CN110666179B - Graphene aluminum-based composite powder for laser deposition manufacturing, and preparation method and application thereof - Google Patents

Graphene aluminum-based composite powder for laser deposition manufacturing, and preparation method and application thereof Download PDF

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CN110666179B
CN110666179B CN201911095343.XA CN201911095343A CN110666179B CN 110666179 B CN110666179 B CN 110666179B CN 201911095343 A CN201911095343 A CN 201911095343A CN 110666179 B CN110666179 B CN 110666179B
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graphene
aluminum
based composite
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孟庆实
王天琦
杨光
李鹏旭
张硕程
王维
任宇航
李长富
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Shenyang Aerospace University
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    • B22F9/00—Making metallic powder or suspensions thereof
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    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract

A graphene aluminum-based composite powder for laser deposition manufacturing and a preparation method and application thereof belong to the field of metal-based composite materials. In the graphene aluminum-based composite powder for laser deposition manufacturing, a few-layer graphene nanosheet is prepared by a thermal expansion-ultrasonic combination method according to the mass ratio: aluminum matrix powder =1 (666-1999), and its sphericity is 0.85-0.9. The few-layer graphene nanosheets are prepared by adopting a thermal expansion ultrasonic combination method, and are uniformly dispersed on the surface of aluminum powder particles under a scanning electron microscope by adopting wet ball milling. The graphene aluminum-based composite material is formed by adopting a laser deposition process, so that the obtained graphene aluminum-based composite material has the advantages of good workpiece interface combination, strong compactness, no defect of air holes and improved strength and toughness.

Description

Graphene aluminum-based composite powder for laser deposition manufacturing, and preparation method and application thereof
Technical Field
The invention relates to the field of metal matrix composite materials, in particular to graphene aluminum matrix composite powder for laser deposition manufacturing and a preparation method and application thereof.
Background
The additive manufacturing is commonly called 3D printing, can rapidly manufacture structural tissues of various forms, can manufacture any complex structure by the additive manufacturing technology as long as a model is provided, also omits the machining treatment after molding, obviously shortens the development cycle of products, has the advantages of low manufacturing cost and short cycle, and becomes one of the most concerned technologies in the manufacturing industry. And materials besides software, devices and the like influence the development of the additive manufacturing technology. The material is an important material basis for the development of additive manufacturing technology, and the performance of the material determines whether additive manufacturing can be applied more widely.
In the manufacturing industry, aluminum alloys have excellent properties of low density, high strength and good ductility, and are widely used in the fields of aerospace and the like. But two problems still need to be solved as additive manufacturing materials: firstly, the method comprises the following steps: the aluminum alloy is used as a structural material, the improvement of the strength of the aluminum alloy is a hot problem in the existing research field, and the methods for regulating and controlling the main components and adjusting the heat treatment and the process are not developed in a breakthrough way. Secondly, the method comprises the following steps: for a Laser Deposition Manufacturing (LDM) technology developed in an additive Manufacturing process, if an aluminum alloy is selected as a material, most of Laser is reflected due to low Laser absorption rate of the aluminum alloy, so that the processing is very difficult.
In the prior art, a patent 201611033221.4 discloses a graphene aluminum-based composite material and a preparation method thereof, the graphene aluminum-based composite material prepared by the method is used for traditional material reduction or equal material manufacturing modes, the manufacturing modes have limitations, a complex structure is difficult to form, the forming quality is unstable, and the prepared composite material has more defects of pores, cracks and the like, so the compactness is poor, the layer-to-layer combination is poor, and the performance parameters are directly lower. Patent 201710496369.x discloses a preparation method of graphene aluminum-based composite powder for selective laser melting forming, the prepared graphene aluminum-based composite powder is used in a selective laser melting forming mode in an additive manufacturing technology, selective laser melting forming is that laser is melted and formed at a position required by a model after powder is laid on each layer, and therefore some powder materials are wasted on each layer, but for composite materials, the process for preparing the composite powder is complex, the cost is high, and the preparation period of the composite powder used for forming is long. In addition, the time for printing the test piece by selective laser melting molding is longer, and is 3-5 times of that of the LDM compared with the test piece with the same size.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides graphene aluminum-based composite powder for laser deposition manufacturing and a preparation method and application thereof. The added graphene has a large specific surface area and good strength and Young modulus, so that the graphene becomes an optimal filling material in the aluminum matrix composite. The graphene is added into the aluminum matrix, so that the strength and the hardness of the aluminum matrix can be obviously improved, the high ductility of the aluminum matrix is kept, and the thermal conductivity of the obtained composite material is also obviously improved.
