CN104831100A - Method for preparing graphene reinforced metal-based composite material through discharge plasma (SPS) sintering - Google Patents
Method for preparing graphene reinforced metal-based composite material through discharge plasma (SPS) sintering Download PDFInfo
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Abstract
The present invention relates to a method for preparing a graphene reinforced metal-based composite material through discharge plasma (SPS) sintering. The method is characterized in that the graphene reinforced metal-based block material is prepared through SPS sintering and has the following advantages that: the preparation method is simple, the material is compact and does not have pores, the graphene mass fraction can be arbitrarily regulated, the distribution is uniform, no aggregation is generated, the material mechanical property isotropy is provided, and the wettability of the metal and the graphene interface is good. The method comprises: (1) reducing graphene oxide through a chemical method or a hydrothermal method to obtain graphene sheets with a sheet layer thickness of not more than 4 nm and sheet layer diameter of not more than 50 [mu]m; and (2) preparing metal powder with a particle size of not more than 200 [mu]m through a rotating electrode atomization method, mechanical crushing or a high-speed ball milling method; (3) carrying out mechanical or ball milling mixing on the graphene powder and the metal powder according to the required mass ratio; and (4) carrying out SPS sintering forming on the mixed powder, wherein the obtained material has characteristics of improved mechanical property, decreased density, good heat conduction capability, and good electric conduction capability, and the performance customizing can be achieved by adjusting the preparation parameters.
Description
Technical field
The present invention relates to the method that a kind of plasma discharging (SPS) sintering prepares graphene reinforced metal-matrix composite, particularly relate to a kind of preparation method of compact metal based composites of high Graphene content.
Background technology
Graphene is a kind of two dimensional surface carbonaceous material being become cellular crystalline network by monolayer carbon atom packing, lamellar spacing is less than 10 carbon atoms usually, and have excellent mechanics and conductive and heat-conductive characteristic, intensity is 125GPa, Young's modulus is 1100GPa, and electronic mobility reaches 200000cm
2/ VS, thermal conductivity reaches 5000w/mK, has low density feature simultaneously.Graphene sheet layer is added to the density that can reduce material in metallic matrix, and expection can obtain high strength and keep good conduction, the capacity of heat transmission, for some particular alloy or pure metal, adding of Graphene even can make material possess some property and become functional materials, inhales ripple, damping and the performance such as wear-resisting as possessed.Graphene reinforced metal-matrix composite has vast potential for future development.
Existing research of being correlated with and the preparation that patent reports graphene reinforced metal-matrix composite, the main method of current employing is casting and hot isostatic pressing (hot pressing) sintering, but these two kinds of method defects are obvious: because Graphene differs larger with liquid metal density, Graphene skewness in cast material, easy reunion, is difficult to obtain the homogeneous material of performance; And pre-treatment prepared by hot pressed sintering is very complicated, surface modification to be carried out to metal-powder, also requirement is had to the shape of metal-powder, generally be only applicable to flaky metal powder, and the temperature of sintering is high, applied pressure is large, and sintering time is also very long wants several to dozens of hours usually, therefore energy consumption is very big, and the matrix material porosity obtained is also very high.Due to Graphene neither hydrophilic also not oleophylic, reactive behavior is not high, surface wettability is very poor, and there is huge nature difference between metal, be difficult to realize interface cohesion with metallic matrix, therefore the addition of Graphene is also restricted, limited to the lifting of metallic substance performance, and traditional powder blending means employing is li quid mixing method, complex process, the content of Graphene also cannot accurately control.
Summary of the invention
The object of the invention is to the deficiency for existing technology of preparing, a kind of method of the metal-base composites by the high Graphene content of plasma discharging (SPS) sintering preparation is provided.The present invention take metal-powder as matrix, with the graphene sheet layer powder of two dimension for strongthener, prepare closely knit Graphene content can arbitrarily, the metal-base composites of accuracy controlling.
The present invention is achieved by the following technical solutions:
1. a graphene reinforced metal-matrix composite for plasma discharging (SPS) sintering preparation, the massfraction of Graphene can reach more than 10%, and can regulate and control mass percent arbitrarily, accurately.
2. the thickness of graphene sheet layer used is not more than 4nm, and lamella diameter is not more than 50 μm.
3. metal-powder used can be the powder of spherical powder or other arbitrary shapes, and powder diameter is not more than 200 μm, and raw materials used can be the pure metal of aluminium, magnesium, titanium, copper, iron, nickel etc., or its one or more alloys.
