CN108772564A - A kind of precinct laser fusion forming graphene reinforced aluminum matrix composites and preparation method thereof - Google Patents
A kind of precinct laser fusion forming graphene reinforced aluminum matrix composites and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to metal-base composites technical fields, and in particular to a kind of precinct laser fusion forming graphene reinforced aluminum matrix composites and preparation method thereof.The method of the invention is prepared by increasing material manufacturing technique, compared with traditional material removal processing technology, saves material and the energy to the full extent；And the evenly dispersed of graphene/aluminum based composites is realized in step by way of ultrasonic disperse+freeze-drying+liquid nitrogen spheroidal graphite, by increasing freeze-drying and liquid nitrogen cold quenching technique in the dispersing technology for the ethyl alcohol dispersed graphite alkene studied at this stage, to realize graphene dispersion and the addition of higher amount.Aluminum matrix composite is further prepared by precinct laser fusion forming technique, product is directly produced on the basis of shortening working hour and cost, is suitable for aeronautical manufacture, mechanical processing, the fields such as medical treatment and household consumption.
Description
Technical field
The invention belongs to metal-base composites technical fields, and in particular to a kind of precinct laser fusion forming graphene increasing
Strong aluminum matrix composite and preparation method thereof.
Background technology
Aluminum matrix composite has high specific strength, specific stiffness and excellent high-temperature mechanics relative to conventional matrix alloy
Energy, low coefficient of thermal expansion, excellent wearability have very wide in Aeronautics and Astronautics, automobile, electronics and communications and transportation industry
Wealthy application prospect.The high-strength light of composite material, multifunctionality determine its huge development potentiality.Therefore aluminum-base composite material
Material becomes one of the most frequently used most important material in metal-base composites.The increasings such as common silicon carbide, boron carbide and aluminium oxide
Strong body is to be improved to the enhancing effect of the comprehensive performance of material, and plasticity reduction is more, limits the application of composite material.With
The progress and development of science and technology, increasingly puts forward higher requirements the aluminum alloy materials of light-high-strength elasticity high-modulus.Therefore it grinds
The demand of hair high-performance aluminum-base composite material has become very urgent.
Graphene (graphene) is a kind of new carbon, is made of in honeycomb crystalline substance with sp2 hybridized orbits carbon atom
The two-dimensional material of the monoatomic layer thickness of lattice and have excellent performance.Graphene has the property such as excellent mechanics, electricity, calorifics
Can, carrier mobility is 15000 cm2/(V·s)；Thermal conductivity is 3 times of diamond up to 5000W/ (mK)；By force
Degree and elasticity modulus are 125 GPa and 1100 GPa respectively；With great specific surface area, reach 2630 m2/g.Cause
This, graphene is the ideal reinforcement for preparing high-performance metal based composites, is added it in aluminum substrate, is expected to substantially carry
The performances such as the mechanics and calorifics of high aluminum substrate.
Increases material manufacturing technology is as a kind of new processing method, by the advantage that " can freely manufacture ", in many needs
The industry of customization is applied.A kind of technique of the precinct laser fusion as increasing material manufacturing, shortens the time of product development, can be with
Increasingly complex part system is manufactured, personalized customized cost is reduced, reduces wastage of material.With the progress of industrial level, people
Aesthetic requirement and the Level of Diversification of daily necessities demand is continuously improved, the practicability of increasing material manufacturing product is inherently more next
It is stronger, it will be used wider and wider.Auto-parts, mold trial-production make, toy models, health care, creative design, jewelry
The industries such as manufacture have been widely applied.
Graphene reinforced aluminum matrix composites are primarily present problems with：Graphene and aluminum substrate wetability are poor, graphene
It is difficult to evenly dispersed in the alloy, to influence the mechanical property of composite material, while graphene content is low.