The graphene is added into the aluminum alloy, so that the absorption rate of the aluminum-based powder to laser can be enhanced, and the graphene is uniformly coated on the surface of the aluminum powder as far as possible. However, graphene is easily agglomerated and has poor dispersibility in aluminum matrix powder. Additive manufacturing requires that the powder be as spherical as possible and ball milling of prior art processes can destroy the sphericity of the powder. And because the method is applied to the laser deposition manufacturing process, pores are easily generated, and the performance of a processed sample is influenced.
The preparation method of the invention realizes that the graphene is uniformly dispersed in the aluminum matrix powder, the prepared graphene aluminum matrix composite powder is spherical or nearly spherical, the sphericity is 0.85-0.9, the graphene aluminum matrix composite powder is used for laser deposition manufacturing, and the obtained graphene aluminum matrix composite material has good workpiece interface combination, strong compactness and no defect of pores.
In order to achieve the purpose, the invention adopts the following scheme:
the invention relates to graphene aluminum-based composite powder for laser deposition manufacturing, which comprises a few-layer graphene nanosheet prepared by a thermal expansion-ultrasonic combination method and aluminum matrix powder, wherein the few-layer graphene nanosheet prepared by the thermal expansion-ultrasonic combination method comprises the following components in percentage by mass: aluminum matrix powder =1 (666-1999), it can be observed under a scanning electron microscope that few graphene nanosheets are uniformly dispersed on the surface of aluminum powder particles, and the sphericity of the prepared graphene aluminum matrix composite powder for laser deposition manufacturing is 0.85-0.9.
The preparation method of the graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combination method
The intercalation expandable graphite raw material is kept at 500-800 ℃ for 1-5 min, taken out and air-cooled to room temperature to obtain expanded graphene sheets;
mixing the expanded graphene sheets with absolute ethyl alcohol, and carrying out ultrasonic treatment for 2-5 h to obtain few-layer graphene nanosheets; according to the solid-liquid ratio, the expanded graphene sheet: absolute ethanol = (0.1-0.3) g: (100-200) mL.
Step 2: wet ball milling
Mixing the millimeter-scale ball grinding ball, the aluminum matrix powder and the few-layer graphene nanosheets in proportion after impurity removal to obtain a mixture; wherein, according to the mass ratio, millimeter level ball grinding ball: (aluminum matrix powder + few-layer graphene nanosheets) = (3-5): 1, aluminum matrix powder: few-layer graphene nanoplatelets = (666-1999): 1;
placing the mixture into a ball milling tank, adding absolute ethyl alcohol into the ball milling tank for wet ball milling, and drying after ball milling to obtain aluminum powder wrapping few-layer graphene nanosheets, namely graphene aluminum-based composite powder; according to the solid-liquid ratio, the mixture: absolute ethanol = (500-800) g: (120-200) mL.
In the step 1, the ultrasonic frequency adopted by the ultrasonic is 38-42KHz.
In the step 2, the aluminum matrix powder is preferably a cast aluminum alloy or a wrought aluminum alloy, specifically one of ZL114A, ZL101A, and 6061.
In the step 2, the millimeter-sized ball is a 2-5mm ball grinding ball, and the ball grinding ball is one of a stainless steel ball grinding ball, a zirconia ball grinding ball and an agate ball grinding ball.
In the step 2, the wet ball milling process comprises the following steps: the ball milling tank is vacuumized until the vacuum degree reaches 4.0 multiplied by 10 -2 Pa, putting the ball milling tank into a ball mill, wherein the ball milling adopts interval ball milling, the total ball milling time is 12-18 h, and each timeStopping ball milling for 10-15min after 30min, wherein the ball milling speed is 220-280 r/min.
The application of the graphene aluminum-based composite powder for laser deposition manufacturing is to prepare a graphene aluminum-based composite material workpiece by using the graphene aluminum-based composite powder as a raw material for laser deposition manufacturing.
