CN103938011A - Graphene/metal-based composite material with heat conduction anisotropy and electric conduction anisotropy and preparation method thereof - Google Patents
Graphene/metal-based composite material with heat conduction anisotropy and electric conduction anisotropy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene/metal-based composite material with heat conduction anisotropy and electric conduction anisotropy. The composite material uses a metal material as a matrix in which graphene is mixed, the graphene is uniformly dispersed in the metal matrix and a layered texture structure is presented, so that the composite material has the heat conduction anisotropy and electric conduction anisotropy, and the composite material has a commercial application value. The invention also provides a method for rapidly preparing the composite material at a low temperature. High-purity ultrafine metal powder and graphene water suspension solutions are used as raw materials, and electric spark ion sintering is carried out after high-speed ball milling, drying and prepressing molding of the raw materials, so that the sintering temperature of the composite material is greatly reduced, and the preparation rate is increased; in addition, certain exerted pressure is controlled in the process of sintering, so that the graphene is textured in the metal matrix, and the compact and uniform composite material with the heat conduction anisotropy and electric conduction anisotropy is prepared simply and conveniently at a low cost.
Description
Technical field
The present invention relates to metal-base composites technical field, relate in particular to the Graphene/metal composite of a kind of heat conduction and electric anisotropy and a kind of method that low temperature is prepared this matrix material fast.
Background technology
The fast development of modern science and technology, makes the design of instrument, equipment, parts and produces to be more and more tending towards miniaturization, lightweight, densification, high efficiency.The particularly development of super large-scale integration, makes the power density of electron device more and more higher, causes producing a large amount of heat in working process, and these heats, as got rid of not in time, will badly influence job stability and the safe reliability of electronic device part.Therefore, thermally conductive material choose the attention that more and more causes people, use highly heat-conductive material can significantly reduce device inside or surface temperature as heat sink or radiating element, also can utilize efficiently, economically heat, thereby there is important practical significance simultaneously.
From making at present for, metallic substance such as copper, silver because thering is good heat conductivility by generally as thermally conductive material.But single metallic substance is often limited because of performance inferior position in a certain respect to use, as high in metallic copper thermal expansivity, is often limited as heat sink material.Therefore, metal-base composites more and more causes concern.By adding of second-phase, in the performance speciality while of bringing into play to greatest extent metal, give single metal material not available premium properties, as high specific strength, high-modulus, high tenacity, high heat-conductivity conducting, the good over-all properties such as the coefficient of expansion is little, wear resistance good, hot strength is high, surface stability is good, it is had a wide range of applications in fields such as aerospace system, national defence, electronic industries.
In recent years, the research of preparing metal-base composites as second-phase with carbon material is increasingly extensive, because carbon material is a kind of very magical material, it both can form the very soft graphite of quality, can also form the hardest in the world diamond, when unique Atomic Arrangement has been given the various allotropic substance of carbon, also given the physical and mechanical properties of the various excellences of carbon material.Wherein, the thermal conductivity of carbon material, higher than metallic substance several times, becomes very excellent enhanced thermal conduction phase; And the conductive capability of carbon material is very superior, make it can be used as adjusting phase.Therefore, be hot subject always, and obtained a lot of achievements about the research of carbon material, it is comprising the research of the metal-base composites that carbon material is strengthened, but the wild phase of research is mainly carbon fiber and carbon nanotube at present.
In carbon material family, Graphene has two dimensional crystal structure, carbon atom intensive by one deck, that have hexagon honeycomb crystalline structure forms, thickness is probably 0.335nm, between carbon atom, with sp2 orbital hybridization, be connected, be that chemical bond between carbon atom is very strong σ key, these very strong covalent linkage make Graphene have very high intensity.The special construction of Graphene makes it show extremely excellent physicals and mechanical property.As, Graphene has higher electroconductibility, physical strength and thermal conductivity, and its intensity is the highest in known materials, can reach 130GPa, is more than 100 times of steel, Young's modulus is 1100GPa, suitable with carbon nanotube; Its thermal conductivity is 5000W.m
-1.K
-1, be adamantine 3 times.Based on above these good performances, make Graphene become one of material of tool prospect of 21 century.
