CN106967392A - The hot three-dimensional grapheme heat sink material of high-strength highly-conductive and its construction method - Google Patents
The hot three-dimensional grapheme heat sink material of high-strength highly-conductive and its construction method Download PDFInfo
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Abstract
The present invention relates to a kind of hot three-dimensional grapheme heat sink material of high-strength highly-conductive and its construction method, the invention solves the problems that graphene radiation material oriented alignment and fine and close sex chromosome mosaicism, so as to prepare the three-dimensional heat dissipation material with superelevation thermal conductivity.Method：Prepare graphene oxide dispersion；The highly directional processing of graphene oxide；It is freeze-dried to obtain graphene oxide foam；Hydrazine hydrate reduction obtains grapheme foam；Grapheme foam is placed in mould and carries out precompressed (preforming), hot pressed sintering obtains the hot three-dimensional grapheme heat sink material of high-strength highly-conductive；Graphene radiation material thickness prepared by the present invention breaches the directionality and compactness problem of graphene heat dissipation film in Centimeter Level and the arrangement of graphene film high orientation.Its thermal conductivity can reach 1800W/ (m.K) and have very high intensity and good processing characteristics, be expected to thoroughly solve radiating problem.
Description
Technical field
The present invention relates to highly heat-conductive material field, and in particular to a kind of hot three-dimensional grapheme heat sink material of high-strength highly-conductive and its
Construction method.
Background technology
The miniaturization of integrated circuit and highly integrated, continues to increase the packing density of electronic component, there is provided strong
While big use function, increased dramatically for its operating power consumption and caloric value is also resulted in.High temperature will be to electronic component
Stability, reliability and life-span produce harmful influence.Mithal result of study shows (Mithal et al.Design
of experimental based evaluation of thermal performance of a flichip
electronic assembly[C].ASME EEP Proceedings.New York：ASME, 1996,18：109-115.),
The temperature of electronic component reduces by 1 DEG C in normal working temperature level, and its fault rate can subtract 4%；If 10~20 DEG C of increase, therefore
Barrier rate improves 100%.Therefore, should to thermal design work in order to make device play optimum performance and ensure high reliability
To pay much attention to therefore, in order to make device play optimum performance and ensure high reliability, it is necessary to ensure that heating electronics member device
Heat produced by part can be discharged timely.
Due to radiating be a comprehensive problem, so scholar's brainstrust of academia and industrial quarters put into it is substantial amounts of
Energy solves all kinds of heat dissipation problems.In addition to industrial means, cooling requirements can be reached and not influence other performances of electronic product by finding
Heat sink material be solve heat dissipation problem key.There is " a weight in traditional heat sink material (copper, aluminium, Delanium, heat pipe etc.)
Two is low " the drawbacks of, i.e., density is big, thermal conductivity is low, heat emissivity coefficient is low.Present electronic product and Aero-Space can not be met
Requirement of the field to heat sink material.Graphene is as a class New Two Dimensional crystalline material, except with mechanical property and electric property
Outside, its individual layer thermal conductivity rate is up to~5300W/ (mK), and the development to heat sink material of new generation provides rare opportunity.Though
Right single-layer graphene has the thermal conductivity of superelevation, but is due to that the size of graphene in itself is very small (only less than 1 receive by thickness
Rice, two-dimensional directional size is at several microns to tens microns), see yardstick receiving and be difficult to control to, therefore commercial applications are difficult to break through.
How using graphene, this advantage is the focus studied both at home and abroad, and one of strategy is exactly that graphene is assembled into macroscopical material
Material.If graphene can be assembled into the structure or material of macroscopic view in some way, graphene can be given full play to again and receives sight chi
The thermal property of degree, realize from receive see yardstick to macro-scale leap, it is possible to so that the thermal property of graphene is had
Effect is utilized.
Graphene is made into the mainly graphene heat dissipation film that macroscopic material is applied to radiating at present, its thermal conductivity can reach
To more than 2000W/m.K, preparation technology is also relatively ripe.But there is an intrinsic disadvantage in graphene heat dissipation film
End, i.e., the preparation method of current graphene heat dissipation film, with the increase of thickness, its compactness is difficult to ensure that bedding void is larger
Causing the phon scattering of interlayer increases, and result in its thermal conductivity and drastically declines (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,
The problem that graphene radiation material is present can not obtain big for that can not realize high heat conductance and big thickness (three-dimensional block) simultaneously
Heat flux.But the radiating effect for wanting to have realized there must be big heat flux, i.e., to do thick film even three-dimensional material.Cause
The reason for contradiction be the preparation method of current graphene heat dissipation film as thickness increases, the compactness of film can not ensure, this
The application of the graphene heat dissipation film of limitation.And graphene sheet layer directionality prepared by prior art is low, interface resistance is big, and then
Cause the thermal conductivity along lamella direction low.And grapheme foam is after carrying out reduction, original oriented alignment can be destroyed, and reduce thermal conductivity.