The application of the graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
the graphene aluminum-based composite powder for laser deposition manufacturing is molded by a laser deposition process to obtain a graphene aluminum-based composite material workpiece, the laser power is 1600-2400W, preferably 1800-2100W, the scanning speed is 3-10mm/s, preferably 4-6mm/s, the lap joint rate is 45-50%, and the powder feeding amount is 0.5-0.8r/min.
Compared with an aluminum base parent material, the tensile strength of the prepared graphene aluminum base composite material workpiece is enhanced by 47.34% -61%, the maximum tensile strength of the graphene aluminum base composite material workpiece can reach 240.49MPa, the maximum tensile strength of the graphene aluminum base composite material workpiece is enhanced by 60.65% compared with a pure ZL114A (149.7 MPa) test piece prepared by the same process, the elongation at break of the graphene aluminum base composite material workpiece is enhanced by 102.1% -216%, the maximum elongation at break of the graphene aluminum base composite material workpiece can reach 9.06%, and the elongation at break of the graphene aluminum base composite material workpiece is enhanced by 215.68% compared with a pure ZL114A (2.87%) test piece prepared by the same process.
The invention relates to graphene aluminum-based composite powder for laser deposition manufacturing and a preparation method and application thereof, and has the beneficial effects that:
1. according to the graphene aluminum-based composite powder for laser deposition manufacturing, after the graphene is added, graphene crystal grains grow in the laser deposition manufacturing process, and the crystal grain refining effect is achieved. A small amount of aluminum carbide generated by slight interface reaction of graphene and aluminum powder increases the wettability of the interface, so that the interface is better and more compact in combination, and the performance is improved.
2. When the graphene aluminum-based composite powder for laser deposition manufacturing is prepared, the agglomeration problem in the graphene ball milling process can be avoided through a wet ball milling mode, and the graphene can be uniformly wrapped on the surfaces of aluminum powder particles after the ball milling time, the rotation speed, the ball-material ratio and other parameters are optimized.
3. The laser deposition manufacturing can realize the processing of a complex structure, and a composite material test block with excellent quality can be formed under optimized technological parameters. Compared with other forming modes such as casting and the like, the performance of the sample is obviously improved, and compared with selective laser melting of selective laser melting forming, the laser deposition manufacturing of the invention adopts synchronous powder feeding, so that the prepared composite powder can be maximally utilized and deposited in the sample, and the prepared graphene aluminum-based composite material workpiece can achieve the toughening effect while being reinforced, and the toughness is not reduced due to the strength improvement in the prior art.
Drawings
FIG. 1: an SEM image of the graphene aluminum-based composite powder for laser deposition manufacturing prepared in embodiment 1 of the present invention;
FIG. 2: the invention discloses a structural schematic diagram of laser deposition manufacturing equipment;
in the figure, 1 is a laser, 2 is a powder feeder, 3 is an argon protection box, 3-1 is a workbench, 3-2 is a base material, 3-3 is a deposition layer, 3-4 is a molten pool, 3-5 is graphene aluminum-based composite powder for laser deposition manufacturing, 3-6 is a laser head, and 3-7 is a coaxial powder feeding head.
FIG. 3: and manufacturing a formed graphene aluminum-based composite material workpiece by laser deposition.
FIG. 4: and comparing the apparent appearances of the formed graphene aluminum-based composite workpiece manufactured by laser deposition and the cast formed graphene aluminum-based composite workpiece.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the intercalated expandable graphite starting material used was 1395 model expandable graphite starting material available from the United states.
In the following embodiment, the adopted laser deposition manufacturing equipment is an LDM-800 type LDM developed by Shenhang-Yu light combination, and comprises a laser 1, a powder feeder 2, an argon protection box 3 and a computer, wherein a substrate 3-2 is arranged above a workbench 3-1 in the argon protection box 3, coaxial powder feeding heads 3-7 are circumferentially arranged on the laser heads 3-6, nozzle openings of the coaxial powder feeding heads 3-7 are vertically arranged above the substrate 3-2, the workbench 3-1, the laser heads 3-6 and the coaxial powder feeding heads 3-7 are all arranged in the argon protection box 3, laser emitted by the laser 1 is transmitted to the laser heads 3-6 through optical fibers, the powder feeder 2 blows graphene composite powder 3-5 for laser deposition manufacturing to the coaxial powder feeding heads through powder pipes, the computer is connected with the coaxial powder feeding heads, the powder feeder and the laser, and the structural schematic diagram of the laser deposition manufacturing equipment is 2.
