CN106978149A - The preparation method and heat sink material of light high heat conducting graphene-based heat sink material containing aluminium - Google Patents
The preparation method and heat sink material of light high heat conducting graphene-based heat sink material containing aluminium Download PDFInfo
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Abstract
Requirement for aerospace field to heat sink material light high heat conducting, the present invention proposes the preparation method and heat sink material of a kind of light high heat conducting graphene-based heat sink material containing aluminium, the invention solves the problems that the formation problems of graphene and aluminium composite material.Method：Prepare aluminium powder dispersion liquid；Prepare graphene dispersing solution；Aluminium powder dispersion liquid is mixed with graphene dispersing solution；Freeze-drying prepares mixed-powder；Mixed-powder is heat-treated；Hot pressed sintering obtains light high heat conducting graphene-based heat sink material containing aluminium；The present invention can prepare thickness in the other three-dimensional graphite alkenyl heat sink material of Centimeter Level.Itself light weight, thermal conductivity are high and heat flux is big, have good radiating effect, can be widely applied to aerospace field.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of system of light high heat conducting graphene-based heat sink material containing aluminium
Preparation Method and heat sink material.
Background technology
In aerospace field, various spacecraft and weaponry functions are stronger and stronger, then internals it is integrated
Degree is increasing, and power density is also increasing, it is necessary to efficient heat sink material and structure, but current heat sink material is
Through the requirement that much can not meet development.Such as, for the deep space instrumentation system (DSIS) of Highgrade integration, detector space is limited and many
Electric energy is produced using nuclear energy to be promoted and system operation, causes electronic component to be integrated in power supply in narrow regions, hot-fluid is close
Degree is sharply increased, and for special outer space environment, we require that the heat sink material of a new generation has high heat conductance, large radiation system concurrently
Quality is relatively lighter again simultaneously for number.
Graphene is as a class New Two Dimensional crystalline material, in addition to the intensity with superelevation, and its individual layer thermal conductivity rate is up to
~5300W/ (mK), and with excellent radiance.Development to heat sink material of new generation provides rare opportunity.
If graphene can be assembled into the structure or material of macroscopic view in some way, graphene can be given full play to again receive and see yardstick
Thermal property, realize from receive see yardstick to macro-scale leap, it is possible to so that the thermal property of graphene obtains effective profit
With.The preparation of current graphene heat dissipation film is relatively ripe, and thermal conductivity can also reach~2000W/ (mK).But graphite
Alkene heat dissipation film is difficult thorough solution radiating problem, because it has a basic contradiction --- and thermal conductivity increases and dropped with thickness
It is low.
Fourier law is the most important theorem for describing thermal conductivity of material.According to Fourier law, list can be calculated
The energy of transmission in the time of position.For the heat transfer of one-dimensional planomural, Fourier law is：
Heat flux:
Q=q " A
Heat flow density q " (W/m2) it is the rate of heat transfer in the x direction in the unit area perpendicular with transmission direction.
It and thermograde in this directionIt is directly proportional, proportionality constant k is thermal conductivity (W/ (mK)).Because heat energy is reduced to temperature
Direction transmission, so there is negative sign in equation.A is the cross-sectional area on heat transfer direction.So we will be dissipated well
Thermal effect, it is necessary to prepare the block materials of thick film or three-dimensional.But graphene film, with the increase of thickness, its compactness is difficult
With ensure and interlayer phon scattering increase, result in its thermal conductivity drastically decline (Y.Zhang, J.Liu et al,
Improved Heat Spreading Performance of Functionalized Graphene in
Microelectronic Device Application[J].Advanced Functional material,2015,25,
4430–4435.).Therefore, for aviation field, the problem that graphene radiation material is present is that can not realize lightweight, hyperpyrexia simultaneously
Conductance and big thickness (three-dimensional block), i.e., can not obtain big heat flux..