Summary of the invention
Technical purpose of the present invention is to provide the Graphene/metal composite of a kind of heat conduction and electric anisotropy, and composite material compositions is even, has each diversity of heat conduction and each diversity of conduction.
The present invention realizes the technical scheme that above-mentioned technical purpose adopts: the Graphene/metal-base composites of a kind of heat conduction and electric anisotropy, take metallic substance as matrix, it is at doped graphene, and described Graphene is laminated structure and interts in metallic matrix.
The per-cent that the Graphene of telling accounts for matrix material is 1%～50%, more preferably 5%～20%.
Described metal-powder is a kind of and the Graphene simple substance powder of the metallic element of react with not in the periodic table of elements, or the mixed powder of the different proportionings of several these metalloid elements, include but not limited to one or more the mixture in the metals such as gold and silver, platinum, copper
Described Graphene/metal-base composites has anisotropic heat conductivity and electric anisotropy.
The present invention also provides a kind of low temperature to prepare fast the method for the Graphene/metal composite of above-mentioned heat conduction and electric anisotropy, it is raw material that the method adopts metal-powder and the Graphene aqueous suspension solution of high pure and ultra-fine, using dehydrated alcohol as medium, raw material is carried out in medium to high speed ball milling, obtain the mixed uniformly slurry of Graphene and metal-powder; Then, this slurry, through vacuum-drying, screening, obtains Graphene and the mixed uniformly composite granule of metal-powder; Then; this composite granule is packed in graphite jig; pre-molding under 10～100MPa pressure; put into again electrical spark ion agglomerating plant; in vacuum or be connected with under protective atmosphere condition, control and exert pressure and temperature rise rate, be heated to after sintering temperature; be incubated certain hour, obtain the sintering block of the Graphene/metal-base composites of heat conduction and electric anisotropy
In above-mentioned preparation method, will after Graphene and the mixed uniformly composite granule pre-molding of metal-powder, carry out electrical spark ion sintering.Electrical spark ion sintering is a kind of advanced person's electric field assisted sintering mode, can melt and seam by the district of the induction particle that sparks between conducting metal particles, and under certain high temperature, promote the mutual diffusion of atoms metal to produce constriction, and eliminate micro-pore of triangle grain boundaries, realize densification.Therefore, this sintering processing heats up fast, and the sintering of current field assistant metal particle can be provided, and the sintering of metal species material is had to advantageous advantage, can significantly reduce sintering temperature, at the temperature lower than 500～1000 ℃ of melting point metals, realize the full densification sintering of metal.
Above-mentioned preparation method's innovation is to adopt the electrical spark ion sintering technology low temperature preparation Graphene/metal-base composites with heat conduction and electric anisotropy of the present invention fast just, composite granule until high speed ball milling carries out electrical spark ion sintering in graphite jig after coldmoulding, thereby significantly reduced the sintering temperature of metal-base composites, improved the preparation speed of metal-base composites, and in sintering process, control certain exerting pressure, make Graphene texturing in metallic matrix, thereby make the Graphene/metal-base composites of preparation there is each diversity of thermal conductivity, therefore there is good using value.
In above-mentioned preparation method, when raw material is carried out to high speed ball milling in medium, preferably adopt planetary ball mill method.Planetary ball mill method is to utilize rotation or the vibration of ball mill, makes hard sphere carry out strong shock, grinding and stirring to raw material, the homodisperse method of metal or alloy powder.Adopt planetary ball mill method, when the ball milling mouth that two or more metal or alloy powder is put into ball mill simultaneously carries out high-energy ball milling, due to powder particle through calendering, pressing, pulverize again, the repetitive process of pressing again, finally can obtain the powdered alloy that microstructure and composition is evenly distributed.
Purity and the granularity of high-purity superfine metal powder are not specifically limited, and as preferably, purity is greater than 99.5%, and size range is 0.1um～100um.
The concentration of Graphene aqueous suspension solution is not specifically limited, and as preferably, the volumn concentration of Graphene is 1vol%～10vol%, more preferably 5vol%.
