CN109277560A - A kind of preparation method of high-strength and high ductility graphene/metallic composite - Google Patents
A kind of preparation method of high-strength and high ductility graphene/metallic composite Download PDFInfo
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- CN109277560A CN109277560A CN201810437448.8A CN201810437448A CN109277560A CN 109277560 A CN109277560 A CN 109277560A CN 201810437448 A CN201810437448 A CN 201810437448A CN 109277560 A CN109277560 A CN 109277560A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000009467 reduction Effects 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 230000008014 freezing Effects 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000008236 heating water Substances 0.000 claims abstract description 5
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000010348 incorporation Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 238000013528 artificial neural network Methods 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 12
- 238000002156 mixing Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000001476 alcoholic effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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- 239000011265 semifinished product Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
Abstract
The present invention relates to a kind of preparation methods of graphene/metallic composite, belong to metal-base composites technical field.Include the following steps: to configure certain density graphene oxide solution, be quickly poured into liquid nitrogen after heating water bath.Solid after freezing is melted, is placed in liquid nitrogen and is rapidly frozen again after ethanol/water solution high speed shear-mixed is uniform with metal powder later, then freeze-drying obtains graphene oxide/composite metal powder.Graphene/metallic composite of high-compactness is obtained through discharge plasma sintering after composite powder thermal reduction.Neural network structure is presented in graphene in graphene/metallic composite prepared by the present invention, and metallic matrix good toughness can be kept while improving the intensity of composite material, and the performance of composite material is substantially better than similar composite material.Process simple possible of the invention, step is easily operated, high safety and reliability, low in cost, is suitable for large-scale production.
Description
Technical field
The invention belongs to metal-base composites technical field, specially a kind of neural network structure graphene enhances metal
The preparation method of based composites.
Background technique
The rapid development of modern industry, to the mechanical property of metal-base composites, more stringent requirements are proposed, traditional fiber
And the addition of reinforced particulate such as oxide, the introducing of carbide nanometer particle, while improving metal-base composites intensity
Make metal toughness decline obvious instead.So the metal-base composites for researching and developing high-intensity and high-tenacity becomes current Metal Substrate
The hot spot of composite material research.
Graphene is a kind of carbon atom with sp2Only one carbon atom of the planar honeycomb shape structure of hybridized orbit composition is thick
The two-dimensional material of degree, specific surface area (2630 m with super large2/ g), elasticity modulus is up to 1 TPa, and tensile strength can reach
1060 GPa are to be currently known the highest material of intensity (up to 130 GPa), also harder than diamond.Increasing of the graphene as metal
When strong body, the stress of matrix is significantly increased by the effects of crystal grain refinement, dislocation strengthening and stress transfer, so blocky stone
Black alkene metal-base composites has good mechanical property.The advantage for giving full play to graphene prepares high performance metal
Base graphene composite material can bring quantum jump to the development of metal and composite material.Such as: Yue et al. (Journal of
691 (2017) 755-762 of Alloys and Compounds) selection copper particle be matrix, graphene nanometer sheet as enhancing
Body has successfully prepared graphene/copper composite material using the technique that ball milling and vacuum heating-press sintering combine, as the result is shown stone
When black alkene nanometer sheet content is 0.5 wt%, the tensile strength for the graphene/copper composite material prepared is 230 MPa or so,
About 25% is improved than fine copper, while the Vickers hardness of graphene/copper composite material reaches 52 HV or so, improves 13% than fine copper
Left and right.But as the agglomeration of graphene can occur for the increase of graphene nanometer sheet amount, graphene nanometer sheet gradually with copper
Matrix is gradually disengaged so that composite property declines, and composite material tension failure result is also changed into brittleness by ductile rupture and breaks
It splits.Muhammad Rashad et al. (Materials International 24(2014) 101-108) pass through semi-finished product powder
Metallurgy method and hot extrusion method successfully prepare graphene nanometer sheet-aluminium composite material, and result of study shows relative to pure aluminum substrate
Material, the yield strength that the graphene reinforced aluminum matrix composites of 0.3 wt% are added improve 14.7%, and tensile strength improves
11%, respectively reach 195 MPa and 280 MPa.At the same time, toughness 9% has dropped 5% or so compared to pure aluminum substrate.
Most of researchs at present are to pass through graphene nanometer sheet or redox graphene and metal powder mechanical mixed
Conjunction or chemically combined mode, in the base using graphene as Dispersion of Reinforcement.But graphene/the metal prepared is multiple
The performance of condensation material is unsatisfactory.Its reason is mainly that the interfacial wettability between graphene and metallic element is poor, and binding force is weak,
Poor dispersion is easy to happen reunion.Especially the too high levels of graphene when, the porosity of composite material rises, graphene
More easy to reunite, this greatly weakens graphene to the strengthening effect of composite materials property, and the intensity of composite material is significantly
Plasticity and toughness are substantially reduced instead while raising.