The content of the invention
For increase of the above-mentioned graphene film with thickness, its compactness is difficult to ensure that and the phon scattering of interlayer increases
Plus, it result in its thermal conductivity and drastically decline, it is impossible to while realizing lightweight, high heat conductance and big thickness (three-dimensional block), i.e., can not
The problems such as obtaining big heat flux, the present invention provides a kind of preparation method of light high heat conducting graphene-based heat sink material containing aluminium,
Specifically follow the steps below：
1) aluminium powder dispersion liquid is prepared：Aluminium powder is scattered in deionized water；
2) graphene dispersing solution is prepared：Graphene powder is scattered in deionized water；
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution；4) freeze-drying obtains a nanometer mixed-powder；
5) mixed-powder is heat-treated；
6) hot pressed sintering：By step 5) obtained mixed-powder is put into hot pressed sintering in graphite jig, that is, obtains lightweight high
Heat conduction graphene-based heat sink material containing aluminium；
First carry out above-mentioned steps 1) above-mentioned steps 2 are carried out afterwards), or first carry out above-mentioned steps 2) above-mentioned steps 1 are carried out afterwards).
It is above-mentioned to concretely comprise the following steps：
1) aluminium powder dispersion liquid is prepared：Particle diameter is scattered in deionized water for 1~3 micron of spherical aluminium powder, be in frequency
Under 10KHz~100KHz, ultrasonically treated 30min~60min is carried out, aluminium powder dispersion liquid is obtained；
2) graphene dispersing solution is prepared：Two-dimensional is dispersed in deionization for 5~10 microns of few layer graphene powder
In water, in the case where frequency is 10KHz~100KHz, ultrasonically treated 30min~60min is carried out, uniform solution is formed it into, obtains
Graphene dispersing solution；
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution：Aluminium powder dispersion liquid and graphene dispersing solution are mixed, in frequency
For under 10KHz~100KHz, water bath sonicator 5-10min, then the ultrasound 30min under 200W power, obtains graphene/aluminum powder
Mixed dispersion liquid；
4) it is freeze-dried：For snap frozen, prevent aluminum particulate from precipitating, mixed dispersion liquid is poured into the larger gold of area
Belong in container, load liquid nitrogen respectively in canister bottom and top, the water speed in dispersion liquid is frozen into ice, formed
The mixture of aluminium, graphene and ice, is put into freeze dryer by mixture and 24h~48h is dried at -100 DEG C, mixed
Close powder；
5) mixed-powder is heat-treated：The mixed-powder of above-mentioned preparation is incubated 2h and removed at 450 DEG C~500 DEG C and is disperseed
Agent,
Powder is put into hydrogen reducing furnace the progress reductase 12 h at 400 DEG C again, to remove the oxygen on aluminium powder surface, finally
To mixed-powder；
7) hot pressed sintering：Mixed-powder after processing is put into graphite jig, under vacuum hot pressed sintering, produced
To light high heat conducting graphene-based heat sink material containing aluminium, and can be by the thickness of the how much control heat sink materials for adding mixed-powder
Degree.
Few layer graphene is 3-10 layer graphenes.
It is preferred that, above-mentioned steps 2) described in graphene powder prepared by liquid phase stripping method, described graphite
In alkene dispersion liquid, the concentration of graphene is 0.1mg/mL~5mg/mL..
It is preferred that, above-mentioned steps 1) described in aluminium powder dispersion liquid in, the concentration of aluminium powder is 1mg/mL~20mg/mL.
It is preferred that, above-mentioned steps 3) described in mixed dispersion liquid in graphene and aluminium powder mass ratio be 1:0.1~1:
0.7。
It is preferred that, above-mentioned steps 4) described in freeze-drying be from sample upper and lower surface to carry out quick freeze with liquid nitrogen,
Drying condition is dry 24h~48h at -100 DEG C.
It is preferred that, above-mentioned steps 5) described in heat treatment condition be to be incubated 2h, reducing condition at 450 DEG C~500 DEG C
It is to use hydrogen reducing 2h at 400 DEG C.
It is preferred that, above-mentioned steps 6) described in the condition of hot pressed sintering be the 20MPa~60MPa that pressurizes at 600 DEG C of temperature,
5min~120min is incubated, 700 DEG C are continuously heating to, 30min~120min, vacuum environment is incubated.
The thickness of heat sink material is controlled by the addition of powder.