When Graphene mixes with metal powder, mixing method is preferably wet ball-milling method, take dehydrated alcohol as medium.Material ball ratio, Ball-milling Time, rotating speed are not specifically limited, and ratio of grinding media to material is preferably 1:2～1:10,1:3 more preferably, and Ball-milling Time is preferably 5 hours～and 20 hours, more preferably 10 hours; Rotating speed is preferably 300 turn/min of turn/min～600.
Vacuum drying temperature is not specifically limited, and as preferably, temperature range is 40 ℃～120 ℃.
As preferably, the sieve of screening is 50 order～1000 orders.
In electrical spark ion agglomerating plant, during vacuum sintering, vacuum tightness is preferably 10
-4pa～1Pa.
In electrical spark ion agglomerating plant during sintering, temperature rise rate, pressure, sintering temperature, soaking time etc. are not specifically limited, as preferably, temperature rise rate is 1 ℃/min～700 ℃/min, exerts pressure as 10MPa～120MPa, sintering temperature are 600 ℃～2000 ℃, and soaking time is 1min～120min.
In electrical spark ion agglomerating plant, during sintering, the size shape of selected graphite jig is not specifically limited, and can design according to actual needs, and as preferably, die size scope is Φ 20mm～Φ 80mm.
In sum, the invention provides a kind of Graphene/metal-base composites of novel texture, in this matrix material, graphene uniform is dispersed in metallic matrix, wetting good with copper matrix, be texturing constitutional features, therefore having anisotropic heat conductivity and electric anisotropy, is a kind of matrix material that commercial applications is worth that has.Under cold condition provided by the invention, the method cost of this Graphene/metal-base composites of preparation is low fast, technique is simple, can access densification, even, has the Graphene/metal-base composites of each diversity of heat conduction and electric anisotropy.
Accompanying drawing explanation
Fig. 1 is the heat conduction that is 20mm of the diameter that adopts electrical spark ion sintering to make in the embodiment of the present invention 1 and Graphene/Cu-base composites block of electric anisotropy;
Fig. 2 is the fracture scanning electron microscope picture of block shown in Fig. 1;
Fig. 3 is the heat conduction that is 20mm of the diameter that adopts electrical spark ion sintering to make in the embodiment of the present invention 2 and Graphene/silver-based composite material block of electric anisotropy;
Fig. 4 is the fracture scanning electron microscope picture of block shown in Fig. 3.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
Embodiment 1:
The present embodiment provides a kind of Graphene/Cu-base composites, and this matrix material be take copper as matrix, doped graphene, Graphene content accounts for the 5wt% of matrix material, and graphene uniform is dispersed in copper matrix, be texturing constitutional features, this matrix material has heat conduction and electric anisotropy.
The preparation of above-mentioned Graphene/Cu-base composites is specific as follows:
The content that is 5wt% according to Graphene takes high pure and ultra-fine copper powder and Graphene aqueous suspension solution, selected high pure and ultra-fine copper powder, and granularity is about 1um, and purity is for being greater than 99.8%, and in selected Graphene aqueous suspension solution, Graphene content is 5vol%; Two kinds of materials are placed in to ball grinder, add dehydrated alcohol as medium, carry out high speed ball milling in high energy ball mill, material ball ratio is 1:6, and rotating speed is 300 turn/min, and Ball-milling Time is 10 hours; Composite mortar after ball milling is dried in vacuum drying oven, and the case vacuum tightness that keeps dry is 10
-2pa, temperature is 40 ℃, and dried powder is sieved through 200 object sieves, obtains the composite granule of Graphene and copper powder; Weigh certain composite granule and put into the graphite jig coldmoulding of Φ 20mm, exert pressure as 10MPa; Finally, the graphite jig after coldmoulding is put into electric field auxiliary electric spark ion sintering oven sintering, temperature rise rate is 50 ℃/min, exert pressure as 30MPa, sintering temperature is 850 ℃, to be sinteredly to sintering temperature, is incubated 5 minutes, whole sintering process is all carried out in a vacuum, and vacuum tightness is 10
-2pa, it is 20mm that sintering obtains diameter, circular Graphene/Cu-base composites block that thickness is 5mm.