Summary of the invention
The present invention combines bad for graphene and metal interface, and graphene dispersion is uneven after mixing, the group of being easy to appear
The problems such as poly-, using the graphene that can not only prepare neural network structure, but also it is mixed with copper to avoid graphene
Lamination problem ensure that composite powder uniformly mixes.Obtained composite material strength maintains Metal Substrate while raising again
The good toughness of body.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of high-strength and high ductility graphene/metallic composite, specific steps include:
1) certain density graphene oxide solution is configured, is quickly poured into liquid nitrogen after heating water bath to certain temperature.
2) it is put again after alcohol/water solution high speed shear-mixed is uniform after melting the solid of freezing with metal powder
It is placed in liquid nitrogen and is rapidly frozen, then freeze-drying obtains graphene oxide/metal mixed powder.
3) discharge plasma sintering obtains graphene/metallic composite of high-compactness after heat-treating composite powder.
Preferably, graphene oxide is laminated structure in step 1), and diameter is 10 ~ 50 μm, with a thickness of 2 ~ 10
Nm, single layer rate be about 99%, purity 99.8%.
Preferably, the concentration of graphene oxide solution is 0.5 ~ 3 mg/mL in step 1).
Preferably, in step 1) the control of ultrasonic disperse device frequency in 10000 ~ 20000 Hz, ultrasonic time 0.5 ~
2.0 h, ultrasonic temperature are controlled at 20 ~ 45 DEG C.
Preferably, the temperature of heating water bath is 60 ~ 90 DEG C in step 1), and heating time is 10 ~ 30 min.
Preferably, metal powder is one to multiple kind in aluminium, copper, nickel, iron and its alloy powder in step 2.
Preferably, the volume fraction of graphene oxide is 0.5 ~ 3 vol% in step 2.
Preferably, the ratio of water and ethyl alcohol is its 1:9 ~ 3:7 v/v in solution in step 2.
Preferably, the revolving speed of step 2 high speed shearing is 5000 ~ 20000 rpm, and incorporation time is 1 ~ 3 h；
Preferably, the time being freeze-dried in step 2 is 24 ~ 72 h, 10 Pa of relative degree of vacuum.
Preferably, the parameter heat-treated in step 3) are as follows: reduction temperature is 300 ~ 500 DEG C, and the recovery time is 1 ~ 3
H, reducing atmosphere are hydrogen, and protective atmosphere is argon gas, and its ratio be 1:9 ~ 3:7 v/v.
Preferably, discharge plasma sintering parameter in step 3) are as follows: sintering temperature is 500 ~ 800 DEG C, sintering pressure
For 30 ~ 50 MPa, sintering time is 5 ~ 10 min.
In graphene/metallic composite prepared by the present invention, graphene showed after liquid nitrogen frozen it is similar
The structure (attached drawing 2) of neural network, the graphene of neural network structure is closely arranged in by high speed shear mixed metal powder
Interlayer and surface, be evenly distributed.When material stress cracks, " dendron " of neural network structure graphene can be played
The effect of bridging causes crack deflection or crack branching, to delay/hinder the extension of crackle.
Therefore composite material interface prepared by the present invention is well combined, even tissue, compact structure, while intensity improves
Maintain the good toughness of metallic matrix.Rationally, simple process is efficient, high safety and reliability, at low cost for instant component proportion
It is honest and clean, it can satisfy industrial application.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is the scanning electron microscope diagram of the neural network structure graphene of one embodiment of the present of invention.
Specific embodiment
In order to keep advantages and objects of the present invention more clear, with the following Examples, to specific implementation of the invention
Mode makes more detailed description, in the following description, elaborates many concrete details in order to adequately understand this
Invention.The present invention is not limited by the specific implementation of following discloses.
Embodiment one
In aqueous solution by graphene oxide (piece diameter is 20 μm, with a thickness of 2 nm) dispersion, 1 h of ultrasonic disperse is configured to concentration
For the graphene oxide solution of 2 mg/mL.Then it is quickly poured into liquid nitrogen after heating 20 min under 80 DEG C of bath temperatures.It will
Graphene oxide after freezing melts, and the flake copper powder (graphene oxide volume fraction is 1%) with 10 μm is in water/alcoholic solution
(v:v=1:9) high speed shear-mixed, revolving speed is 10000 rpm when mixing, and incorporation time is 1 h, obtains graphene-copper mixing
Dispersion liquid.Mixed dispersion liquid is placed in rapidly to freezing in liquid nitrogen to be freeze-dried after forming solid, drying time is 48 h, is obtained
Graphene/copper composite powder.Graphene/copper powders are transferred in tube furnace, under argon gas/hydrogen (9:1 v/v) atmosphere,
60 min are restored at a temperature of 300 DEG C.Composite powder after thermal reduction carries out discharge plasma sintering, and sintering temperature is 700 DEG C,
Sintering pressure is 50 MPa, and sintering time is 8 min, obtains block graphene/copper composite material.The composite material of preparation is through drawing
Measuring is stretched, tensile strength can reach 385 MPa, elongation percentage 29%.