Invention content
The object of the present invention is to provide a kind of precinct laser fusion forming graphene reinforced aluminum matrix composites and its preparations
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of precinct laser fusion shapes graphene reinforced aluminum matrix composites, and graphene content is 2- in the composite material
5wt%。
A kind of precinct laser fusion provided by the invention shapes graphene reinforced aluminum matrix composites, and the present invention greatly improves
The content of graphene, and graphene uniform is made to be dispersed in aluminum substrate.
The present invention still further provides a kind of preparation of precinct laser fusion forming graphene reinforced aluminum matrix composites
Method, steps are as follows：
1）Graphene, stearic acid are dispersed in ethyl alcohol, freeze-drying is carried out later and obtains powders A；
2）Powders A, spherical silicon powder, stearic acid are subjected to liquid nitrogen cold quenching successively in ball mill, vacuum ball milling obtains modified graphite
Alkene；
3）Ball milling will be carried out under modified graphene, aluminium powder, stearic acid in the ball mill liquid nitrogen environment, obtains modified graphene-
Aluminium powder mixed-powder, and carry out vacuum drying；
4）The raw material shaped using modified graphene-aluminium powder mixed-powder as precinct laser fusion, under the protection of Ar into
Row selective laser melting (SLM) molding.
Wherein, the grain size of spherical silicon powder is 10-18 μm, and the grain size of aluminium powder is 38-45 μm.The preferred high pure spherical of aluminium powder
Aluminium powder, aluminium content 99.8%.Stringent control powder size advantageously reduce precinct laser fusion drip molding surface roughness and
Quality.
Step 1）In, stearic acid is the 1-5wt% of graphene quality, and 200-500ml ethyl alcohol is added in 1g graphenes；Using super
Sound disperses, jitter time 0.5-6h.
Step 1）In, the temperature of freeze-drying is subzero 50 DEG C to 0 DEG C, time 2-12h.
Step 2）In, the mass ratio of graphene and spherical silicon powder is 1:3-6, the amount that stearic acid is added are spherical silicon powder quality
1-3wt%.
Step 2）In, the time of liquid nitrogen cold quenching is 0.5-5h；When vacuum ball milling, ratio of grinding media to material 5-7:1, rotating speed 100-
300rpm, Ball-milling Time 1-3h.
Step 3）In, the mass percent of modified graphene and aluminium powder is 1:4-7, the quality that stearic acid is added are aluminium powder matter
The amount of the 1-5wt% of amount, liquid nitrogen submerge abrading-ball.
Step 3）In, when ball milling, ratio of grinding media to material 5-7:1, rotating speed 100-150rpm, time 0.5-1.5h；Vacuum is dried
Dry temperature is 50-60 DEG C.If the improper structure for being possible to destroy graphene of ratio of grinding media to material, rotating speed, time control, so needing tight
Lattice control.
The step 4）In, when selective laser melting (SLM) molding, laser power：280-340W, sweep speed：4-12m/s, layer
It is thick：0.03-0.06mm.
A kind of preparation method of precinct laser fusion graphene aluminum matrix composite of the present invention, passes through increasing material manufacturing technique system
It is standby, compared with traditional material removal processing technology, material and the energy are saved to the full extent；And pass through ultrasonic disperse in step
The mode of+freeze-drying+liquid nitrogen spheroidal graphite realizes the evenly dispersed of graphene/aluminum based composites, by being studied at this stage
Ethyl alcohol dispersed graphite alkene dispersing technology in increase freeze-drying and liquid nitrogen cold quenching technique, to realize the graphite of higher amount
Alkene disperses and addition.Aluminum matrix composite further is prepared by choosing laser thawing forming technique, is shortening working hour and cost
On the basis of directly produce product, be suitable for aeronautical manufacture, mechanical processing, medical treatment and the fields such as household consumption.