Fig. 1 is the above-mentioned Graphene/Cu-base composites block outside drawing making, and this block is even and fine and close, has bright golden colour lustre after mechanical polishing; The density that records this block through Archimedes's method is 7.234g/cm
3, relative density reaches 97.1%; Through scanning electron microscopic observation, determine that in this block, Graphene is uniformly dispersed, show certain stratiform texturing, as shown in Figure 2.
The heat conduction of the above-mentioned Graphene/Cu-base composites block making, conductive test result show, in temperature, be under 300k, the thermal conductivity of its vertical axis direction is 182.954W/ (m*K), the thermal conductivity of the direction that parallels to the axis is 110.874W/ (m*K), shows the feature of anisotropic heat conductivity; In temperature, be under 273k, the resistivity of vertical axis direction is 3.794 * 10
-8Ω m, the direction that parallels to the axis resistivity is 1.855 * 10
-7Ω m, shows electric anisotropy equally.
Embodiment 2:
The present embodiment provides a kind of Graphene/silver-based composite material, and this matrix material be take silver as matrix, doped graphene, Graphene content accounts for the 10wt% of matrix material, and graphene uniform is dispersed in silver matrix, be texturing constitutional features, this matrix material has heat conduction and electric anisotropy.
The concrete preparation method of above-mentioned Graphene/silver-based composite material is as follows:
The content that is 10wt% according to Graphene takes high pure and ultra-fine silver powder and Graphene aqueous suspension solution, selected high pure and ultra-fine silver powder, and granularity is about 1um, and purity is for being greater than 99.5%, and in selected Graphene aqueous suspension solution, Graphene content is 5vol%; Two kinds of materials are placed in to ball grinder, add dehydrated alcohol as medium, carry out high speed ball milling in planetary ball mill, material ball ratio is 1:3, and rotating speed is 500 turn/min, and Ball-milling Time is 20 hours; Composite mortar after ball milling is dried in vacuum drying oven, and the case vacuum tightness that keeps dry is 10
-2pa, temperature is 60 ℃, and dried powder is sieved through 300 object sieves, obtains the composite granule of Graphene and silver powder; Weigh certain composite granule and put into the graphite jig coldmoulding of Φ 20mm, exert pressure as 20MPa; Finally, graphite jig after coldmoulding is put into electric field auxiliary electric spark ion sintering oven sintering, temperature rise rate is 60 ℃/min, exert pressure as 35MPa, sintering temperature is 800 ℃, to be sinteredly to sintering temperature, be incubated 10 minutes, whole sintering process is all carried out in a vacuum, and vacuum tightness is 10
-4pa, it is 20mm that sintering obtains diameter, circular Graphene/silver-based composite material block that thickness is 3mm.
Fig. 3 is the above-mentioned Graphene/silver-based composite material block outside drawing making, and this block is even and fine and close, has bright silvery white gloss after mechanical polishing; Through Archimedes's method, record the density 6.936g/cm of this block
3, relative density reaches 98.1%; Through scanning electron microscopic observation, determine that in this block, Graphene is uniformly dispersed, show certain stratiform texturing, as shown in Figure 4.
The heat-conductivity conducting test result of the above-mentioned Graphene/silver-based composite material block making shows, in temperature, be under 300k, the thermal conductivity of its vertical axis direction is 119.342W/ (m*K), the thermal conductivity of the direction that parallels to the axis is 60.808W/ (m*K), shows the feature of anisotropic heat conductivity; In temperature, be under 273k, the resistivity of vertical axis direction is 7.974 * 10
-8Ω m, the direction that parallels to the axis resistivity is 4.460 * 10
-7Ω m, shows electric anisotropy equally.
Embodiment 3:
The present embodiment provides a kind of Graphene/auri matrix material, and this matrix material be take gold as matrix, doped graphene, Graphene content accounts for the 15wt% of matrix material, and graphene uniform is dispersed in auri body, be texturing constitutional features, this matrix material has heat conduction and electric anisotropy.
