CN108772564B - Selective laser melting formed graphene reinforced aluminum matrix composite and preparation method thereof - Google Patents
Selective laser melting formed graphene reinforced aluminum matrix composite and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a selective laser melting formed graphene reinforced aluminum matrix composite material and a preparation method thereof. The method is prepared by an additive manufacturing process, and compared with the traditional material removing processing process, the method saves materials and energy to the maximum extent; in the steps, the graphene/aluminum-based composite material is uniformly dispersed in a mode of ultrasonic dispersion, freeze drying and liquid nitrogen nodular graphite, and the processes of freeze drying and liquid nitrogen cold quenching are added in the dispersion process of the ethanol-dispersed graphene researched at the present stage, so that the dispersion and addition of the graphene with higher content are realized. Further, the aluminum-based composite material is prepared by a selective laser melting forming technology, so that the product is directly manufactured on the basis of shortening working hours and cost, and the method is suitable for the fields of aviation manufacturing, machining, medical treatment, household consumption and the like.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a selective laser melting formed graphene reinforced aluminum matrix composite material and a preparation method thereof.
Background
Compared with the traditional matrix alloy, the aluminum-based composite material has high specific strength and specific stiffness, excellent high-temperature mechanical property, low thermal expansion coefficient and excellent wear resistance, and has very wide application prospect in the aviation, aerospace, automobile, electronic and transportation industries. The light weight, high strength and multiple functions of the composite material determine the great development potential of the composite material. Therefore, aluminum matrix composites are one of the most important materials in metal matrix composites. The common reinforcements such as silicon carbide, boron carbide, aluminum oxide and the like have to improve the enhancement effect on the comprehensive performance of the material, reduce the plasticity more and limit the application of the composite material. With the progress and development of science and technology, higher requirements are increasingly put forward on light-weight, high-strength, elastic and high-modulus aluminum alloy materials. Therefore, the need for developing high performance aluminum matrix composites has become very urgent.
Graphene (graphene) is a novel class of carbon materials, and has excellent properties because it is a two-dimensional material with a single atomic layer thickness in a honeycomb lattice composed of carbon atoms with sp2 hybrid orbitals. The graphene has excellent mechanical, electrical and thermal properties and the like, and the carrier mobility is 15000cm2V · s; the thermal conductivity can reach 5000W/(m.K), which is 3 times of that of diamond; the strength and the elastic modulus were 125GPa and 1100GPa, respectively; has extremely large specific surface area reaching 2630m2(ii) in terms of/g. Therefore, the graphene is an ideal reinforcement for preparing the high-performance metal matrix composite, and is added into the aluminum matrix, so that the mechanical and thermal properties of the aluminum matrix are expected to be greatly improved.
As a new processing mode, the additive manufacturing technology is applied to many industries needing customization by virtue of the advantage of free manufacturing. The selective laser melting is used as a process for additive manufacturing, so that the time for product development is shortened, more complex parts can be manufactured, the personalized customization cost is reduced, and the raw material waste is reduced. With the progress of industrial level, the aesthetic requirements of people and the diversification degree of the requirements of living goods are continuously improved, the practicability of the additive manufacturing product is certainly stronger and stronger, and the application range is wider and wider. Has been widely and mature applied in the industries of automobile spare parts, mold trial manufacturing, toy models, medical treatment and health, creative design, jewelry manufacturing and the like.
The graphene reinforced aluminum matrix composite mainly has the following problems: the wettability of graphene and an aluminum matrix is poor, the graphene is difficult to uniformly disperse in the alloy, so that the mechanical property of the composite material is influenced, and meanwhile, the content of the graphene is low.
Disclosure of Invention
The invention aims to provide a selective laser melting formed graphene reinforced aluminum matrix composite and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a selective laser melting formed graphene reinforced aluminum-based composite material is disclosed, wherein the graphene content in the composite material is 2-5 wt%.
According to the selective laser melting formed graphene reinforced aluminum matrix composite material, the content of graphene is greatly improved, and the graphene is uniformly dispersed in an aluminum matrix.
The invention further provides a preparation method of the selective laser melting formed graphene reinforced aluminum matrix composite, which comprises the following steps:
1) uniformly dispersing graphene and stearic acid in ethanol, and then carrying out freeze drying to obtain powder A;
2) sequentially carrying out liquid nitrogen cold quenching and vacuum ball milling on the powder A, the spherical silicon powder and the stearic acid in a ball mill to obtain modified graphene;
3) carrying out ball milling on the modified graphene, aluminum powder and stearic acid in a ball mill under the liquid nitrogen environment to obtain modified graphene-aluminum powder mixed powder, and carrying out vacuum drying;
4) and taking the modified graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar.