Specific implementation mode
Below the technical scheme of the invention is illustrated by a specific example, but the scope of the present invention is not limited thereto：
Embodiment 1
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）Graphene 2g, stearic acid 0.06g are placed in beaker, ethyl alcohol 400ml is added and is placed on ultrasonic disperse in ultrasonic machine, obtains
To mixed-powder, mixed-powder is freeze-dried；Wherein, ultrasonic disperse time 0.5h is freeze-dried -50 DEG C of temperature, cold
Freeze drying time 2h；
2）By step 1）Dried powder, spherical silicon powder, stearic acid are placed in ball mill, are filled with one section of liquid nitrogen cold quenching thereto
Vacuum sphere mill is carried out after time, obtains modified graphene；The mass ratio of modified graphene and silica flour is 1:6, stearic acid is spherical
The 1wt% of silica flour, 0.5 hour liquid nitrogen cold quenching time, ratio of grinding media to material：5:1, rotating speed：100rpm, ball milling 1h；
3）By the modified graphene, high pure spherical aluminium powder（Aluminium content 99.8%, similarly hereinafter）, stearic acid be placed in ball mill, Xiang Qi
In be filled with liquid nitrogen, carry out ball milling, obtain modified graphene-aluminium powder mixed-powder, and carry out vacuum drying；Modified graphene with
The mass ratio of high purity aluminum powder is 1:7, stearic acid is the 3wt% of aluminium powder quality；Liquid nitrogen submerges abrading-ball, ratio of grinding media to material 6:1, rotating speed
100rpm, ball milling 0.5h；Vacuum drying temperature is：50℃；
4）Using the modified graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 340W, sweep speed 12m/s, thickness 0.06mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
Embodiment 2
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）Graphene 2g, stearic acid 0.06g are placed in beaker, ethyl alcohol 400ml is added and is placed in ultrasonic disperse in ultrasonic machine, obtains
Mixed-powder is freeze-dried；Wherein, ultrasonic disperse time 2h is freeze-dried -40 DEG C of temperature, sublimation drying 6h；
2）By step 1）Dried powder, spherical silicon powder, stearic acid are placed in ball mill, are filled with one section of liquid nitrogen cold quenching thereto
Vacuum sphere mill is carried out after time, obtains modified graphene；Modified graphene and the mass ratio of high-purity silicon powder are 1:5, stearic acid is
The 1wt% of spherical silicon powder, liquid nitrogen cold quenching time 2 h, ratio of grinding media to material：7:1, rotating speed：200rpm, ball milling：2h；
3）The modified graphene, high pure spherical aluminium powder, stearic acid are placed in ball mill, are filled with liquid nitrogen thereto, carries out ball
Mill, obtains modified graphene-aluminium powder mixed-powder, and carry out vacuum drying；The mass ratio of modified graphene and high purity aluminum powder
It is 1:6, stearic acid is the 3wt% of aluminium powder quality；Liquid nitrogen submerges abrading-ball, ratio of grinding media to material 6:1, rotating speed 100rpm, ball milling 1h；Vacuum is dried
Dry temperature is：55℃；
4）Using the modified graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 320W, sweep speed 10m/s, thickness 0.05mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
Embodiment 3
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）Graphene 2g, stearic acid 0.06g are placed in beaker, ethyl alcohol 400ml is added and is placed in ultrasonic disperse in ultrasonic machine, obtains
Mixed-powder is freeze-dried；Wherein, ultrasonic disperse time 4h is freeze-dried -20 DEG C of temperature, sublimation drying 8h；
2）By step 1）Dried powder, spherical silicon powder, stearic acid are placed in ball mill, are filled with one section of liquid nitrogen cold quenching thereto
Vacuum sphere mill is carried out after time, obtains modified graphene；Graphene and the mass ratio of high-purity silicon powder are 1:4, stearic acid is spherical
The 1wt% of silica flour, liquid nitrogen cold quenching time 4h, ratio of grinding media to material：6:1, rotating speed：250rpm, ball milling 2.5h；
3）The modified graphene, high pure spherical aluminium powder, stearic acid are placed in ball mill, are filled with liquid nitrogen thereto, carries out ball