The content of the invention
Be to solve above-mentioned current graphene heat dissipation film with the increase of thickness, its compactness is difficult to ensure that, bedding void compared with
Cause the phon scattering of interlayer to increase greatly, cause its thermal conductivity drastically to decline, the problem that graphene radiation material is present is can not
High heat conductance and big thickness (three-dimensional block) are realized simultaneously, i.e., can not obtain big heat flux, and stone prepared by prior art
Black alkene lamella directionality is low, and interface resistance is big, and then causes the low problem of thermal conductivity of prolonging lamella direction, and the present invention provides a kind of high
The construction method of strong high heat conduction three-dimensional grapheme heat sink material, is specifically followed the steps below：
1) graphene oxide dispersion is prepared；
2) the highly directional processing of graphene oxide；
3) it is freeze-dried：Obtain graphene oxide foam；
4) hydrazine hydrate reduction：By step 4) obtained graphene oxide foam obtains grapheme foam with hydrazine hydrate reduction；
5) it is preforming：Multiple grapheme foams are put into graphite jig, is pressurizeed with constant speed, makes grapheme material
It is preforming.
6) hot pressed sintering：By preform hot pressed sintering, that is, obtain the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
It is above-mentioned to concretely comprise the following steps：
1) graphene oxide dispersion is prepared：Graphene oxide powder is scattered in deionized water, it is 10KHz in frequency
Under~100KHz, ultrasonically treated 30min~60min is carried out, uniform solution is formed it into, obtains graphene oxide dispersion；
2) the highly directional processing of graphene oxide：Graphene oxide dispersion is put into cylinder or cuboid hollow mould
In, preferred metal die, then with liquid nitrogen, is cooled down, because mould surrounding to the metal edge frame (lateral wall) of mould surrounding
Degree of supercooling than larger, then water is crystallized along XY directions, and graphene oxide layer is also along XY directions oriented alignment；
3) it is freeze-dried：By step 2) prepare graphene oxide and water mixture be put into freeze dryer at -20 DEG C do
Dry 24h~48h, obtains graphene oxide foam；
4) hydrazine hydrate reduction：In order to keep the highly directional structure of material, by the way of steam reduction.By graphene oxide
Foam is placed on the porose support in bottom, and hydrazine hydrate is placed on and is heated to reflux in device, and heating evaporates hydrazine hydrate, will be equipped with oxygen
The support of graphite alkene foam is placed on above hydrazine hydrate liquid, the steam after hydrazine hydrate evaporation is just entered oxidation stone
In black alkene foam, so that graphene oxide be reduced, 1h is heated to reflux at 118 DEG C, grapheme foam is obtained；
5) it is preforming：Because the grapheme foam for making three-dimensional block materials needs is more, it is not smooth to there is exhaust in direct hot pressing
The problem of, influence the compactness of material.So multiple (more than 2) grapheme foams are overlayed into graphite mo(u)ld in layer first
With the pre-stamped shaping of constant speed in tool.
6) hot pressed sintering：By above-mentioned steps 5) prepare preform be put into vacuum sintering funace together with mould,
Pressurize 20MPa~60MPa at 2000 DEG C, is incubated 30min~120min, and vacuum environment obtains the three-dimensional stone of high-strength highly-conductive heat
Black alkene heat sink material.
It is preferred that, above-mentioned steps 2) described in graphene oxide powder from large stretch of (20-30 μm) mono-layer graphite oxide
Alkene, ultrasonically treated condition is processing 30min~60min under 10KHz~100KHz, and the concentration of graphene oxide dispersion is
0.1mg/mL~5mg/mL.
It is preferred that, above-mentioned steps 3) described in graphene oxide highly directional processing procedure, by mould surrounding
Frame leads to liquid nitrogen to realize that the high orientation of graphene oxide is arranged.
It is preferred that, above-mentioned steps 4) described in freeze-drying condition be that 24h~48h is dried at -20 DEG C.
It is preferred that, above-mentioned steps 5) described in the reduction hydrazine hydrate of 80% mass fraction, using the side of steam reduction
Method is to keep aligning for graphene, and reducing condition is 118 DEG C and is heated to reflux 1h.
It is preferred that, step 6) described in preforming condition be 5~15mm/min of compression rate, maximum pressure is 0.5~
1MPa, pressurize 1min.