The concrete preparation method of above-mentioned Graphene/auri matrix material is as follows:
The content that is 15wt% according to Graphene takes high pure and ultra-fine bronze and Graphene aqueous suspension solution, selected high pure and ultra-fine bronze, and granularity is 5um, and purity is for being greater than 99.9%, and in selected Graphene aqueous suspension solution, Graphene content is 5vol%; Two kinds of materials are placed in to ball grinder, add dehydrated alcohol as medium, carry out high speed ball milling in planetary ball mill, material ball ratio is 1:3, and rotating speed is 250 turn/min, and Ball-milling Time is 24 hours; Composite mortar after ball milling is dried in vacuum drying oven, and the case vacuum tightness that keeps dry is 10
-3pa, temperature is 100 ℃, and dried powder is sieved through 100 object sieves, obtains the composite granule of Graphene and bronze; Weigh certain composite granule and put into the graphite jig coldmoulding of Φ 20mm, exert pressure as 20MPa; Finally, graphite jig after coldmoulding is put into electric field auxiliary electric spark ion sintering oven sintering, to be sinteredly to sintering temperature, be incubated, temperature rise rate is 40 ℃/min, exert pressure as 25MPa, sintering temperature is 950 ℃, to be sinteredly to sintering temperature, is incubated 8 minutes, whole sintering process is all carried out in a vacuum, and vacuum tightness is 10
-3pa, it is 20mm that sintering obtains diameter, circular Graphene/auri matrix material block that thickness is 2mm.
Above-mentioned Graphene/auri matrix material the block making is even and fine and close, has bright golden colour lustre after mechanical polishing; The density that records this block through Archimedes's method is 7.473g/cm
3, relative density reaches 95.2%; Through scanning electron microscopic observation, determine that Graphene is uniformly dispersed, show good texturing pattern.
The heat-conductivity conducting the performance test results of the above-mentioned Graphene/auri matrix material block making shows, under 300k, the thermal conductivity of vertical axis direction is 140.798W/ (m*K), and the thermal conductivity of the direction that parallels to the axis is 68.226W/ (m*K), shows the feature of anisotropic heat conductivity; Under 273k, the resistivity of vertical axis direction is 9.822 * 10
-8Ω m/, the direction that parallels to the axis resistivity is 8.731 * 10
-7Ω m, shows electric anisotropy equally.
Embodiment 4:
The present embodiment provides a kind of graphene/platinum based composites, and this matrix material be take platinum as matrix, doped graphene, Graphene content accounts for the 10wt% of matrix material, and graphene uniform is dispersed in platinum matrix, be texturing constitutional features, this matrix material has heat conduction and electric anisotropy.
The concrete preparation method of above-mentioned graphene/platinum based composites block is as follows:
The content that is 10wt% according to Graphene takes high pure and ultra-fine platinum powder and Graphene aqueous suspension solution, selected high pure and ultra-fine platinum powder, and granularity is 2um, and purity is for being greater than 99.9%, and in selected Graphene aqueous suspension solution, Graphene content is 5vol%; Two kinds of materials are placed in to ball grinder, add dehydrated alcohol as medium, carry out high speed ball milling in planetary ball mill, material ball ratio is 1:3, and rotating speed is 300 turn/min, and Ball-milling Time is 20 hours; Composite mortar after ball milling is dried in vacuum drying oven, and the case vacuum tightness that keeps dry is 10
-3pa, temperature is 80 ℃, and dried powder is sieved through 100 object sieves, obtains the composite granule of Graphene and platinum powder; Weigh certain composite granule and put into the graphite jig coldmoulding of Φ 20mm, exert pressure as 20MPa; Finally, graphite jig after coldmoulding is put into electric field auxiliary electric spark ion sintering oven sintering, to be sinteredly to sintering temperature, be incubated, temperature rise rate is 25 ℃/min, exert pressure as 30MPa, sintering temperature is 1550 ℃, to be sinteredly to sintering temperature, is incubated 20 minutes, whole sintering process is all carried out in a vacuum, and vacuum tightness is 10
-3pa, it is 20mm that sintering obtains diameter, the circular graphene/platinum based composites block that thickness is 3mm.
The above-mentioned graphene/platinum based composites block making is even and fine and close, has bright silvery white gloss after mechanical polishing; The density that records this block through Archimedes's method is 9.861g/cm
3, relative density reaches 96.3%; Through scanning electron microscopic observation, determine that Graphene is uniformly dispersed, show good texturing pattern.