Wherein the particle size of the spherical silicon powder is 10-18 μm, and the particle size of the aluminum powder is 38-45 μm. The aluminum powder is preferably high-purity spherical aluminum powder, and the aluminum content is 99.8%. The strict control of the powder granularity is beneficial to reducing the surface roughness and the quality of a selective laser melting formed part.
In the step 1), stearic acid accounts for 1-5wt% of the mass of the graphene, and 1g of the graphene is added with 200 ml of ethanol; ultrasonic dispersion is adopted, and the dispersion time is 0.5-6 h.
In the step 1), the temperature of freeze drying is from minus 50 ℃ to 0 ℃ and the time is 2 to 12 hours.
In the step 2), the mass ratio of the graphene to the spherical silicon powder is 1:3-6, and the adding amount of the stearic acid is 1-3wt% of the mass of the spherical silicon powder.
In the step 2), the time of liquid nitrogen cold quenching is 0.5-5 h; during vacuum ball milling, the ball-material ratio is 5-7:1, the rotating speed is 100-.
In the step 3), the mass percentage of the modified graphene to the aluminum powder is 1:4-7, the mass of the stearic acid added is 1-5wt% of the mass of the aluminum powder, and the grinding ball is immersed by the amount of liquid nitrogen.
In the step 3), during ball milling, the ball-material ratio is 5-7:1, the rotating speed is 100-; the vacuum drying temperature is 50-60 ℃. If the ball-material ratio, the rotation speed and the time are not properly controlled, the structure of the graphene can be damaged, so that strict control is required.
In the step 4), when the selective laser melting is formed, the laser power is as follows: 280-340W, scanning speed: 4-12m/s, layer thickness: 0.03-0.06 mm.
According to the preparation method of the selective laser melting graphene aluminum-based composite material, disclosed by the invention, the material and energy are saved to the greatest extent compared with the traditional material removing processing technology by preparing the selective laser melting graphene aluminum-based composite material through an additive manufacturing process; in the steps, the graphene/aluminum-based composite material is uniformly dispersed in a mode of ultrasonic dispersion, freeze drying and liquid nitrogen nodular graphite, and the processes of freeze drying and liquid nitrogen cold quenching are added in the dispersion process of the ethanol-dispersed graphene researched at the present stage, so that the dispersion and addition of the graphene with higher content are realized. Further, the aluminum-based composite material is prepared by selecting a laser melting forming technology, so that the product is directly manufactured on the basis of shortening the working hours and the cost, and the method is suitable for the fields of aviation manufacturing, machining, medical treatment, household consumption and the like.
Detailed Description
The technical solution of the present invention is illustrated by the following specific examples, but the scope of the present invention is not limited thereto:
example 1
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) 2g of graphene and 0.06g of stearic acid are placed in a beaker, 400ml of ethanol is added, and then the mixture is placed in an ultrasonic machine for ultrasonic dispersion to obtain mixed powder, and the mixed powder is frozen and dried; wherein the ultrasonic dispersion time is 0.5h, the freeze-drying temperature is-50 ℃, and the freeze-drying time is 2 h;
2) putting the powder dried in the step 1), spherical silicon powder and stearic acid into a ball mill, filling liquid nitrogen into the ball mill, performing cold quenching for a period of time, and performing vacuum ball milling to obtain modified graphene; the mass ratio of the graphene to the silicon powder is 1:6, the stearic acid accounts for 1 wt% of the spherical silicon powder, the liquid nitrogen cold quenching time is 0.5 hour, and the ball material ratio is as follows: 5:1, rotation speed: ball milling for 1h at 100 rpm;
3) putting the modified graphene, high-purity spherical aluminum powder (the aluminum content is 99.8 percent, the same below) and stearic acid into a ball mill, filling liquid nitrogen into the ball mill, carrying out ball milling to obtain modified graphene-aluminum powder mixed powder, and carrying out vacuum drying; the mass ratio of the modified graphene to the high-purity aluminum powder is 1:7, and the stearic acid accounts for 3wt% of the aluminum powder; immersing a grinding ball in liquid nitrogen at a ball-material ratio of 6:1 and a rotating speed of 100rpm, and carrying out ball milling for 0.5 h; the vacuum drying temperature is as follows: 50 ℃;
4) and taking the dried modified graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 340W, the scanning speed is 12m/s, and the layer thickness is 0.06 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Example 2
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) 2g of graphene and 0.06g of stearic acid are placed in a beaker, 400ml of ethanol is added and the beaker is placed in an ultrasonic machine for ultrasonic dispersion to obtain mixed powder, and freeze drying is carried out; wherein the ultrasonic dispersion time is 2h, the freeze-drying temperature is-40 ℃, and the freeze-drying time is 6 h;