Embodiment two
In aqueous solution by graphene oxide (piece diameter is 20 μm, with a thickness of 2 nm) dispersion, 1 h of ultrasonic disperse is configured to concentration
The graphene oxide solution of 1 mg/mL.Then it is quickly poured into liquid nitrogen after heating 20 min at a temperature of 80 DEG C of waters.It will be cold
Graphene oxide after jelly melts, with 5 μm of spherical copper powder (graphene oxide volume fraction is 1%) water/alcoholic solution (v:
V=1:9) high speed shear-mixed, revolving speed is 10000 rpm when mixing, and incorporation time is 2 h, obtains graphene-copper mixing point
Dispersion liquid.Mixed dispersion liquid is poured into rapidly after liquid nitrogen frozen forms solid and be freeze-dried, drying time is 48 h, obtains graphite
Alkene/copper composite powder.Graphene-copper powders are transferred in tube furnace, under argon gas/hydrogen (9:1 v/v) atmosphere, 400 DEG C
At a temperature of restore 60 min.Composite powder after thermal reduction is subjected to discharge plasma sintering, sintering temperature is 700 DEG C, sintering
Pressure is 50 MPa, and sintering time is 8 min, obtains block graphene/copper composite material.The composite material finally obtained is through drawing
Measuring is stretched, tensile strength can reach 397 MPa, elongation percentage 32%.
Embodiment three
In aqueous solution by graphene oxide (piece diameter is 10 μm, with a thickness of 2 nm) dispersion, 1 h of ultrasonic disperse is configured to concentration
The graphene oxide solution of 1 mg/mL.Then it is quickly poured into liquid nitrogen after heating 20 min under 60 DEG C of bath temperatures.It will be cold
Graphene oxide after jelly melts, with 2 μm of aluminium powder (graphene oxide volume fraction is 1%) water/alcoholic solution (v:v=1:
9) high speed shear-mixed, revolving speed is 10000 rpm when mixing, and incorporation time is 1 h, obtains graphene-aluminium mixed dispersion liquid.
Mixed dispersion liquid is placed in rapidly in liquid nitrogen after freezing forms solid and is freeze-dried, drying time is 48 h, obtain graphene/
Aluminium composite powder.Graphene-aluminium composite powder is transferred in tube furnace, under argon gas/hydrogen (9:1 v/v) atmosphere, 300
60 min are restored at a temperature of DEG C.Composite powder after thermal reduction is subjected to discharge plasma sintering, sintering temperature is 550 DEG C, is burnt
Knot pressure power is 50 MPa, and sintering time is 8 min, obtains block graphene/aluminum composite material.The composite material warp finally obtained
Stretching experiment measurement, tensile strength can reach 255 MPa, elongation percentage 28%.
Example IV
In aqueous solution by graphene oxide (piece diameter is 10 μm, with a thickness of 2 nm) dispersion, 60 min of ultrasonic disperse is configured to
The graphene oxide solution of 1 mg/mL of concentration.Then it is quickly poured into liquid nitrogen after heating 20 min at a temperature of 80 DEG C of waters.
Graphene oxide after freezing is melted, with 1 μm of nickel powder (graphene oxide volume fraction is 1%) alcohol/water solution (v:
V=1:9) high speed shear-mixed, revolving speed is 10000 rpm when mixing, and incorporation time is 60 min, obtains graphene-nickel mixing
Dispersion liquid.Mixed dispersion liquid is poured into rapidly after liquid nitrogen frozen forms solid and be freeze-dried, drying time is 48 h, obtains graphite
Alkene/nickel composite powder.Graphene-nickel powder is transferred in tube furnace, under argon gas/hydrogen (7:3 v/v) atmosphere, 400 DEG C
At a temperature of restore 60 min.Composite powder after thermal reduction is subjected to discharge plasma sintering, sintering temperature is 800 DEG C, sintering
Pressure is 50 MPa, and sintering time is 10 min, obtains block graphene/nickel composite material.The composite material warp finally obtained
Stretching experiment measurement, intensity can reach 850 MPa, elongation percentage 30%.
Above example will be helpful to those skilled in the art and further understand the present invention, but not limit this in any form
Invention.It should be pointed out that those skilled in the art, without departing from the inventive concept of the premise, may be used also
To make several modifications and improvements.These are all within the scope of protection of the present invention.
