximately" includes the values described and means, for example, within the acceptable range of deviation for a particular value as determined by one of ordinary skill in the art in view of the measurements in question and the errors associated with the measurement of the particular quantity (i.e., limitations of the measurement system). All ratios of components refer to weight percent (wt%) unless otherwise specified; unless otherwise indicated, all ranges of parameters disclosed include the endpoints and all values therebetween.
It should be noted that in this specification, like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
While the application has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing is a further detailed description of the application with reference to specific embodiments, and it is not intended to limit the practice of the application to those descriptions. Various changes in form and detail may be made therein by those skilled in the art, including a few simple inferences or alternatives, without departing from the spirit and scope of the present application.
Claims (10)
1. A method for preparing a modified layer on the surface of a magnesium alloy, which is characterized by comprising the following steps:
s1: preparing an as-cast high-entropy alloy sheet having a thicknessThe degree is 0.2-1.5 mm; the high-entropy alloy in the high-entropy alloy sheet is AlCoCrFeNi, coCr Mo5 and FeMnCoCrSiCu, alCoCrFeNi 2.1 One of the following;
s2: tightly attaching one surface of the high-entropy alloy sheet and the surface of the magnesium alloy substrate, and fixing the high-entropy alloy sheet and the surface of the magnesium alloy substrate on a friction stir welding machine by adopting a clamping tool of the friction stir welding machine;
s3: the stirring head is a needleless stirring head, and the needleless stirring head is adopted to carry out multi-pass friction stir processing along the surface of the high-entropy alloy sheet so as to connect the high-entropy alloy sheet and the magnesium alloy substrate; the shaft shoulder pressing amount of the needleless stirring head is smaller than the thickness of the high-entropy alloy sheet, the rotating speed of the needleless stirring head is 5000-10000 rpm, and the advancing speed is 500-1000 mm/min.
2. The method for preparing a modified layer on a magnesium alloy surface according to claim 1, wherein the surface of the shoulder of the needleless stirring head is uniformly provided with a plurality of spiral grooves extending from the edge to the center.
3. The method for preparing a modified layer on a magnesium alloy surface according to claim 2, wherein the number of the spiral grooves is 3.
4. The method for preparing a modified layer on a magnesium alloy surface according to claim 3, wherein the diameter of the shoulder is 10-14 mm.
5. The method for preparing a modified layer on a magnesium alloy surface according to claim 4, wherein the friction stir welding machine comprises at least one group of clamping tools, each group of clamping tools is respectively arranged at two sides of the needleless stirring head, and the distance between each group of clamping tools is 14-18 mm.
6. The method for preparing a modified layer on a magnesium alloy surface according to claim 1, wherein the magnesium alloy substrate comprises the following components in mass fraction:
al:3.2%, zn:1.4%, mn:0.7%, si:0.07%, ca:0.04%, cu:0.01%, the balance Mg and unavoidable impurities.
7. The method for preparing a modified layer on a magnesium alloy surface according to claim 1, wherein the needleless stirring head is made of tungsten-rhenium alloy.
8. The method for preparing a modified layer on a magnesium alloy surface according to claim 7, wherein the high-entropy alloy sheet is composed of the following components in mass fraction:
12.59% of Al, 17.24% of Co, 16.47% of Cr, 36.68% of Ni, and the balance of Fe and unavoidable impurities.
9. The method for preparing a modified layer on a magnesium alloy surface according to any one of claims 1 to 8, wherein in step S3, the shoulder pressing amount of the needleless stirring head is 0.4 to 0.8 times the thickness of the high-entropy alloy sheet.
10. A magnesium alloy characterized in that a modified layer is produced on the surface of the magnesium alloy by the method for producing a modified layer on the surface of the magnesium alloy according to any one of claims 1 to 9.
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