In the following examples, the laser used is a 6KW fiber laser from IPG, germany
Example 1
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combination method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 3min at 600 ℃, taking out and cooling to obtain the expanded graphene sheet.
And (3) putting 0.15g of the expanded graphene sheet into a beaker, adding 150mL of absolute ethyl alcohol, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 2 hours to obtain the few-layer graphene nanosheet.
And 2, step: wet ball milling
Before ball milling, 2-5mm ball milling balls are placed into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, and each time is 5-10 minutes, so that 2-5mm ball milling balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank by absolute ethyl alcohol, and performing ball milling on the ball milling tank by 2-5mm in mass ratio: (cast aluminum powder ZL114A + few-layer graphene nanosheets) =5:1, cast aluminum powder ZL114A: few-layer graphene nanoplatelets =666:1;
putting graphene, cast aluminum powder ZL114A and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600:160 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 Pa, putting the ball milling tank into a ball mill, milling for 12h (stopping for 15min every 30 min), and adjustingAnd (3) performing ball milling at a rotation speed of 240r/min, and drying after ball milling to obtain aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The SEM image of the prepared graphene aluminum-based composite powder for laser deposition fabrication is shown in fig. 1, and the sphericity thereof is 0.89.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared by the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece, and the method comprises the following steps:
step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeder 2, the power of a 6KW semiconductor laser 1 and the scanning speed of a coaxial powder feeding head 3-7 are set through a computer system of a computer, a molten pool 3-4 is formed at a nozzle opening of the coaxial powder feeding head, a deposition layer 3-3 is formed by layer-by-layer deposition, the laser power is 1900W, the scanning speed is 5mm/s, the lap joint rate is 50%, and the powder feeding amount is 0.6r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared, and a schematic view thereof is shown in FIG. 3.
Step II: and (4) performance testing:
according to the requirement of the size of the stretching plate in GB/T228.1-2010 metal material stretching test standard, the stretching plate is taken from a test block for stretching test, the average value of the tensile strength is 221.96MPa, the average value of the elongation at break is 6.1 percent, and the result shows that the tensile strength and the elongation at break are both obviously improved by comparing with the pure ZL114A tensile strength of 149.7MPa and the elongation at break of 2.87 percent.
Example 2
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combined method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 5min at 500 ℃, taking out and cooling to obtain the expanded graphene sheet.
And (3) putting 0.3g of the expanded graphene sheet into a beaker, adding 200mL of absolute ethyl alcohol, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 5 hours to obtain the few-layer graphene nanosheet.
Step 2: wet ball milling
Before ball milling, 2-5mm ball milling balls are placed into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, and each time is 5-10 minutes, so that 2-5mm ball milling balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank by absolute ethyl alcohol, and performing ball milling on the ball milling tank by 2-5mm in mass ratio: (cast aluminum powder ZL114A + few-layer graphene nanosheets) =3:1, cast aluminum powder ZL114A: few-layer graphene nanoplatelets =1999:1;
putting graphene, cast aluminum powder ZL114A and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600:160 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 Pa, putting the ball milling tank into a ball mill, performing ball milling for 18 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 280/min, and drying after ball milling to obtain aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The sphericity of the prepared graphene aluminum-based composite powder for laser deposition manufacturing is 0.85.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared by the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece, and the method comprises the following steps:
step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeding barrel, the power of a 6KW semiconductor laser and the scanning speed of a coaxial powder feeding head are set through a computer system of a computer, and the laser power is 2100W, the scanning speed is 4mm/s, the overlapping rate is 45%, and the powder feeding amount is 0.8r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared.
Step II: and (3) performance testing:
according to the requirement of the tensile plate size in the GB/T228.1-2010 metal material tensile test standard, the tensile plate is taken from the test block for tensile test, the average value of the tensile strength is 240.49MPa, the average value of the elongation at break is 9.06%, and the results show that the tensile strength and the elongation at break are obviously improved by comparing with the pure ZL114A tensile strength of 149.7MPa and the elongation at break of 2.87%.