4. the step adopting SPS to sinter graphene reinforced metal-matrix composite described in preparation 1 is:
(1) by hummers legal system for graphite oxide, after ultrasonic disperse, cleaning, filtration, drying, high speed ball milling, obtains graphene oxide powder, hydrothermal method, chemical reduction method, hightemperature gas-phase reduction or metal powder reduction method can be adopted to reduce and obtain graphene powder; Also can vapour deposition again ball milling obtain graphene powder.
(2) adopt in rotating electrode atomized method, mechanical crushing method or high speed ball milled any one prepare the metal-powder that particle diameter is less than 200 μm.
(3) take graphene powder and metal-powder according to required quality proportioning and mix, adopt the further homogenizing of mode of ball milling or mechanically mixing, rotating speed is 200-300r/min, mixing time 30-60min.
(4) Graphene-composite metal powder mixed is loaded in graphite jig, carry out SPS sinter molding, sintering parameter: sintering pressure is 40Mpa, current switching (on/off) is than being 4:1 (32ms/8ms), temperature rise rate is 50 DEG C/min, 1min is incubated, water-cooled cooling after arriving final sintering temperature.Final sintering temperature is determined according to the kind of metal, should lower than the fusing point 150-300 DEG C of pure metal used or alloy.
Advantage of the present invention is: (1) can prepare the metal-base composites of high Graphene content, and the massfraction of Graphene can reach more than 10%, and can arbitrarily, accuracy controlling.(2) preparation technology is simply efficient, to the source of Graphene without particular requirement, does not also need to carry out pre-treatment; To the particle diameter of metal-powder and shape without particular requirement, do not need to carry out surface modification treatment yet.(3) can adjust the size of the particle diameter of metal-powder and graphene sheet layer, realize the preparation of the matrix material of different degree of scatter.(4) Graphene and metal-powder carry out physical mechanical under drying regime to mix, and not easily produces the agglomeration of solution dispersion, and graphene powder is uniformly distributed and in a metal without specific orientation, the homogeneous isotropy of performance of matrix material.(5) during SPS sintering, effective electric discharge between metal-powder and Graphene can produce localized hyperthermia makes metal-powder local melting, also graphenic surface can be made to produce activation, under high-temperature plasma sputtering, discharge impact and electric field acceleration effect, make metallic matrix and Graphene interface produce atomic diffusion to be connected, realize good interface cohesion.(6) temperature of SPS sintering is lower, lower than melting point metal 150-300 DEG C, little on the impact of metal and Graphene, and sintering time is short simultaneously, and whole sintering process is less than half an hour, and energy consumption is low.(7) the metal or alloy kind that sintering method is applicable is many, substantially goes for any solid metal.
Accompanying drawing explanation
The massfraction of Fig. 1 Graphene powder is the SEM image of 7055 Al alloy composites of 4%
The compound shape appearance figure of Fig. 2 monolithic graphite alkene in 7055 aluminium alloys, graphene sheet layer is that atomic diffusion is combined with 7055 aluminium alloy interfaces, and interface cohesion is good
The power spectrum line sweep result of Fig. 3 graphene sheet layer and 7055 alloy matrix aluminums
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
embodiment 1
Choose 7055 Al alloy powders of particle diameter 50 μm, ball milling 45min, after ball milling, powder is loaded in graphite jig and carry out SPS sintering, sintering parameter: pressure is 40MPa, sintering temperature is 400 DEG C, and temperature rise rate is 50 DEG C/min, 400 DEG C of isobaric insulation 1min, current switching is than being 4:1, and insulation terminates water-cooled.Obtain 7055 aluminium alloy blocks of fine and close not graphene-containing, be numbered 1# sample
embodiment 2
According to the mass ratio of 1:49 by 7055 Al alloy powder Homogeneous phase mixing of graphene powder and particle diameter 50 μm, ball milling 45min; Loaded in graphite jig by the composite powder mixed and carry out SPS sintering, sintering parameter: pressure is 40MPa, and sintering temperature is 400 DEG C, and temperature rise rate is 50 DEG C/min, 400 DEG C of isobaric insulation 1min, current switching is than being 4:1, and insulation terminates water-cooled.Obtain the 7055 Al-alloy based matrix materials that fine and close Graphene massfraction is 2%, be numbered 2# sample.
