CN106521208A - Method for preparing copper-graphene composite material - Google Patents
Method for preparing copper-graphene composite material Download PDFInfo
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- CN106521208A CN106521208A CN201610994624.9A CN201610994624A CN106521208A CN 106521208 A CN106521208 A CN 106521208A CN 201610994624 A CN201610994624 A CN 201610994624A CN 106521208 A CN106521208 A CN 106521208A
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- copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention discloses a method for preparing a copper-graphene composite material. Polyacrylamide is added in the mixing process of a copper-based material and graphene, so the copper-based material and graphene mixing uniformity is greatly improved, segregation is difficult, the copper-based material and graphene wet each other, the interface combination force is enhanced, prevention of crack expansion in the impact process is facilitated, and stress concentration is alleviated. The prepared composite material has excellent performances; and the preparation method has the advantages of simplicity and low cost.
Description
Technical field
It is an object of the invention to provide a kind of preparation method of copper-graphite alkene composite
Background technology
Powder surface modification is with organic or inorganic chemical assistant as modifying agent, by modifying agent in granule or particle aggregation
The covering in body surface face, makes the functional group of modifying agent be attached to particle surface, thus changes the wettability of particle surface.Solid is in powder
Acted on by a large amount of mechanical energy during broken, in addition to being consumed in grain refine, some is used to change these energy
Become the lattice and surface texture of granule, so as to activity raising, the enhanced activation phenomenon of alternate respond is presented, using mechanical force
Chemical effect carries out the technique of powder surface modification and is referred to as mechanical-chemical modification, and it is generally considered at present most to have now and sends out
One of high effective and modified method of exhibition prospect.
Graphene is the single layer structure of graphite, relative to graphite, with more excellent heat conduction, conductive and mechanical properties.
The characteristics of copper and copper alloy also have preferable electrical and thermal conductivity, corrosion resistance and are easy to molding.But Graphene and Copper substrate
Completely different physicochemical properties, are difficult to mix with powder metallurgic method, and produce segregation, and the two is mutually nonwetting, interface knot
It is poor to close, and is susceptible to reunite, causes the hydraulic performance decline of composite.
CN104862512A discloses Graphene and Copper substrate adhesion in a kind of raising copper-base graphite alkene composite
Method, the method utilize discharge plasma sintering skill by adding a small amount of alloying element in Copper substrate, after mixing with Graphene
Art is obtained composite.Experiment confirms to the method increase the interface binding power of matrix and Graphene enhancing phase in composite,
Compared with without the composite obtained by alloying element, with high tensile resistance.In addition, added through optimization
The quality of the amount and Graphene of alloying element, can obtain having the cuprio stone of excellent conduction, heat conduction and anti-wear performance concurrently
Black alkene composite, therefore have a good application prospect.
CN103773985A is passed through hydrogen by copper powder is placed in plasma enhanced chemical vapor deposition vacuum equipment
Gas, and being incubated at high temperature, then it is passed through argon and carbon-source gas are deposited, after deposition terminates, stopping is passed through carbon-source gas, most
After be cooled to below room temperature, obtain Graphene/copper composite powder, then by Graphene/copper composite powder first pressing, sintering and it is multiple press,
Obtaining Graphene strengthens Cu-base composites.
CN105965025A by set up outside the aerochamber of traditional fuel pulverizing plant many gas circuit Controllable Income Air systems with can
Control air-washer, temperature regulating device step by step and material deceleration device are set up inside aerochamber, make high-temperature liquid state copper in high velocity air
Percussion under, be atomized as after the small copper drop of high temperature, enter the aerochamber atmosphere containing certain proportion carbon-source gas composition
It is interior so that the copper drop of atomization realizes that grapheme material exists under temperature control process of setting and/or material deceleration device decelerating effect
The in-stiu coating growth on copper powder particle surface, finally obtains novel high-strength, the high Graphene Cu-base powder composite led.
After technical scheme disclosed in CN105908007A is by graphene powder, MAX phase ceramics powder body and copper powder mix homogeneously,
Hot pressed sintering is carried out, Graphene-carbon/carbon-copper composite material is obtained.