Example 3
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combined method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 5min at 500 ℃, taking out and cooling to obtain the expanded graphene sheet.
And (3) putting 0.2g of the expanded graphene sheet into a beaker, adding 200mL of absolute ethyl alcohol, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 4 hours to obtain the few-layer graphene nanosheet.
Step 2: wet ball milling
Before ball milling, 2-5mm ball milling balls are placed into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, and each time is 5-10 minutes, so that 2-5mm ball milling balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank by absolute ethyl alcohol, and performing ball milling on balls with the mass ratio of 2-5 mm: (cast aluminum powder ZL114A + few-layer graphene nanosheets) =3:1, cast aluminum powder ZL114A: few-layer graphene nanoplatelets =999:1;
putting graphene, cast aluminum powder ZL114A and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 600:160 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 Pa, putting the ball milling tank into a ball mill, carrying out ball milling for 16h (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 260r/min, and drying after ball milling to obtain aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The sphericity of the prepared graphene aluminum-based composite powder for laser deposition manufacturing is 0.86.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared in the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece.
Step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeding barrel, the power of a 6KW semiconductor laser and the scanning speed of a coaxial powder feeding head are set through a computer system of a computer, and the laser power is 2000W, the scanning speed is 4.5mm/s, the overlapping rate is 45%, and the powder feeding amount is 0.7r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared.
Example 4
A method for preparing graphene aluminum-based composite powder for laser deposition manufacturing, which is different from that of example 1 in that: the laser power was 2000W and the scanning speed was 5.5mm/s.
Example 5
A method for preparing graphene aluminum-based composite powder for laser deposition manufacturing, which is different from that of example 3 in that: the ball milling time is 14h (stopping for 15min every 30 min), and the ball milling speed is adjusted to 240r/min
Example 6
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combination method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 3min at 600 ℃, taking out, and then cooling to room temperature in air to obtain the expanded graphene sheet.
And (3) putting 0.2g of expanded graphene sheet into a beaker, adding 150mL of absolute ethyl alcohol, putting into an ultrasonic machine, and carrying out ultrasonic treatment for 3 hours at the ultrasonic frequency of 40KHz to obtain the few-layer graphene nanosheet.
Step 2: wet ball milling
Before ball milling, 2-5mm stainless steel balls are prepared and put into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, 5-10 minutes each time, and the 2-5mm stainless steel balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank with absolute ethyl alcohol, and grinding with 2-5mm stainless steel balls according to the mass ratio: (wrought aluminum alloy 6061+ few-layer graphene nanosheets) =4:1, wrought aluminum alloy 6061: few-layer graphene nanoplatelets =1000:1;
putting graphene, wrought aluminum alloy 6061 and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 800:200 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 And Pa, putting the ball milling tank into a ball mill, ball milling for 15h (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 250r/min, and drying after ball milling to obtain aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The sphericity of the prepared graphene aluminum-based composite powder for laser deposition manufacturing is 0.88.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared by the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece, and the method comprises the following steps:
step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeding barrel, the power of a 6KW semiconductor laser and the scanning speed of a coaxial powder feeding head are set through a computer system of a computer, and the laser power is 1800W, the scanning speed is 4mm/s, the lap joint rate is 45%, and the powder feeding amount is 0.5r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared.
Step II: and (3) performance testing:
and (3) taking a tensile plate from a test block according to the dimensional requirement of the tensile plate in the GB/T228.1-2010 metal material tensile test standard, and carrying out a tensile test, wherein the average value of the tensile strength is 220.57MPa, and the average value of the elongation at break is 5.8%.
Example 7
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combined method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 3min at 600 ℃, taking out the crucible, and then cooling to room temperature in air to obtain the expanded graphene sheet.
And (3) putting 0.15g of expanded graphene sheet into a beaker, adding 150mL of absolute ethyl alcohol, putting into an ultrasonic machine, and performing ultrasonic treatment for 2.5 hours at the ultrasonic frequency of 40KHz to obtain the few-layer graphene nanosheet.