It is preferred that, above-mentioned steps 7) described in hot pressed sintering condition be pressurization 20MPa at 2000 DEG C of temperature~
60MPa, is incubated 30min~120min, and vacuum is less than 0.1Pa.
The beneficial effects of the invention are as follows：Although the first, single-layer graphene has superelevation thermal conductivity, pure graphene is difficult reality
Existing individual layer, so the present invention obtains the single-layer graphene of high heat conductance by reduction, greatly using large stretch of single-layer graphene oxide
Macroscopical heat sink material interface resistance prepared by piece graphene is relatively small, realizes high heat conductance.2nd, it is real by " ice template method "
The high orientation arrangement of existing graphene (principle schematic is shown in Fig. 1)：Make the water in graphene oxide dispersion first in mould surrounding
First forming core, is then crystallized along degree of supercooling direction (XY directions), so that crystallization direction deflection of the graphene oxide layer along water takes
To realizing and mutually overlapped between highly directional arrangement, graphene oxide layer, so as to realize along the highly thermally conductive of graphene sheet layer direction
Rate.3rd, the present invention makes the grapheme foam after reduction can be very good to keep originally using the method for hydrazine hydrate steam reduction
Highly directional arrangement.4th, preform process eliminates the gas of grapheme foam inner most, it is ensured that later stage hot pressing can have
The raising compactness of effect.External force is provided by hot pressing, the space between graphene sheet layer is reduced, adds compactness, so that
Add the thermal conductivity of material.
Brief description of the drawings
Fig. 1 is the principle schematic that " ice template method " realizes the highly directional arrangement of graphene film；
Fig. 2 is the microcosmic arrangement schematic diagram of graphene sheet layer；
Fig. 3 is the photomacrograph of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive and sweeping for cross section prepared by embodiment one
Retouch photo；A) full face；B) side photo, thickness is 4mm；C) profile scanning photo；
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 construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive described in the present embodiment, is specifically according to following step
Suddenly carry out：
1) graphene oxide dispersion is prepared：By the single-layer graphene oxide powder of 20~30 micron-scales be dispersed in from
In sub- water, in the case where frequency is 10KHz, ultrasonically treated 60min is carried out, uniform solution is formed it into, obtain concentration for 0.1mg/
ML graphene oxide dispersions；
2) the highly directional processing of graphene oxide：Graphene oxide dispersion is put into metal die (100 × 100 ×
50mm cuboid-type mould；The surrounding fine copper of mould, hollow structure), then the metal edge frame of surrounding is carried out with liquid nitrogen
Cooling, it is 0.5L/min to lead to liquid nitrogen speed；
3) it is freeze-dried：By step 2) prepare graphene oxide and water mixture be put into freeze dryer at -20 DEG C do
Dry 24h, obtains graphene oxide foam；
4) hydrazine hydrate reduction：Graphene oxide foam is placed on the porose support in bottom, by the water of 80% mass fraction
Conjunction hydrazine, which is placed on, to be heated to reflux in device, and heating evaporates hydrazine hydrate, and the support that will be equipped with graphene oxide foam is placed on hydrazine hydrate
Above liquid, make hydrazine hydrate evaporate after steam can just enter in graphene oxide foam so that by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) it is preforming：By 10 pieces of steps 4) size for preparing stacks in layer for 100*100*50mm grapheme foam
In the graphite jig of 100*100mm sizes, 0.5MPa is forced into 5mm/min speed from the top down on subpress, protected
Press 1min.
6) hot pressed sintering：Above-mentioned preform is put into vacuum sintering funace together with mould, added at 2000 DEG C
20MPa is pressed, 120min is incubated, vacuum is 1 × 10-3Pa, that is, obtain the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
Fig. 3 is the hot three-dimensional grapheme heat sink material of high-strength highly-conductive manufactured in the present embodiment, and thickness is 4mm, can be with from photo
It is three-dimensional block materials to find out this sample, is realized between can be seen that graphene sheet layer from the scanned photograph in cross section highly directional
Arrangement.Its microstructure schematic diagram is as shown in Figure 2.
Thermal conductivity is 1712W/ (mK) in the hot three-dimensional grapheme heat sink material of high-strength highly-conductive manufactured in the present embodiment, face,
Thickness is 4mm, at present report graphene heat dissipation film thermal conductivity reduced with the increase of thickness, 40 micron thickness thermal conductivity most
Height arrives 1234W/ (mK) (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.), the hot three-dimensional grapheme radiating of high-strength highly-conductive prepared by the present invention
Material thickness improves two orders of magnitude, and thermal conductivity also improves 40% but density only has 1.70g/cm3, its bending strength
It can reach with 68MPa and have certain toughness.In addition, the heat sink material that prepared by this method has good processing characteristics,
Arbitrary shape can be processed into.Therefore the hot three-dimensional grapheme heat sink material of high-strength highly-conductive that the present invention is obtained has radiating effect well
Fruit and practicality.