The universal complex operation of existing method, or the expensive raw material price for using, the performance of product are also not fully up to expectations.
The content of the invention
It is an object of the invention to overcoming, copper-graphite alkene composite material interface bond strength is high, the problem that wettability is poor,
There is provided a kind of preparation process simple, can method that effectively modified graphene surface prepares copper-graphite alkene composite.
The technical solution used in the present invention is：
A kind of preparation method of copper-graphite alkene composite, comprises the steps：
1) graphene dispersing solution, copper-based material powder, appropriate polyacrylamide gel and water are mixed, ball milling fully, obtains ball
Abrasive material；
2) appropriate polyacrylamide solution is added in ball milling material, carry out pugging；
3) by clay drying after the completion of pugging, crush, obtain powder；
4) powder is placed in into mould, cold moudling obtains base substrate；
5) by base substrate in 450～600 DEG C of pre-burnings, make Elements Diffusion uniform, be warming up to 800～1000 DEG C of roastings afterwards, after cooling
Obtain pre-sintered body；
6) pre-sintered body is pressed again, the pressed compact for obtaining obtains section bar in 800～1000 DEG C of resinterings.
As the further improvement of said method, in copper-graphite alkene composite, the mass percent of Graphene is 1～
4%.
Used as the further improvement of said method, copper-based material powder is copper powder, at least one in copper alloy powder.Especially
, copper alloy powder is selected from tin bronze powder, copper-nickel alloy powder, brass powder.
Used as the further improvement of said method, the addition of polyacrylamide gel is (2～4) ml/g Graphenes.
Used as the further improvement of said method, the addition of polyacrylamide solution is (15～25) ml/100g ball millings
Material.
Used as the further improvement of said method, the concentration of polyacrylamide solution is (0.5～3.5) mol/L.
Used as the further improvement of said method, the pressure colded pressing and press again is independently not less than 1T/cm2。
Used as the further improvement of said method, pre-burning, roasting and resintering are carried out under reducing atmosphere protection.Especially
, the protective atmosphere of pre-burning, roasting and resintering is H2。
The invention has the beneficial effects as follows：
The inventive method is simple to operate, and raw material is easy to get, and cheaply, production efficiency is high, can be manufactured using existing production equipment.In stone
Adding polyacrylamide in black alkene powder body can make powder body that splendid dispersity is presented, and stabilization effect occurs in system.Poly- third
The amide groups and carboxyl of acrylamide have highly polar, easily form hydrogen bond, can improve graphenic surface activity, strengthen itself and cuprio
The interface bond strength of body, is conducive to the cracks can spread in prevention impact process, slows down stress concentration.
In the composite of the present invention, the characteristics of Graphene has high conductivity, good mechanical performance, copper and copper alloy
With preferable conductive and heat-conductive type, corrosion resistance and the characteristics of be easy to molding, by using polyacrylamide to graphene powder
Surface carries out mechanical-chemical modification, promotes which effectively to be combined with Copper substrate, prepares high-performance copper-graphene composite material.
The copper-graphite alkene composite that the inventive method is prepared, consistency are high, three-point bending resistance intensity >=200Mpa, and resistivity≤
12μΩ·m。
Operating process is tested using pug mill, and the strong mechanical force of the process produces fierce stirring action, can make
Polyacrylamide is fully dispersed in system, and the mechanical force being applied on Graphene produces Mechanochemical Effect, so as to promote
The carrying out that Graphene is reacted with polyacrylamide.This modified technique is simple and efficiency high, can successfully solve copper-graphite alkene
Composite material interface combines the problem of difference.The inventive method is applied to compound, its method of many Albatra metals and graphite alkene
With good adaptability.
Description of the drawings
Fig. 1～4 are the sintered sample scanning figure of embodiment 1～4 respectively.