Step 2: wet ball milling
Before ball milling, 2-5mm stainless steel balls are prepared and put into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, 5-10 minutes each time, and the 2-5mm stainless steel balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank with absolute ethyl alcohol, and grinding with 2-5mm stainless steel balls according to the mass ratio: (wrought aluminum alloy 6061+ few-layer graphene nanosheets) =3:1, wrought aluminum alloy 6061: few-layer graphene nanoplatelets =666:1;
putting graphene, wrought aluminum alloy 6061 and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 700:150 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 Pa, putting the ball milling tank into a ball mill, performing ball milling for 13 hours (stopping for 15min every 30 min), adjusting the ball milling rotation speed to 230r/min, and drying after ball milling to obtain aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The sphericity of the prepared graphene aluminum-based composite powder for laser deposition manufacturing is 0.89.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared by the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece, and the method comprises the following steps:
step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeding barrel, the power of a 6KW semiconductor laser and the scanning speed of a coaxial powder feeding head are set through a computer system of a computer, and the laser power is 1900W, the scanning speed is 5mm/s, the lap joint rate is 46 percent, and the powder feeding amount is 0.6r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared.
Step II: and (4) performance testing:
according to the requirement of the size of the stretching plate in GB/T228.1-2010 metal material stretching test standard, the stretching plate is taken from a test block for stretching test, the average value of the tensile strength is 228.75MPa, and the average value of the elongation at break is 7.3%.
Example 8
A preparation method of graphene aluminum-based composite powder for laser deposition manufacturing comprises the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combined method
And (3) putting the intercalation expandable graphite raw material into a crucible, putting the crucible into a muffle furnace by using crucible tongs, heating for 3min at 600 ℃, taking out, and then cooling to room temperature in air to obtain the expanded graphene sheet.
And (3) putting 0.3g of expanded graphene sheet into a beaker, adding 150mL of absolute ethyl alcohol, putting into an ultrasonic machine, and carrying out ultrasonic treatment for 5 hours at the ultrasonic frequency of 40KHz to obtain the few-layer graphene nanosheet.
And 2, step: wet ball milling
Before ball milling, 2-5mm stainless steel balls are prepared and put into a beaker, absolute ethyl alcohol is added for ultrasonic cleaning for 3-5 times, 5-10 minutes each time, and the 2-5mm stainless steel balls after impurity removal are obtained.
Wiping the inner wall of the ball milling tank with absolute ethyl alcohol, and grinding with 2-5mm stainless steel balls according to the mass ratio: (wrought aluminum alloy 6061+ few-layer graphene nanosheets) =5:1, wrought aluminum alloy 6061: few-layer graphene nanoplatelets =1999:1;
placing graphene, wrought aluminum alloy 6061 and 2-5mm ball-milling balls into a ball-milling tank to form a mixture, and adding absolute ethyl alcohol into the ball-milling tank, wherein the ratio of the mixture to the absolute ethyl alcohol is 500:200 in g: mL.
The ball milling tank is vacuumized, and the vacuum degree is 4.0 multiplied by 10 -2 Pa, placing the ball milling pot into a ball mill, and performing ball milling for 18h (stopping for 15min every 30 min)Adjusting the ball milling rotation speed to 280r/min, and drying after ball milling to obtain the aluminum powder wrapping the graphene nanosheets, namely the graphene aluminum-based composite powder for laser deposition manufacturing.
The sphericity of the prepared graphene aluminum-based composite powder for laser deposition manufacturing is 0.85.
The graphene aluminum-based composite powder for laser deposition manufacturing prepared by the embodiment is subjected to laser deposition manufacturing to obtain a graphene aluminum-based composite material workpiece, and the method comprises the following steps:
step I: laser deposition manufacturing:
the laser deposition manufacturing is carried out by adopting LDM-800 in the experiment, the mixed graphene aluminum-based composite powder for the laser deposition manufacturing is placed in a powder feeding barrel, the power of a 6KW semiconductor laser and the scanning speed of a coaxial powder feeding head are set through a computer system of a computer, and the laser power is 1800W, the scanning speed is 6mm/s, the overlapping rate is 48 percent, and the powder feeding amount is 0.6r/min. Test pieces 70mm long, 16mm wide and 8mm high were prepared.