embodiment 3
According to the mass ratio of 1:24 by 7055 Al alloy powder Homogeneous phase mixing of graphene powder and particle diameter 50 μm, ball milling 45min; Loaded in graphite jig by the composite powder mixed and carry out SPS sintering, sintering parameter: pressure is 40MPa, and sintering temperature is 400 DEG C, and temperature rise rate is 50 DEG C/min, 400 DEG C of isobaric insulation 1min, current switching is than being 4:1, and insulation terminates water-cooled.Obtain the 7055 Al-alloy based matrix materials that fine and close Graphene massfraction is 4%, be numbered 3# sample.
embodiment 4
According to the mass ratio of 3:47 by 7055 Al alloy powder Homogeneous phase mixing of graphene powder and particle diameter 50 μm, ball milling 45min; Loaded in graphite jig by the composite powder mixed and carry out SPS sintering, sintering parameter: pressure is 40MPa, and sintering temperature is 400 DEG C, and temperature rise rate is 50 DEG C/min, 400 DEG C of isobaric insulation 1min, current switching is than being 4:1, and insulation terminates water-cooled.Obtain the 7055 Al-alloy based matrix materials that fine and close Graphene massfraction is 6%, be numbered 4# sample.
embodiment 5
According to the mass ratio of 2:23 by 7055 Al alloy powder Homogeneous phase mixing of graphene powder and particle diameter 50 μm, ball milling 45min; Loaded in graphite jig by the composite powder mixed and carry out SPS sintering, sintering parameter: pressure is 40MPa, and sintering temperature is 400 DEG C, and temperature rise rate is 50 DEG C/min, 400 DEG C of isobaric insulation 1min, current switching is than being 4:1, and insulation terminates water-cooled.Obtain the 7055 Al-alloy based matrix materials that fine and close Graphene massfraction is 8%, be numbered 5# sample.
The above embodiment only have expressed several embodiments that the present invention is directed to 7055 aluminium alloys, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.
The fundamental characteristics of 7055 Al-alloy based matrix materials of table 1 different Graphene content
| Sample number into spectrum | Graphene content (wt, %) | Density (g/cm 3) | Hardness (HV) | Specific conductivity (MS/m) |
| 1# | 0 | 2.823 | 100.39 | 24.6 |
| 2# | 2 | 2.775 | 127.79 | 23.7 |
| 3# | 4 | 2.729 | 143.33 | 23.3 |
| 4# | 6 | 2.692 | 153.11 | 23.0 |
| 5# | 8 | 2.678 | 159.56 | 22.7 |
Claims (5)
1. a plasma discharging (SPS) sintering prepares the method for graphene reinforced metal-matrix composite, it is characterized by and graphene powder is mixed with metal-powder machinery (ball milling), obtained the metal matrix block composite material of fine and close Graphene enhancing by SPS sintering.
2. a kind of SPS sintering as claimed in claim 1 prepares the method for graphene reinforced metal-matrix composite, it is characterized by and comprises following methods step:
(1) by hummers legal system for graphite oxide, after ultrasonic disperse, cleaning, filtration, drying, high speed ball milling, obtains graphene oxide powder, hydrothermal method, chemical reduction method, hightemperature gas-phase reduction or metal powder reduction method can be adopted to reduce and obtain graphene powder; Also can vapour deposition again ball milling obtain graphene powder;
(2) metal-powder of the required pure metal of preparation or alloy;
(3) graphene powder prepared and metal-powder are mixed according to required quality proportioning, adopt without abrading-ball mechanically mixing or ball milling mixing, rotating speed is 200-300r/min, mixing time 30-60min;
(4) Graphene-composite metal powder mixed is loaded in graphite jig, carry out SPS sinter molding, sintering parameter: sintering pressure is 40Mpa, current switching (on/off) is than being 4:1 (32ms/8ms), and temperature rise rate is 50 DEG C/min, is incubated 1min after arriving final sintering temperature, water-cooled cooling, from mould, take out block composite material, final sintering temperature is determined according to the kind of metal, should lower than the fusing point 150-300 DEG C of pure metal used or alloy.
3. graphene oxide high speed ball milling parameter is as described in claim 2: ball grinder and abrading-ball are stainless steel or agate material, and ratio of grinding media to material is 20-30:1, and rotating speed is 300-600r/min, and Ball-milling Time is 2-6h.
4. metallic matrix can be the pure metal such as aluminium, magnesium, titanium, iron, copper, nickel as described in claim 2, also can be one or more in above metal alloy.
5. as described in claim 2 metal powder preparation method comprises rotating electrode atomized method, mechanical crushing method and high-energy ball milling method, and metal-powder can be spherical, sheet and irregularly shaped, and particle diameter is not more than 200 μm.
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Application publication date: 20150812 |