The beneficial effects of the invention are as follows：First, the inventive method technique is simple, and can obtain the three-dimensional plate of high heat conductance
Shape heat sink material, solves the problem that high heat conductance and big heat flux can not be taken into account；2nd, the present invention utilizes graphene superelevation thermal conductivity
Rate, using graphene as elementary cell, using aluminium powder as binding agent, the hot pressing at a temperature of higher than aluminium powder fusing point, aluminium plays bonding
The effect of graphene film, and external force is provided by hot pressing, the space between graphene sheet layer is reduced, compactness is added,
Phon scattering is reduced, so as to add the thermal conductivity of material；3rd, light high heat conducting graphene/aluminum nanometer prepared by the present invention
Fluid matasomatism when composite fin is discharged in hot pressing due to gas, it is in align to make graphene, layer and layer
It is mutually lapped, forms the passage of heat, so that fin obtains thermal conductivity in higher face；4th, aluminium of the present invention is used as bonding
Agent, using the small density of aluminium in itself, can obtain the graphene composite material fin of light high heat conducting, can meet modern to dissipating
The requirement of hot material lightweight, has greater advantages than heat sink materials such as copper and aluminium at present.With reference to described in above-mentioned one-four, this
Invention is using graphene as elementary cell, with lightweight, and the of a relatively high metallic aluminium of thermal conductivity is as binding agent and filler, additional machine
Tool pressure, so as to solve compactness problem, the thickness of fin is controlled by the addition of powder, realization prepares thick film, three
Ensure compactness while dimension material, it is to avoid thermal conductivity declines, it is final to realize high heat conductance and big thickness (three-dimensional block) simultaneously,
Obtain big heat flux.
Brief description of the drawings
Fig. 1 is the thermal conductivity test process of embodiment one；A) in test process on sample power and the temperature difference matched curve；b)
Thermo parameters method (thermal infrared imager shooting) on sample；
Fig. 2 is the stereoscan photograph of the light high heat conducting of embodiment one graphene-based heat sink material section containing aluminium；
Fig. 3 is the light high heat conducting of embodiment one graphene-based heat sink material photo containing aluminium；
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：
The preparation method of light high heat conducting graphene-based heat sink material containing aluminium described in the present embodiment, is specifically according to following
What step was carried out：
1) aluminium powder dispersion liquid is prepared：Particle diameter is scattered in deionized water for 1~3 micron of spherical aluminium powder, be in frequency
Under 100KHz, carry out ultrasonically treated 30min and obtain aluminium powder dispersion liquid；
Described aluminium powder dispersion liquid concentration is 0.5mg/mL.
2) graphene dispersing solution is prepared：Two-dimensional is dispersed in deionization for 5~10 microns of few layer graphene powder
In water, under 100KHz, ultrasonically treated 30min is carried out, graphene dispersing solution is obtained；
Described graphene dispersing solution concentration is 0.1mg/mL.
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution：Aluminium powder dispersion liquid and graphene dispersing solution are mixed, in frequency
For under 100KHz, water bath sonicator 5min, then the ultrasound 30min under 200W power, obtains the mixing of graphene/aluminum powder scattered
Liquid；
Described mixed dispersion liquid graphene and the mass ratio of aluminium powder are 1:0.1.
4) it is freeze-dried：By mixed dispersion liquid under liquid nitrogen quick freeze, at -100 DEG C dry 24h obtain mixed powder
End；
5) mixed-powder is heat-treated：The mixed-powder of above-mentioned preparation is incubated 2h at 450 DEG C and removes dispersant, at 400 DEG C
Lower hydrogen reducing 2h, the mixed-powder after being heat-treated；
6) hot pressed sintering：Mixed-powder after processing is put into graphite jig, under vacuum hot pressed sintering, obtained
Light high heat conducting graphene-based heat sink material containing aluminium.
The condition of described hot pressed sintering is the 60MPa that pressurizes at 600 DEG C of temperature, is incubated 5min, is continuously heating to 700 DEG C,
It is incubated 30min, vacuum environment.
The thermal conductivity test process of the present embodiment is shown in Fig. 1.