Step II: and (3) performance testing:
according to the requirement of the size of the stretching plate in the GB/T228.1-2010 metal material stretching test standard, the stretching plate is taken from a test block for stretching test, the average value of the tensile strength is 230.54MPa, and the average value of the elongation at break is 8.7%.
Example 9
A method for preparing graphene aluminum-based composite powder for laser deposition manufacturing, which is different from that of example 6 in that: the laser power is 2000W, the scanning speed is 5mm/s, the lap joint rate is 50 percent, and the powder feeding amount is 0.7r/min.
Example 10
A method for preparing graphene aluminum-based composite powder for laser deposition manufacturing, which is different from that of example 8 in that: the ball milling time is 14h (stopping for 15min every 30 min), and the ball milling speed is adjusted to 230r/min.
Comparative example 1:
preparing aluminum-based powder, determining the optimal parameters suitable for the aluminum powder by using an orthogonal test, carrying out laser deposition manufacturing, similarly preparing test pieces with the length of 70mm, the width of 16mm and the height of 8mm, taking out a drawing plate shown in the figure by using wire-electrode cutting, carrying out a tensile test, measuring the tensile strength and the elongation at break of three test pieces, and calculating the average value, wherein the average value of the tensile strength of pure ZL114A is 149.7MPa, and the average value of the elongation at break is 2.87%.
Comparative example 2:
taking the ball-milled graphene aluminum-based composite powder, performing additive manufacturing and forming by using a KUKA robot, preparing a test piece with the length of 70mm, the width of 16mm and the height of 8mm, taking out a tensile plate shown in the figure by using spark wire cutting, performing a tensile test, and measuring the tensile strength and the elongation at break. Tests show that when each layer of the robot is processed, a corresponding starting point and a corresponding end point are needed, the operation is complex, the efficiency is low, and meanwhile, certain errors are considered to exist in points, so that the forming quality is influenced.
Comparative example 3:
the surface appearance of the obtained cast-formed workpiece is shown in fig. 4, and compared with the surface appearance of the graphene aluminum-based composite material workpiece prepared by laser deposition in the embodiment 1, it is found that the surface of the graphene aluminum-based composite material workpiece prepared by laser deposition in the invention is relatively flat, which indicates that no air holes are generated in the invention, but a cavity is generated on the surface of the cast-formed workpiece, which indicates that the problem that the air holes are easily generated in the method of the invention through the improvement of the material in the laser deposition manufacturing process can be solved, and the defect that the performance of the workpiece is reduced due to the air holes easily generated in the cast-formed workpiece can also be solved.

Claims (10)

1. The graphene aluminum-based composite powder for laser deposition manufacturing is characterized by comprising a few-layer graphene nanosheet prepared by a thermal expansion-ultrasonic combined method and aluminum-based powder, wherein the few-layer graphene nanosheet prepared by the thermal expansion-ultrasonic combined method comprises the following components in percentage by mass: aluminum matrix powder =1 (666-1999), wherein few-layer graphene nanosheets are uniformly dispersed on the surface of aluminum powder particles, and the prepared graphene aluminum-based composite powder for laser deposition manufacturing has a sphericity of 0.85-0.9; the graphene aluminum-based composite powder for laser deposition manufacturing is aluminum powder wrapped by few layers of graphene nanosheets;
the temperature of thermal expansion of the few-layer graphene nanosheet prepared by the thermal expansion-ultrasonic combination method is 500-800 ℃;
the graphene aluminum-based composite powder for laser deposition manufacturing is prepared by the following steps:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combination method
Insulating the intercalation expandable graphite raw material at 500 to 800 ℃ for 1 to 5min, taking out, and air-cooling to room temperature to obtain an expanded graphene sheet;
mixing the expanded graphene sheets with absolute ethyl alcohol, and carrying out ultrasonic treatment for 2 to 5 hours to obtain few-layer graphene nanosheets; according to the solid-liquid ratio, the expanded graphene sheet: absolute ethanol = (0.1-0.3) g: (100-200) mL;
and 2, step: wet ball milling
Mixing the millimeter-scale ball grinding ball, the aluminum matrix powder and the few-layer graphene nanosheets in proportion after impurity removal to obtain a mixture; wherein, according to the mass ratio, millimeter level ball grinding ball: (aluminum matrix powder + few-layer graphene nanosheets) = (3-5): 1, aluminum matrix powder: few-layer graphene nanoplatelets = (666-1999): 1;
placing the mixture into a ball milling tank, adding absolute ethyl alcohol into the ball milling tank to perform wet ball milling, and drying after ball milling to obtain aluminum powder wrapping few-layer graphene nanosheets, namely graphene aluminum-based composite powder; according to the solid-liquid ratio, the mixture: absolute ethanol = (500-800) g: (120-200) mL.