Claims (12)
1. a kind of high-strength and high ductility graphene/metallic composite, it is characterized in that method includes the following steps:
(1) certain density graphene oxide solution is configured, is quickly poured into liquid nitrogen after heating water bath to certain temperature;
(2) are placed again after ethanol/water solution high speed shear-mixed is uniform with metal powder after the solid of freezing is melted
It is rapidly frozen in liquid nitrogen, then freeze-drying obtains graphene oxide/composite metal powder;
(3) discharge plasma sintering obtains graphene/metallic composite of high-compactness after heat-treating composite powder.
2. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 1)
In, graphene oxide is laminated structure, diameter is 10 ~ 50 μm, with a thickness of 2 ~ 10 nm, single layer rate be about 99%, purity is
99.8%。
3. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 1)
In, the concentration of graphene oxide solution is 0.5 ~ 3 mg/mL.
4. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 1)
In, the control of ultrasonic disperse device frequency exists in 10000 ~ 20000 Hz, 0.5 ~ 2.0 h of ultrasonic time, ultrasonic temperature control
20 ~ 45 ℃。
5. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 1)
In, the temperature of heating water bath is 60 ~ 90 DEG C, and heating time is 10 ~ 30 min.
6. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 2)
In, metal powder is one to multiple kind in aluminium, copper, nickel, iron and its alloy powder.
7. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 2)
In, the volume fraction of graphene oxide is 0.5 ~ 3 vol%.
8. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 2)
In, the ratio of water and ethyl alcohol is its 1:9 ~ 3:7 v/v in solution.
9. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 2)
In, the revolving speed of high speed shear is 5000 ~ 20000 rpm, and incorporation time is 1 ~ 3 h.
10. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 2)
In, the time of freeze-drying is 24 ~ 72 h, 10 Pa of relative degree of vacuum.
11. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that the step 3)
In, the parameter of thermal reduction are as follows: reduction temperature is 300 ~ 500 DEG C, and the recovery time is 1 ~ 3 h, and reducing atmosphere is hydrogen, is protected
Shield atmosphere is argon gas, and its ratio be 1:9 ~ 3:7 v/v.
12. such as claim 1 high-strength and high ductility graphene/metallic composite preparation method, it is characterized in that being put in step 3)
Electric plasma agglomeration parameter are as follows: sintering temperature is 500 ~ 800 DEG C, and sintering pressure is 30 ~ 50 MPa, sintering time 5
~10 min。
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Cited By (6)
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| CN109825734A (en) * | 2019-04-01 | 2019-05-31 | 江西理工大学 | Collaboration enhancing Cu-base composites and preparation method thereof |
| CN111549246A (en) * | 2020-04-24 | 2020-08-18 | 郑州大学 | Preparation method of high-toughness graphene/ZK 61 magnesium alloy composite material |
| CN111686714A (en) * | 2020-07-27 | 2020-09-22 | 兰州交通大学 | Preparation method of oxygen-enriched vacancy cerium-molybdenum-based nanosphere electrochemical nitrogen fixation catalyst |
| CN111701598A (en) * | 2020-06-29 | 2020-09-25 | 兰州交通大学 | Efficient iron-molybdenum-based nitrogen reduction electrocatalyst and preparation method thereof |
| CN113333773A (en) * | 2021-06-24 | 2021-09-03 | 中国矿业大学 | Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock |
| CN113894293A (en) * | 2021-10-08 | 2022-01-07 | 江苏省特种设备安全监督检验研究院 | Method for preparing graphene composite 18Ni-300 antifriction metal material based on SLM technology |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396586A (en) * | 2013-08-09 | 2013-11-20 | 中国科学院宁波材料技术与工程研究所 | Graphene oxide fiber, preparation method, and preparation method of graphene oxide fiber composite material |
| CN105349846A (en) * | 2015-11-02 | 2016-02-24 | 唐山建华科技发展有限责任公司 | Preparation method of graphene/aluminum composite material |
| CN105385870A (en) * | 2015-11-02 | 2016-03-09 | 唐山建华科技发展有限责任公司 | Preparation method of graphene/aluminum composite material |
| CN105821227A (en) * | 2016-06-01 | 2016-08-03 | 哈尔滨理工大学 | Method for preparing graphene reinforced copper base composite material |
| CN105838913A (en) * | 2016-04-08 | 2016-08-10 | 上海和伍复合材料有限公司 | Graphene/nickel composite material and preparation method thereof |
| CN106226365A (en) * | 2016-08-11 | 2016-12-14 | 安徽省宁国天成电工有限公司 | A kind of graphene/copper composite material and its preparation method and application |
| CN106513694A (en) * | 2016-12-14 | 2017-03-22 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of graphene/ metal composite powder |
-
2018
- 2018-05-09 CN CN201810437448.8A patent/CN109277560A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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