Stereoscan photograph such as Fig. 2 of light high heat conducting graphene-based heat sink material section containing aluminium prepared by the present embodiment one
It is shown, as shown in Figure 2, graphite in the preparation method of light high heat conducting graphene-based heat sink material containing aluminium prepared by the present embodiment one
It is mutually lapped between alkene lamella, graphene is aligned in stratiform, interface resistance is smaller, therefore with high heat conductance in face；
Light high heat conducting graphene/aluminum nano composite material fin prepared by the present embodiment one is as shown in figure 3, its thickness
For 3mm；
Thermal conductivity in the face that the present embodiment passes through test sample, obtains light high heat conducting graphene-based heat sink material containing aluminium
Thermal conductivity is 710W/ (mK) in the face of preparation method.For graphene-based heat sink material, the thickness accomplished at present is all in micron
Rank, and with the increase of thickness, thermal conductivity drastically declines, when general thickness reaches 50 microns, thermal conductivity is only 800W/
(m.K).Three-dimensional grapheme based composites fin thickness two orders of magnitude higher than graphene film prepared by the present invention, still
Thermal conductivity is but approached.It is 3 times of the thermal conductivity 237W/ (mK) of pure metallic aluminum, but density only has 2.0g/cm3, compare metallic copper
Density 8.93g/cm3It is much smaller, than the density 2.7g/cm of metallic aluminium3It is also small.Therefore, the material conduct that prepared by the method
Heat sink material is used has bigger advantage than copper and aluminium and its alloy material at present.It is particularly suitable for the requirement such as spacecraft light
The field of material.
Embodiment two：
The preparation method of light high heat conducting graphene-based heat sink material containing aluminium described in the present embodiment, is specifically according to following
What step was carried out：
1) aluminium powder dispersion liquid is prepared：Particle diameter is scattered in deionized water for 1~3 micron of spherical aluminium powder, be in frequency
Under 10KHz, carry out ultrasonically treated 60min and obtain aluminium powder dispersion liquid；
Described aluminium powder dispersion liquid concentration is 15mg/mL.
2) graphene dispersing solution is prepared：5~10 microns of few layer graphene powder of two-dimensional is dispersed in deionized water
In, under 10KHz, ultrasonically treated 60min is carried out, graphene dispersing solution is obtained；
Described graphene dispersing solution concentration is 5mg/mL.
3) theoretical aluminium powder dispersion liquid is mixed with graphene dispersing solution：Aluminium powder dispersion liquid and graphene dispersing solution are mixed,
Under frequency is 10KHz, water bath sonicator 10min, then the ultrasound 30min under 200W power obtain the mixing of graphene/aluminum powder and divided
Dispersion liquid；
Described mixed dispersion liquid graphene and the mass ratio of aluminium powder are 1:0.7.
4) it is freeze-dried：By mixed dispersion liquid under liquid nitrogen quick freeze, at -100 DEG C dry 48h obtain mixed powder
End；
5) mixed-powder is heat-treated：The mixed-powder of above-mentioned preparation is incubated 2h at 500 DEG C and removes dispersant, at 400 DEG C
Lower hydrogen reducing 2h, the mixed-powder after being heat-treated；
6) hot pressed sintering：Mixed-powder after processing is put into graphite jig, under vacuum hot pressed sintering, obtained
Light high heat conducting graphene-based heat sink material containing aluminium.
The condition of described hot pressed sintering is the 20MPa that pressurizes at 600 DEG C of temperature, is incubated 120min, is continuously heating to 700
DEG C, it is incubated 120min, vacuum environment.
The thickness of light high heat conducting manufactured in the present embodiment graphene-based heat sink material containing aluminium is that thermal conductivity is in 7mm, face
876W/(m·K).For graphene-based heat sink material, the thickness accomplished at present is all in micron level, and with the increase of thickness,
Thermal conductivity drastically declines, when general thickness reaches 50 microns, and thermal conductivity is only 800W/ (m.K).Three-dimensional graphite prepared by the present invention
Alkenyl composite fin thickness two orders of magnitude higher than graphene film, thermal conductivity can but reach identical level.It is
4 times or so of the thermal conductivity 237W/ (mK) of pure metallic aluminum, but density only has 2.2g/cm3, than the density of metallic copper
8.93g/cm3It is much smaller, than the density 2.7g/cm of metallic aluminium3It is also small.