Specific embodiment
A kind of preparation method of copper-graphite alkene composite, comprises the steps：
1) graphene dispersing solution, copper-based material powder, appropriate polyacrylamide gel and water are mixed, ball milling fully, obtains ball
Abrasive material；
2) appropriate polyacrylamide solution is added in ball milling material, carry out pugging；
3) by clay drying after the completion of pugging, crush, obtain powder；
4) powder is placed in into mould, cold moudling obtains base substrate；
5) by base substrate in 450～600 DEG C of pre-burnings, make Elements Diffusion uniform, be warming up to 800～1000 DEG C of roastings afterwards, after cooling
Obtain pre-sintered body；
6) pre-sintered body is pressed again, the pressed compact for obtaining obtains section bar in 800～1000 DEG C of resinterings.
As the further improvement of said method, in copper-graphite alkene composite, the mass percent of Graphene is 1～
4%.
Used as the further improvement of said method, copper-based material powder is copper powder, at least one in copper alloy powder.Especially
, copper alloy powder is selected from tin bronze powder, copper-nickel alloy powder, brass powder.
Graphene can be various types of Graphenes, including but not limited to heat-conducting type, conductivity type or thermal conductivity type stone
Black alkene.
The effect of polyacrylamide gel is to make Graphene mix homogeneously with copper-based material in mechanical milling process, can be with root
The consumption of polyacrylamide gel is adjusted according to specific mixing situation, Graphene is mixed with being more uniformly distributed with copper-based material
Close.Used as the further improvement of said method, the addition of polyacrylamide gel is (2～4) ml/g Graphenes.
Polyacrylamide solution is acted on beneficial to smash to mud, and its consumption equally can be adjusted according to practical situation accordingly
It is whole, it is beneficial to pugging.Used as the further improvement of said method, the addition of polyacrylamide solution is (15～25) ml/
100g ball milling material.
Used as the further improvement of said method, the concentration of polyacrylamide solution is (0.5～3.5) mol/L.
As known to those skilled, pressure is too small, then be unfavorable for obtaining the material of densification, therefore, permit in condition
Perhaps in the case of, pressure should be big as far as possible, to obtain more fine and close material.But under practical situation, pressure crosses conference pair
Mould causes to damage, and affects its service life.Consider, as the further improvement of said method, the pressure colded pressing and press again
Power is independently not less than 1T/cm2, more preferably 1～4T/cm2。
Used as the further improvement of said method, pre-burning, roasting and resintering are carried out under reducing atmosphere protection.Especially
, the protective atmosphere of pre-burning, roasting and resintering is H2。
With reference to embodiment, technical scheme is further illustrated.
In following examples, for the sake of conveniently comparing, if no special instructions, Graphene adds ultrasonic disperse in ethanol
45min obtains graphene dispersing solution, and in dispersion liquid, the amount of Graphene is 10g/100ml.If no special instructions, in embodiment
The addition of graphene dispersing solution is in terms of the quality of Graphene.
Certainly, the graphene dispersing solution for being obtained using additive method dispersion is also feasible, and Graphene is mixed with dispersant
Composition and division in a proportion can also be adjusted according to practical situation, as long as disperse can graphene uniform.
If no special instructions, all of pre-burning, roasting, resintering are in H2Carry out under protective atmosphere.
Embodiment 1
1) graphene dispersing solution 1g is taken, adds copper powder 99g, 3ml polyacrylamide gel and suitable quantity of water to be put into ball milling in ball mill
Mixing 6h, obtains ball milling material；
2) in ball milling material, add the polyacrylamide solution of 20ml 0.5mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 2T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 830 DEG C of roasting 90min afterwards in 500 DEG C of pre-burning insulation 30min, cooling obtains pre-sintered body；
5) by pre-sintered body in 2T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 830 DEG C of resintering 90min.
Embodiment 2
1) graphene dispersing solution 2g is taken, and stanniferous amount is added for tin bronze powder 98g, the 6ml polyacrylamide gel of 10wt% and is fitted
Amount water is put into ball milling mixing 6h in ball mill, obtains ball milling material；
2) in ball milling material, add the polyacrylamide solution of 20ml 1.5mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 2.5T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 840 DEG C of roasting 90min afterwards in 500 DEG C of pre-burning insulation 30min, cooling obtains pre-sintered body；
5) by pre-sintered body in 2.5T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 840 DEG C of resintering 90min.