Its heat-conductivity conducting the performance test results of the above-mentioned Graphene/auri matrix material block making shows, under 300k, the thermal conductivity of vertical axis direction is 28.362W/ (m*K), and the thermal conductivity of the direction that parallels to the axis is 13.696W/ (m*K), shows the feature of anisotropic heat conductivity; Under 273k, the resistivity of vertical axis direction is 8.914 * 10
-7Ω m/, the direction that parallels to the axis resistivity is 6.539 * 10
-6Ω m, shows electric anisotropy equally.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making within the scope of principle of the present invention, supplement or similar fashion substitutes etc., within all should being included in protection scope of the present invention.
Claims (10)
1. Graphene/metal-base composites of heat conduction and electric anisotropy, is characterized in that: take metallic substance as matrix, and doped graphene wherein, described Graphene is laminated structure and interts in metallic matrix.
2. Graphene/the metal-base composites of heat conduction as claimed in claim 1 and electric anisotropy, is characterized in that: the degree that described Graphene accounts for matrix material is 1%～50%.
3. Graphene/the metal-base composites of heat conduction as claimed in claim 1 and electric anisotropy, is characterized in that: the degree that described Graphene accounts for matrix material is 5%～20%.
4. Graphene/the metal-base composites of heat conduction as claimed in claim 1 and electric anisotropy, is characterized in that: described metal comprises gold and silver, platinum, copper, and one or more mix in the metal not reacting with Graphene.
5. the preparation method of the Graphene/metal-base composites of the heat conduction as described in arbitrary claim in claim 1 to 4 and electric anisotropy, it is characterized in that: adopting metal-powder and the Graphene aqueous suspension solution of high pure and ultra-fine is raw material, first, using ethanol solution as medium, raw material is carried out in medium to high speed ball milling, obtain the mixed uniformly slurry of Graphene and metal-powder; Then, this slurry, through vacuum-drying, screening, is obtained to the mixed uniformly composite granule of Graphene and metal-powder; Then; this composite granule is packed in graphite grinding tool; pre-molding under 10～100MPa pressure; put into again electrical spark ion agglomerating plant; in vacuum or be connected with under protective atmosphere condition; control is exerted pressure and temperature rise rate, is heated to be incubated certain hour after sintering temperature, obtains the sintering block of the Graphene/metal-base composites of heat conduction and electric anisotropy.
6. the preparation method of the Graphene/metal-base composites of heat conduction as claimed in claim 5 and electric anisotropy, is characterized in that: when raw material is carried out to high speed ball milling in medium, adopt planetary ball mill method.
7. the preparation method of the Graphene/metal-base composites of heat conduction as claimed in claim 5 and electric anisotropy, is characterized in that: the granularity of described metal-powder is 0.1um～100um.
8. the preparation method of the Graphene/metal-base composites of heat conduction as claimed in claim 5 and electric anisotropy, is characterized in that: the Graphene content of described Graphene aqueous suspension solution is 1vol%～10vol%.
9. the preparation method of the Graphene/metal-base composites of heat conduction as claimed in claim 5 and electric anisotropy, is characterized in that: described temperature rise rate is that 1 ℃/min～700 ℃/min, sintering temperature are 600 ℃～2000 ℃.
10. the preparation method of the Graphene/metal-base composites of heat conduction as claimed in claim 5 and electric anisotropy, is characterized in that: described exerts pressure as 10MPa～120MPa.
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| CN105385877A (en) * | 2015-11-09 | 2016-03-09 | 昆明贵金属研究所 | Novel silver-based electrical contact composite material and preparing method thereof |
| CN105624446A (en) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | Graphene-reinforced magnesium-aluminium matrix composite material and preparation method thereof |
| CN105803244A (en) * | 2016-04-07 | 2016-07-27 | 北京卫星环境工程研究所 | Space multi-factor environment comprehensive protection material and protection structure |
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| CN105385877A (en) * | 2015-11-09 | 2016-03-09 | 昆明贵金属研究所 | Novel silver-based electrical contact composite material and preparing method thereof |
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Application publication date: 20140723 |