Embodiment two：
The construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive described in the present embodiment, is specifically according to following step
Suddenly carry out：
1) graphene oxide dispersion is prepared：By the single-layer graphene oxide powder of 20~30 micron-scales be dispersed in from
In sub- water, in the case where frequency is 100KHz, ultrasonically treated 30min is carried out, uniform solution is formed it into, obtain concentration for 5mg/mL
Graphene oxide dispersion；
2) the highly directional processing of graphene oxide：Graphene oxide dispersion is put into metal die (100 × 100 × 50mm
Cuboid-type mould；The surrounding fine copper of mould, hollow structure) in, then the metal edge frame of surrounding is carried out with liquid nitrogen cold
But, the speed for leading to liquid nitrogen is 0.5L/min；
3) it is freeze-dried：By step 2) prepare graphene oxide and water mixture be put into freeze dryer at -20 DEG C do
Dry 48h, obtains graphene oxide foam；
4) hydrazine hydrate reduction：Graphene oxide foam is placed on the porose support in bottom, by the water of mass fraction 80%
Conjunction hydrazine, which is placed on, to be heated to reflux in device, and heating evaporates hydrazine hydrate, and the support that will be equipped with graphene oxide foam is placed on hydrazine hydrate
Above liquid, make hydrazine hydrate evaporate after steam can just enter in graphene oxide foam so that by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) it is preforming：By 6 pieces of steps 4) size for preparing stacks in layer for 100*100*50mm grapheme foam
In the graphite jig of 100*100mm sizes, 1MPa, pressurize are forced into 15mm/min speed from top to bottom on subpress
1min。
6) hot pressed sintering：Above-mentioned preform is put into vacuum sintering funace together with mould, added at 2000 DEG C
60MPa is pressed, 30min is incubated, vacuum is 1 × 10-3Pa, that is, obtain the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
The hot three-dimensional grapheme heat sink material of high-strength highly-conductive manufactured in the present embodiment, thickness is that thermal conductivity is in 2.5mm, face
1798W/ (mK), report graphene heat dissipation film thermal conductivity is reduced with the increase of thickness at present, in the thermal conductivity of 20 micron thickness
Rate up to 1642W/ (mK) (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.), the hot three-dimensional graphite of highly directional high-strength highly-conductive prepared by the present invention
Alkene heat sink material thickness improves two orders of magnitude, and it is that density only has 1.7g/cm that thermal conductivity, which also improves 10%,3, it bends
Intensity is 78MPa.
Embodiment three：
The construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive described in the present embodiment, is specifically according to following step
Suddenly carry out：
1) graphene oxide dispersion is prepared：By the single-layer graphene oxide powder of 20~30 micron-scales be dispersed in from
In sub- water, in the case where frequency is 50KHz, ultrasonically treated 45min is carried out, uniform solution is formed it into, obtain concentration for 3mg/mL
Graphene oxide dispersion；
2) the highly directional processing of graphene oxide：Graphene oxide dispersion is put into metal die (100 × 100 × 50mm
Cuboid-type mould；The surrounding fine copper of mould, hollow structure) in, liquid nitrogen is then passed through by the air admission hole on mould, it is right
The metal edge frame of surrounding is cooled down；
3) it is freeze-dried：By step 2) prepare graphene oxide and water mixture be put into freeze dryer at -20 DEG C do
Dry 36h, obtains graphene oxide foam；
4) hydrazine hydrate reduction：Graphene oxide foam is placed on the porose support in bottom, by the water of mass fraction 80%
Conjunction hydrazine, which is placed on, to be heated to reflux in device, and heating evaporates hydrazine hydrate, and the support that will be equipped with graphene oxide foam is placed on hydrazine hydrate
Above liquid, make hydrazine hydrate evaporate after steam can just enter in graphene oxide foam so that by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) it is preforming：By 8 pieces of steps 4) size for preparing stacks in layer for 100*100*50mm grapheme foam
In the graphite jig of 100*100mm sizes, 0.8MPa is forced into 10mm/min speed from top to bottom on subpress, protected
Press 1min.