Embodiment 3
1) graphene dispersing solution 3g is taken, copper-nickel alloy powder 97g, 9ml polyacrylamide gel and suitable quantity of water that nickel content is 5wt% is added
Ball milling mixing 6h in ball mill is put into, ball milling material is obtained；
2) in ball milling material, add the polyacrylamide solution of 20ml 2.5mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 3T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 850 DEG C of roasting 90min afterwards in 500 DEG C of pre-burning insulation 30min, cooling obtains pre-sintered body；
5) by pre-sintered body in 3T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 850 DEG C of resintering 90min.
Embodiment 4
1) take graphene dispersing solution 4g, zinc content is added for brass powder 96g, 12ml polyacrylamide gel of 15wt% and appropriate
Water is put into ball milling mixing 6h in ball mill, obtains ball milling material；
2) in ball milling material, add the polyacrylamide solution of 20ml 3.5mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 4T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 860 DEG C of roasting 90min afterwards in 550 DEG C of pre-burning insulation 30min, cooling obtains pre-sintered body；
5) by pre-sintered body in 4T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 860 DEG C of resintering 90min.
Embodiment 5
1) graphene dispersing solution 2g is taken, adds copper powder 98g, 3ml polyacrylamide gel and suitable quantity of water to be put into ball milling in ball mill
Mixing 6h, obtains ball milling material；
2) in ball milling material, add the polyacrylamide solution of 25ml 1.0mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 1T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 900 DEG C of roasting 50min afterwards in 600 DEG C of pre-burning insulation 20min, cooling obtains pre-sintered body；
5) by pre-sintered body in 1T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 950 DEG C of resintering 45min.
Embodiment 6
1) graphene dispersing solution 3.5g is taken, adds copper powder 96.5g, 4ml polyacrylamide gel and suitable quantity of water to be put in ball mill
Ball milling mixing 6h, obtains ball milling material；
2) in ball milling material, add the polyacrylamide solution of 15ml 1.5mol/L, drying and crushing after pugging to underflow shape to obtain
Powder；
3) powder is placed in mould, then in 2T/cm2Cold moudling under pressure, obtains base substrate；
4) base substrate is warming up to into 1000 DEG C of roasting 45min afterwards in 450 DEG C of pre-burning insulation 60min, cooling obtains pre-sintered body；
5) by pre-sintered body in 2T/cm2Pressed under pressure again, obtain pressed compact；
6) pressed compact is obtained into section bar in 1000 DEG C of resintering 30min.
Performance detection：
The sintered sample scanning figure of embodiment 1～4 is respectively as shown in figures 1-4.From Fig. 1～4, the inventive method is prepared into
The composite for arriving, feed distribution are uniform, do not have agglomeration.Illustrate that copper-graphite alkene composite material interface is combined by force, Copper base material
The compatibility of material and Graphene is high.
Performance test results are as shown in the table：
Explanation：
1) using drainage survey calculation consistency, experiment condition is room temperature for bulk density measurement；
2) tensile strength test uses universal testing machine, and specimen size is 6mm × 9.5mm, and experiment condition is room temperature；
3) bending strength test using U.S. Instron3369 material mechanical test machines determine, specimen size be 38mm × 6mm ×
3mm, loading speed 1.00000mm/min.Experiment condition is room temperature；
4) resistivity measurement adopts double bridge, and test size is 55mm × 5mm × 5mm.Experiment condition is room temperature；
5) anti-wear performance test is using M-2000 type ring block testing machines, specimen size 18mm × 18mm × 12mm.Experiment condition is
Room temperature；
6) Vickers hardness measurement adopts Vickers, pressure 1Kg, and dwell time 10s, experiment condition are room temperature.
It can be seen that, by carrying out mechanical-chemical modification to graphene powder surface using polyacrylamide, promote itself and copper
Matrix is effectively combined, can will be the characteristics of Graphene high conductivity, good mechanical performance and copper and copper alloy conductive and heat-conductive type, resistance to
Corrosivity and organically combine the characteristics of be easy to molding, prepare high-performance copper-graphene composite material.