2) putting the powder dried in the step 1), spherical silicon powder and stearic acid into a ball mill, filling liquid nitrogen into the ball mill, performing cold quenching for a period of time, and performing vacuum ball milling to obtain modified graphene; the mass ratio of the graphene to the high-purity silicon powder is 1:5, the stearic acid accounts for 1 wt% of the spherical silicon powder, the liquid nitrogen cold quenching time is 2 hours, and the ball material ratio is as follows: 7:1, rotating speed: 200rpm, ball milling: 2 h;
3) placing the modified graphene, the high-purity spherical aluminum powder and the stearic acid in a ball mill, filling liquid nitrogen into the ball mill, performing ball milling to obtain modified graphene-aluminum powder mixed powder, and performing vacuum drying; the mass ratio of the modified graphene to the high-purity aluminum powder is 1:6, and the stearic acid accounts for 3wt% of the aluminum powder; immersing a grinding ball in liquid nitrogen at a ball-material ratio of 6:1 and a rotating speed of 100rpm, and carrying out ball milling for 1 h; the vacuum drying temperature is as follows: 55 ℃;
4) and taking the dried modified graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 320W, the scanning speed is 10m/s, and the layer thickness is 0.05 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Example 3
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) 2g of graphene and 0.06g of stearic acid are placed in a beaker, 400ml of ethanol is added and the beaker is placed in an ultrasonic machine for ultrasonic dispersion to obtain mixed powder, and freeze drying is carried out; wherein the ultrasonic dispersion time is 4h, the freeze-drying temperature is-20 ℃, and the freeze-drying time is 8 h;
2) putting the powder dried in the step 1), spherical silicon powder and stearic acid into a ball mill, filling liquid nitrogen into the ball mill, performing cold quenching for a period of time, and performing vacuum ball milling to obtain modified graphene; the mass ratio of the graphene to the high-purity silicon powder is 1:4, the stearic acid accounts for 1 wt% of the spherical silicon powder, the liquid nitrogen cold quenching time is 4h, and the ball material ratio is as follows: 6:1, rotating speed: ball milling at 250rpm for 2.5 hr;
3) placing the modified graphene, the high-purity spherical aluminum powder and the stearic acid in a ball mill, filling liquid nitrogen into the ball mill, performing ball milling to obtain modified graphene-aluminum powder mixed powder, and performing vacuum drying; the mass ratio of the modified graphene to the high-purity aluminum powder is 1:5, and the stearic acid accounts for 3wt% of the aluminum powder; immersing a grinding ball in liquid nitrogen at a ball-material ratio of 6:1 and a rotation speed of 150rpm, and carrying out ball milling for 1 h; the vacuum drying temperature is as follows: 55 ℃;
4) and taking the dried modified graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 300W, the scanning speed is 6m/s, and the layer thickness is 0.04 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Example 4
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) placing 4g of graphene and 0.12g of stearic acid in a beaker, adding 800ml of ethanol, placing in an ultrasonic machine, performing ultrasonic dispersion to obtain mixed powder, and performing freeze drying; wherein the ultrasonic dispersion time is 6h, the freeze-drying temperature is-30 ℃, and the freeze-drying time is 12 h;
2) putting the powder dried in the step 1), spherical silicon powder and stearic acid into a ball mill, filling liquid nitrogen into the ball mill, performing cold quenching for a period of time, and performing vacuum ball milling to obtain modified graphene; the mass ratio of the graphene to the high-purity silicon powder is 1:3, the stearic acid accounts for 1 wt% of the spherical silicon powder, the liquid nitrogen cold quenching time is 5h, and the ball material ratio is as follows: 5:1, rotation speed: ball milling for 3 hours at 300 rpm;
3) placing the modified graphene, the high-purity spherical aluminum powder and the stearic acid in a ball mill, filling liquid nitrogen into the ball mill, performing ball milling to obtain modified graphene-aluminum powder mixed powder, and performing vacuum drying; the mass ratio of the modified graphene to the high-purity aluminum powder is 1:4, and the stearic acid accounts for 3wt% of the aluminum powder; immersing a grinding ball in liquid nitrogen at a ball-material ratio of 7:1 and a rotation speed of 150rpm, and carrying out ball milling for 1.5 h; the vacuum drying temperature is as follows: 55 ℃;
4) and taking the dried modified graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 320W, the scanning speed is 8m/s, and the layer thickness is 0.04 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Comparative example 1
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) 1g of graphene, 99g of aluminum powder and stearic acid (stearic acid accounts for 3wt% of the aluminum powder) are subjected to ball milling in a ball milling tank to obtain mixed powder. Ball material ratio: 5:1, rotation speed: ball milling is carried out for 1h at 100rpm, and the obtained mixed powder is subjected to vacuum heat drying at 60 ℃ to remove stearic acid.