2. The method for preparing graphene aluminum-based composite powder for laser deposition fabrication according to claim 1, comprising the steps of:
step 1: graphene sheet prepared by thermal expansion-ultrasonic combined method
Keeping the temperature of the intercalated expandable graphite raw material at 500-800 ℃ for 1-5 min, taking out, and air-cooling to room temperature to obtain expanded graphene sheets;
mixing the expanded graphene sheets with absolute ethyl alcohol, and carrying out ultrasonic treatment for 2 to 5 hours to obtain few-layer graphene nanosheets; according to the solid-liquid ratio, the expanded graphene sheet: absolute ethanol = (0.1-0.3) g: (100-200) mL;
and 2, step: wet ball milling
Mixing the millimeter-scale ball grinding ball, the aluminum matrix powder and the few-layer graphene nanosheets in proportion after impurity removal to obtain a mixture; wherein, according to the mass ratio, millimeter level ball grinding ball: (aluminum matrix powder + few-layer graphene nanosheets) = (3-5): 1, aluminum matrix powder: few-layer graphene nanoplatelets = (666-1999): 1;
placing the mixture into a ball milling tank, adding absolute ethyl alcohol into the ball milling tank to perform wet ball milling, and drying after ball milling to obtain aluminum powder wrapping few-layer graphene nanosheets, namely graphene aluminum-based composite powder; according to the solid-liquid ratio, the mixture: absolute ethanol = (500-800) g: (120-200) mL.
3. The method for preparing graphene aluminum-based composite powder for laser deposition manufacturing according to claim 2, wherein in the step 1, ultrasonic frequency is 38-42KHz.
4. The method as claimed in claim 2, wherein in step 2, the aluminum matrix powder is one of ZL114A, ZL101A and 6061.
5. The method according to claim 2, wherein in the step 2, the millimeter-sized balls are 2-5mm balls, and the balls are stainless steel balls, zirconia balls or agate balls.
6. The method for preparing graphene aluminum-based composite powder for laser deposition manufacturing according to claim 2, wherein in the step 2, the wet ball milling process is as follows: vacuumizing the ball milling tank until the vacuum degree reaches 4.0 multiplied by 10 -2 PaPutting a ball milling tank into a ball mill, wherein the ball milling adopts interval ball milling, the total ball milling time is 12 to 18h, the ball milling is stopped for 10 to 15min at the time of 30min each time, and the ball milling is carried outThe grinding speed is 220 to 280r/min.
7. The application of the graphene aluminum-based composite powder for laser deposition manufacturing as claimed in claim 1, wherein the graphene aluminum-based composite powder for laser deposition manufacturing is used as a raw material for laser deposition manufacturing to perform additive manufacturing to prepare a graphene aluminum-based composite workpiece.
8. Use of the graphene aluminium-based composite powder for laser deposition fabrication according to claim 7, characterized by comprising the following steps:
the graphene aluminum-based composite powder for laser deposition manufacturing is molded by adopting a laser deposition process to obtain a graphene aluminum-based composite material workpiece, the laser power is 1600-2400W, the scanning speed is 3-10mm/s, the lap joint rate is 45-50%, and the powder feeding amount is 0.5-0.8r/min.
9. Use of the graphene aluminum-based composite powder for laser deposition fabrication according to claim 7, wherein the laser power is 1800-2100W and the scanning speed is 4-6mm/s.
10. The application of the graphene aluminum-based composite powder for laser deposition manufacturing according to claim 7 or 8, wherein the tensile strength of the prepared graphene aluminum-based composite workpiece is enhanced by 47.34% -61% compared with an aluminum-based base material, and the elongation at break of the prepared graphene aluminum-based composite workpiece is enhanced by 102.1% -216% compared with the aluminum-based base material.
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