Polyacrylamide be with the addition of in copper-graphite alkene composite, its network structure causes it easily to roll up face entanglement, can
Physical crosslinking is formed in the composite；And as surface modifier, the amide groups (- CONH of polyacrylamide2) and carboxyl (-
COOH) hydrogen bond is easily formed with highly polar again, can improve graphenic surface activity, strengthen which strong with the interface cohesion of matrix
Degree, is conducive to the cracks can spread in prevention impact process, slows down stress concentration.
The strong mechanical force of pugging process produces fierce stirring action, and polyacrylamide can be made fully to divide in system
Dissipate, the mechanical force being applied on Graphene produces Mechanochemical Effect, so as to promote Graphene with polyacrylamide reaction
Carry out.
Claims (10)
1. a kind of preparation method of copper-graphite alkene composite, comprises the steps：
1）Graphene dispersing solution, copper-based material powder, appropriate polyacrylamide gel and water are mixed, ball milling fully, obtains ball
Abrasive material；
2）Appropriate polyacrylamide solution is added in ball milling material, pugging is carried out；
3）By clay drying after the completion of pugging, crush, obtain powder；
4）Powder is placed in into mould, cold moudling obtains base substrate；
5）By base substrate in 450～600 DEG C of pre-burnings, make Elements Diffusion uniform, be warming up to 800～1000 DEG C of roastings afterwards, after cooling
Obtain pre-sintered body；
6）Pre-sintered body is pressed again, the pressed compact for obtaining obtains section bar in 800～1000 DEG C of resinterings.
2. preparation method according to claim 1, it is characterised in that：In copper-graphite alkene composite, the quality of Graphene
Percentage ratio is 1～4%.
3. preparation method according to claim 1, it is characterised in that：Copper-based material powder is copper powder, in copper alloy powder
It is at least one.
4. preparation method according to claim 3, it is characterised in that：Copper alloy powder is selected from tin bronze powder, copper-nickel alloy powder, pyrite
Powder.
5. preparation method according to claim 1, it is characterised in that：The addition of polyacrylamide gel is（2～4）
Ml/g Graphenes.
6. preparation method according to claim 1, it is characterised in that：The addition of polyacrylamide solution is（15～25）
Ml/100g ball milling material.
7. preparation method according to claim 1, it is characterised in that：The pressure colded pressing and press again is independently not less than 1 T/
cm2。
8. preparation method according to claim 1, it is characterised in that：Pre-burning, roasting and resintering are protected in reducing atmosphere
Carry out under shield.
9. preparation method according to claim 1, it is characterised in that：The concentration of polyacrylamide solution is（0.5～3.5）
mol/L。
10. preparation method according to claim 1, it is characterised in that：The protective atmosphere of pre-burning, roasting and resintering is H2。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329976A (en) * | 2011-09-06 | 2012-01-25 | 上海交通大学 | Preparation method of graphene reinforced metal-matrix composite |
| CN104310388A (en) * | 2014-10-15 | 2015-01-28 | 宁波墨西科技有限公司 | Graphene composite powder material and preparation method thereof |
| CN104862512A (en) * | 2015-04-21 | 2015-08-26 | 中国科学院宁波材料技术与工程研究所 | Method for improving graphene and copper basal body binding force in copper-based graphene composite material |
-
2016
- 2016-11-11 CN CN201610994624.9A patent/CN106521208B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329976A (en) * | 2011-09-06 | 2012-01-25 | 上海交通大学 | Preparation method of graphene reinforced metal-matrix composite |
| CN104310388A (en) * | 2014-10-15 | 2015-01-28 | 宁波墨西科技有限公司 | Graphene composite powder material and preparation method thereof |
| CN104862512A (en) * | 2015-04-21 | 2015-08-26 | 中国科学院宁波材料技术与工程研究所 | Method for improving graphene and copper basal body binding force in copper-based graphene composite material |
Non-Patent Citations (1)
| Title |
|---|
| BINGWEI WEI ET AL；: "Synthesis and Physical Properties of Graphene Nanosheets Reinforced Copper Composites", 《ADVANCED MATERIALS RESEARCH》 * |
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