6) hot pressed sintering：Above-mentioned preform is put into vacuum sintering funace together with mould, added at 2000 DEG C
40MPa is pressed, 60min is incubated, vacuum is 1 × 10-3Pa, that is, obtain the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
The hot three-dimensional grapheme heat sink material thickness of high-strength highly-conductive manufactured in the present embodiment is that thermal conductivity is in 3.2mm, face
1744W/ (mK), reports that graphene heat dissipation film thermal conductivity is reduced with the increase of thickness, in the thermal conductivity of 40 micron thickness at present
Rate up to 1234W/ (mK) (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.), highly directional three-dimensional grapheme heat sink material prepared by the present invention
Thickness improves two orders of magnitude, and thermal conductivity also improves 40% but density only has 1.70g/cm3, its bending strength is
79MPa.By above example it can be seen that the present invention can obtain the high starch breeding alkene fin with superelevation thermal conductivity,
And the fin has higher intensity and excellent machining property.Therefore the three-dimensional stone of high-strength highly-conductive heat that the present invention is obtained
Black alkene heat sink material has good practicality, is expected to substitute traditional heat sink material, thoroughly solves radiating problem.
Claims (8)
1. a kind of construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive, it is characterised in that：Comprise the following steps：
1) graphene oxide dispersion is prepared；
2) the highly directional processing of graphene oxide；
3) it is freeze-dried：Obtain graphene oxide foam；
4) hydrazine hydrate reduction：By step 3) obtained graphene oxide foam obtains grapheme foam with hydrazine hydrate reduction；
5) it is preforming：By 2 above steps 4) made from grapheme foam be put into graphite jig, pressurizeed with constant speed,
Make grapheme material preforming.
6) hot pressed sintering：By step 5) obtained preform hot pressed sintering, that is, obtain the hot three-dimensional grapheme radiating of high-strength highly-conductive
Material.
2. the construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive according to claim 1, it is characterised in that：Institute
Stating step is specially：
1) graphene oxide dispersion is prepared：The single-layer graphene oxide powder of 20~30 micron-scales is passed through ultrasonically treated point
Dissipate in deionized water, form it into uniform graphene oxide dispersion；
2) the highly directional processing of graphene oxide：Graphene oxide dispersion is put into cylinder or cuboid hollow mould, used
Liquid nitrogen mould lateral wall frame is cooled down, and it is 0.5L/min to lead to liquid nitrogen speed；
3) it is freeze-dried：By step 3) prepare graphene oxide and water mixture be put into freeze dryer freeze-drying, obtain oxygen
Graphite alkene foam；
4) hydrazine hydrate reduction：Hydrazine hydrate reduction step 3) obtained graphene oxide foam, obtain grapheme foam；
5) it is preforming：By 2 above steps 4) made from grapheme foam be put into graphite jig, pressurizeed with constant speed,
Make grapheme material preforming.
6) hot pressed sintering：By above-mentioned steps 5) prepare preform be put into vacuum sintering funace together with graphite jig,
Under vacuum environment, hot pressed sintering obtains the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
3. according to the construction method of any described hot three-dimensional grapheme heat sink materials of high-strength highly-conductive of claim 1-2, its feature
It is：Step 1) described in graphene oxide powder be large stretch of single-layer graphene oxide, maximum two-dimensional directional size is 20-30
Micron, ultrasonically treated condition is processing 30min~60min under 10KHz~100KHz, and the concentration of graphene oxide dispersion is
0.1mg/mL~5mg/mL.
4. according to the construction method of any described hot three-dimensional grapheme heat sink materials of high-strength highly-conductive of claim 1-3, its feature
It is：Step 3) described in freeze-drying condition be that 24h~48h is dried at -20 DEG C.
5. according to the construction method of any described hot three-dimensional grapheme heat sink materials of high-strength highly-conductive of claim 1-4, its feature
It is：Step 4) described in hydrazine hydrate be 80% mass fraction hydrazine hydrate, the method for using steam reduction, reduce bar
Part is 118 DEG C and is heated to reflux 1h.
6. according to the construction method of any described hot three-dimensional grapheme heat sink materials of high-strength highly-conductive of claim 1-5, its feature
It is：Step 5) described in preforming condition be 5~15mm/min of compression rate, maximum pressure is 0.5~1MPa, pressurize
1min。
7. according to the construction method of any described hot three-dimensional grapheme heat sink materials of high-strength highly-conductive of claim 1-6, its feature
It is：Step 6) described in hot pressed sintering condition be the 20MPa~60MPa that pressurizes at 2000 DEG C of temperature, insulation 30min~
120min, vacuum environment.
8. a kind of hot three-dimensional grapheme heat sink material of high-strength highly-conductive prepared according to any methods describeds of claim 1-7.
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