Embodiment three：
The preparation method of light high heat conducting graphene-based heat sink material containing aluminium described in the present embodiment, is specifically according to following
What step was carried out：
1) aluminium powder dispersion liquid is prepared：Particle diameter is scattered in deionized water for 1~3 micron of spherical aluminium powder, be in frequency
Under 50KHz, carry out ultrasonically treated 45min and obtain aluminium powder dispersion liquid；
Described aluminium powder dispersion liquid concentration is 10mg/mL.
2) graphene dispersing solution is prepared：Two-dimensional is dispersed in deionization for 5~10 microns of few layer graphene powder
In water, under 50KHz, ultrasonically treated 45min is carried out, graphene dispersing solution is obtained；
Described graphene dispersing solution concentration is 3mg/mL.
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution：Aluminium powder dispersion liquid and graphene dispersing solution are mixed, in frequency
For under 50KHz, water bath sonicator 8min, then the ultrasound 30min under 200W power, obtains graphene/aluminum powder mixed dispersion liquid；
Described mixed dispersion liquid graphene and the mass ratio of aluminium powder are 1:0.4.
4) it is freeze-dried：By mixed dispersion liquid under liquid nitrogen quick freeze, at -100 DEG C dry 36h obtain mixed powder
End；
5) mixed-powder is heat-treated：The mixed-powder of above-mentioned preparation is incubated 2h at 480 DEG C and removes dispersant, at 400 DEG C
Lower hydrogen reducing 2h, the mixed-powder after being heat-treated；
6) hot pressed sintering：Mixed-powder after processing is put into graphite jig, under vacuum hot pressed sintering, obtained
Light high heat conducting graphene-based heat sink material containing aluminium.
The condition of described hot pressed sintering is pressurize at 600 DEG C of temperature 40MPa, pressurize 60min, is continuously heating to 700 DEG C,
It is incubated 60min, vacuum environment.
The thickness of light high heat conducting manufactured in the present embodiment graphene-based heat sink material containing aluminium is that thermal conductivity is in 5mm, face
1134W/(m·K).For graphene-based heat sink material, the thickness accomplished at present is all in micron level, and with the increasing of thickness
Plus, thermal conductivity drastically declines, when general thickness reaches 50 microns, and thermal conductivity is only 800W/ (m.K).Three-dimensional prepared by the present invention
Graphene-based composite fin thickness two number higher than graphene film, but thermal conductivity is but improved more than 30%.Significantly
Improve radiating efficiency.It is nearly 5 times of the thermal conductivity 237W/ (mK) of pure metallic aluminum, but density only has 2.1g/cm3.From with
Upper embodiment can be seen that light high heat conducting graphene-based heat sink material containing aluminium prepared by the present invention not only realizes lightweight, and
Thermal conductivity is controllable, and the field for requiring lightweight heat sink material in aerospace field and electronic information etc. is widely used, and energy
It is effectively promoted the update of heat sink material.
Claims (8)
1. the preparation method of light high heat conducting graphene-based heat sink material containing aluminium, it is characterised in that：Comprise the following steps：
1) aluminium powder dispersion liquid is prepared：Aluminium powder is scattered in deionized water；
2) graphene dispersing solution is prepared：Graphene powder is scattered in deionized water；
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution；
4) freeze-drying obtains a nanometer mixed-powder；
5) mixed-powder is heat-treated；
6) hot pressed sintering：By step 5) obtained mixed-powder is put into hot pressed sintering in graphite jig, that is, obtains light high heat conducting
Containing the graphene-based heat sink material of aluminium；
First carry out above-mentioned steps 1) above-mentioned steps 2 are carried out afterwards), or first carry out above-mentioned steps 2) above-mentioned steps 1 are carried out afterwards).