2) And taking the dried graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 320W, the scanning speed is 12m/s, and the layer thickness is 0.06 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Comparative example 2
A selective laser melting graphene aluminum matrix composite material is prepared by the following steps:
1) 2g of graphene, 98g of aluminum powder and stearic acid (accounting for 3wt% of the aluminum powder) are added and ball-milled in a ball milling tank to obtain mixed powder. Ball milling is carried out for 1.5h at the ball material ratio of 7:1 and the rotating speed of 150 rpm; the resulting mixed powder was vacuum heat dried at 60 ℃ to remove stearic acid.
2) And taking the dried graphene-aluminum powder mixed powder as a raw material for selective laser melting molding, and performing selective laser melting molding under the protection of Ar, wherein the laser power is 340W, the scanning speed is 8m/s, and the layer thickness is 0.04 mm. The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
Comparative example 3 a selective laser melting graphene aluminum-based composite material, the preparation method is as follows:
1) 2.5g of graphene and 87.5g of aluminum powder are added with stearic acid (accounting for 3wt percent of the aluminum powder) and are ball-milled in a ball milling tank to obtain mixed powder. Ball milling is carried out for 2.5h at the ball material ratio of 6:1 and the rotation speed of 200 rpm; the resulting mixed powder was vacuum heat dried at 60 ℃ to remove stearic acid.
2) And taking the dried graphene-aluminum powder mixed powder as a raw material for selective laser melting forming, and performing selective laser melting forming under the protection of Ar, wherein the laser power is 340W, the scanning speed is 6mm/s, and the layer thickness is 0.04 mm.
The room-temperature mechanical properties of the finally obtained graphene aluminum-based composite material are detailed in table 1.
TABLE 1
The invention is not restricted to the details of the above-described exemplary examples, but can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention is indicated by the appended claims rather than the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (5)
1. A preparation method of a selective laser melting formed graphene reinforced aluminum matrix composite is characterized by comprising the following steps:
1) uniformly dispersing graphene and stearic acid in ethanol, and then carrying out freeze drying to obtain powder A, wherein the stearic acid accounts for 1-5wt% of the mass of the graphene, and 1g of the graphene is added into 200 ml of ethanol; ultrasonic dispersion is adopted, and the dispersion time is 0.5-6 h;
2) sequentially carrying out liquid nitrogen cold quenching and vacuum ball milling on the powder A, the spherical silicon powder and stearic acid in a ball mill to obtain modified graphene, wherein the mass ratio of the graphene to the spherical silicon powder is 1:3-6, and the adding amount of the stearic acid is 1-3wt% of the mass of the spherical silicon powder; the liquid nitrogen cold quenching time is 0.5-5 h; during vacuum ball milling, the ball-material ratio is 5-7:1, the rotating speed is 100-;
3) carrying out ball milling on the modified graphene, aluminum powder and stearic acid in a ball mill under the liquid nitrogen environment to obtain modified graphene-aluminum powder mixed powder, and carrying out vacuum drying; during ball milling, the ball-material ratio is 5-7:1, the rotating speed is 100-; the vacuum drying temperature is 50-60 ℃;
4) taking the modified graphene-aluminum powder mixed powder as a raw material for selective laser melting forming, and performing selective laser melting forming under the protection of Ar;
the graphene content in the composite material is 2-5 wt%.
2. The preparation method of the selected area laser melting formed graphene reinforced aluminum matrix composite material as claimed in claim 1, wherein in the step 1), the temperature of freeze drying is 50 ℃ below zero to 0 ℃, and the time is 2-12 h.
3. The preparation method of the selected area laser melting formed graphene reinforced aluminum matrix composite material as claimed in claim 1, wherein in the step 3), the mass percentage of the modified graphene and the aluminum powder is 1:4-7, the mass of the stearic acid added is 1-5wt% of the mass of the aluminum powder, and the grinding ball is immersed by the amount of liquid nitrogen.
4. The method for preparing the selective laser melting formed graphene reinforced aluminum matrix composite material according to claim 1, wherein in the step 4), the laser power is 280-340W: scanning speed: 4-12m/s, layer thickness: 0.03-0.06 mm.
5. The preparation method of the selective laser melting forming graphene reinforced aluminum matrix composite material as claimed in any one of claims 1 to 4, wherein the particle size of the spherical silicon powder is 10 to 18 μm, and the particle size of the aluminum powder is 38 to 45 μm.
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