Mill, obtains modified graphene-aluminium powder mixed-powder, and carry out vacuum drying；The mass ratio of modified graphene and high purity aluminum powder
It is 1:5, stearic acid is the 3wt% of aluminium powder quality；Liquid nitrogen submerges abrading-ball, ratio of grinding media to material 6:1, rotating speed 150rpm, ball milling 1h；Vacuum is dried
Dry temperature is：55℃；
4）Using the modified graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 300W, sweep speed 6m/s, thickness 0.04mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
Embodiment 4
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）Graphene 4g, stearic acid 0.12g are placed in beaker, ethyl alcohol 800ml is added and is placed in ultrasonic disperse in ultrasonic machine, obtains
Mixed-powder is freeze-dried；Wherein, ultrasonic disperse time 6h is freeze-dried -30 DEG C of temperature, sublimation drying 12h；
2）By step 1）Dried powder, spherical silicon powder, stearic acid are placed in ball mill, are filled with one section of liquid nitrogen cold quenching thereto
Vacuum sphere mill is carried out after time, obtains modified graphene；Graphene and the mass ratio of high-purity silicon powder are 1:3, stearic acid is spherical
The 1wt% of silica flour, liquid nitrogen cold quenching time 5h, ratio of grinding media to material：5:1, rotating speed：300rpm, ball milling 3h；
3）The modified graphene, high pure spherical aluminium powder, stearic acid are placed in ball mill, are filled with liquid nitrogen thereto, carries out ball
Mill, obtains modified graphene-aluminium powder mixed-powder, and carry out vacuum drying；The mass ratio of modified graphene and high purity aluminum powder
It is 1:4, stearic acid is the 3wt% of aluminium powder quality；Liquid nitrogen submerges abrading-ball, ratio of grinding media to material 7:1, rotating speed 150rpm, ball milling 1.5h；Vacuum
Drying temperature is：55℃；
4）Using the modified graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 320W, sweep speed 8m/s, thickness 0.04mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
Comparative example 1
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）By 1g graphenes and 99g aluminium powders, then stiffened resin acid（Stearic acid is the 3wt% of aluminium powder quality）Ball milling obtains in ball grinder
To mixed-powder.Ratio of grinding media to material：5:1, rotating speed：100rpm, ball milling 1h, obtained mixed-powder carry out Vacuum Heat drying at 60 DEG C,
To remove stearic acid.
2）Using the graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 320W, sweep speed 12m/s, thickness 0.06mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
Comparative example 2
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）By 2g graphenes and 98g aluminium powders, then ball milling obtains mixed-powder to stiffened resin acid (3wt% for accounting for aluminium powder) in ball grinder.
Ratio of grinding media to material 7:1, rotating speed 150rpm, ball milling 1.5h；, obtained mixed-powder carries out Vacuum Heat drying at 60 DEG C, destearinized with removing
Acid.
2）Using the graphene of the drying-aluminium powder mixed-powder as the raw material of selective laser melting (SLM) molding, Ar's
Protection is lower to carry out selective laser melting (SLM) molding, laser power 340W, sweep speed 8m/s, thickness 0.04mm.The stone finally obtained
The room-temperature mechanical property of black alkene aluminum matrix composite refers to table 1.
Comparative example 3
A kind of precinct laser fusion graphene aluminum matrix composite, preparation method are as follows：
1）By 2.5g graphenes and 87.5g aluminium powders, then stiffened resin acid（Account for the 3wt% of aluminium powder）Ball milling is mixed in ball grinder
Powder.Ratio of grinding media to material 6:1, rotating speed 200rpm, ball milling 2.5h；Obtained mixed-powder carries out Vacuum Heat drying at 60 DEG C, to remove
Stearic acid.
2）The raw material that the graphene of the drying-aluminium powder mixed-powder is shaped as precinct laser fusion, Ar's
Protection is lower to carry out precinct laser fusion forming, laser power 340W, sweep speed 6mm/s, thickness 0.04mm.