2. the preparation method of light high heat conducting according to claim 1 graphene-based heat sink material containing aluminium, it is characterised in that：
The step is specially：
1) aluminium powder dispersion liquid is prepared：Particle diameter is scattered in deionized water for 1~3 micron of spherical aluminium powder, it is 10KHz in frequency
Under~100KHz, ultrasonically treated 30min~60min is carried out, aluminium powder dispersion liquid is obtained；
2) graphene dispersing solution is prepared：Two-dimensional is scattered in deionized water for 5~10 microns of few layer graphene powder,
In the case where frequency is 10KHz~100KHz, ultrasonically treated 30min~60min is carried out, uniform solution is formed it into, obtains graphite
Alkene dispersion liquid；
3) aluminium powder dispersion liquid is mixed with graphene dispersing solution：Aluminium powder dispersion liquid and graphene dispersing solution are mixed, are in frequency
Under 10KHz~100KHz, water bath sonicator 5-10min, then the ultrasound 30min under 200W power, obtains graphene/aluminum powder and mixes
Close dispersion liquid；
4) it is freeze-dried：By step 3) gained mixed dispersion liquid is quick-frozen, the mixture of aluminium, graphene and ice is formed, by mixture
It is put into freeze dryer and 24h~48h is dried at -100 DEG C, obtains mixed-powder；
5) mixed-powder is heat-treated：The mixed-powder of above-mentioned preparation is incubated 2h at 450 DEG C~500 DEG C, then powder is put into
Reductase 12 h is carried out in hydrogen reducing furnace at 400 DEG C, mixed-powder is obtained；
6) hot pressed sintering：By step 5) obtained mixed-powder is put into mould, and hot pressed sintering, that is, obtain light under vacuum
Matter high heat conduction graphene-based heat sink material containing aluminium.
3. according to the preparation method of any described light high heat conducting graphene-based heat sink materials containing aluminium of claim 1-2, it is special
Levy and be：Step 2) described in graphene powder prepared by liquid phase stripping method, in described graphene dispersing solution, stone
The concentration of black alkene is 0.1mg/mL~5mg/mL.
4. according to the preparation method of any described light high heat conducting graphene-based heat sink materials containing aluminium of claim 1-3, it is special
Levy and be：Step 1) described in aluminium powder dispersion liquid, aluminium powder concentration be 0.5mg/mL~15mg/mL.
5. according to the preparation method of any described light high heat conducting graphene-based heat sink materials containing aluminium of claim 1-4, it is special
Levy and be：Step:3) mass ratio of graphene and aluminium powder is 1 in the mixed dispersion liquid described in:0.1~1:0.7.
6. according to the preparation method of any described light high heat conducting graphene-based heat sink materials containing aluminium of claim 1-5, it is special
Levy and be：Step 4) described in freeze-drying liquid nitrogen quickly cooling technology.
7. according to the preparation method of any described light high heat conducting graphene-based heat sink materials containing aluminium of claim 1-6, it is special
Levy：Step 6) described in hot pressed sintering condition be vacuum environment under, pressurize 20MPa~60MPa at 600 DEG C of temperature, insulation
5min~120min, is continuously heating at 700 DEG C, is incubated 30min-120min.
8. a kind of light high heat conducting graphene-based heat sink material containing aluminium prepared according to any methods describeds of claim 1-7.
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| CN112280540A (en) * | 2019-07-22 | 2021-01-29 | 天津大学 | Preparation method of high-thermal-conductivity graphene-metal particle composite material |
| CN112852389A (en) * | 2021-03-23 | 2021-05-28 | 依润特工业智能科技(苏州)有限公司 | High-strength heat conduction material for 5G communication and preparation method thereof |
| CN113345809A (en) * | 2021-08-05 | 2021-09-03 | 度亘激光技术（苏州）有限公司 | Semiconductor device and heat sink bonding method |
| CN114069096A (en) * | 2021-11-12 | 2022-02-18 | 天津市捷威动力工业有限公司 | Composite film capable of regulating and controlling heat conduction and lithium ion battery |
| CN115181873A (en) * | 2022-08-02 | 2022-10-14 | 苏州大学 | Copper-modified graphene oxide-based composite material, and preparation method and application thereof |
| CN116496632A (en) * | 2023-04-07 | 2023-07-28 | 深圳力越新材料有限公司 | Graphite aluminum composite heat dissipation material and preparation method thereof |
| CN116496632B (en) * | 2023-04-07 | 2024-02-13 | 深圳力越新材料有限公司 | Graphite aluminum composite heat dissipation material and preparation method thereof |
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