The room-temperature mechanical property of the graphene aluminum matrix composite finally obtained refers to table 1.
The present invention is not limited to the details of above-mentioned exemplary embodiment, and in the spirit or essential attributes without departing substantially from the present invention
In the case of, the present invention can be realized in other specific forms.Therefore, in all respects, embodiment should all be regarded as
It is exemplary, and is non-limiting.The scope of the invention being indicated by the appended claims rather than by the foregoing description, therefore
It includes within the present invention to be intended to fall all changes in the meaning and scope of the same important document of claim.
Claims (10)
1. a kind of preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites, which is characterized in that step is such as
Under：
1）Graphene, stearic acid are dispersed in ethyl alcohol, freeze-drying is carried out later and obtains powders A；
2）Powders A, spherical silicon powder, stearic acid are subjected to liquid nitrogen cold quenching successively in ball mill, vacuum ball milling obtains modified graphite
Alkene；
3）Ball milling will be carried out under modified graphene, aluminium powder, stearic acid in the ball mill liquid nitrogen environment, obtains modified graphene-
Aluminium powder mixed-powder, and carry out vacuum drying；
4）The raw material shaped using modified graphene-aluminium powder mixed-powder as precinct laser fusion, under the protection of Ar into
Row selective laser melting (SLM) molding.
2. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 1）In, stearic acid is the 1-5wt% of graphene quality, and 200-500ml ethyl alcohol is added in 1g graphenes；Using super
Sound disperses, jitter time 0.5-6h.
3. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 1）In, the temperature of freeze-drying is subzero 50 DEG C to 0 DEG C, time 2-12h.
4. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 2）In, the mass ratio of modified graphene and spherical silicon powder is 1:3-6, the amount that stearic acid is added are spherical silicon powder
The 1-3wt% of quality.
5. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 2）In, the time of liquid nitrogen cold quenching is 0.5-5h；When vacuum ball milling, ratio of grinding media to material 5-7:1, rotating speed 100-
300rpm, Ball-milling Time 1-3h.
6. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 3）In, the mass percent of modified graphene and aluminium powder is 1:4-7, the quality that stearic acid is added are aluminium powder matter
The amount of the 1-5wt% of amount, liquid nitrogen submerge abrading-ball.
7. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, step 3）In, when ball milling, ratio of grinding media to material 5-7:1, rotating speed 100-150rpm, time 0.5-1.5h；Vacuum drying
Temperature is 50-60 DEG C.
8. the preparation method of precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1, special
Sign is, the step 4）In, when selective laser melting (SLM) molding, laser power 280-340W：Sweep speed：4-12m/s, layer
It is thick：0.03-0.06mm.
9. the preparation side of the precinct laser fusion forming graphene reinforced aluminum matrix composites as described in claim 1-8 is any
Method, which is characterized in that the grain size of spherical silicon powder is 10-18 μm, and the grain size of aluminium powder is 38-45 μm.
10. the precinct laser fusion that any the methods of claim 1-9 obtain shapes graphene reinforced aluminum matrix composites,
It is characterized in that, graphene content is 2-5wt% in the composite material.
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| CN109454240A (en) * | 2018-12-19 | 2019-03-12 | 西安增材制造国家研究院有限公司 | A kind of graphene alloy nano composite material preparation method and SLM forming technology |
| CN110257657A (en) * | 2019-07-25 | 2019-09-20 | 成都先进金属材料产业技术研究院有限公司 | The method for preparing graphene enhancing aluminum alloy materials based on selective laser smelting technology |
| CN110640140A (en) * | 2019-10-31 | 2020-01-03 | 中北大学 | Preparation method of graphene reinforced porous aluminum-based composite material |
| CN113814415A (en) * | 2021-10-08 | 2021-12-21 | 江苏省特种设备安全监督检验研究院 | Method for preparing graphene composite antifriction metal material by adopting SLM (selective laser melting) technology |
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