CN106967392B - 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 methods, and the invention solves graphene radiation material oriented alignments and compactness problem, to prepare the three-dimensional heat dissipation material with superelevation thermal conductivity.Method: graphene oxide dispersion is prepared；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 on progress precompressed (preforming), hot pressed sintering in mold and 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 achieve 1800W/ (m.K) and have very high intensity and good processing performance, be expected to thoroughly solve heat dissipation problem.
Description
Technical field
The present invention relates to highly heat-conductive material fields, and in particular to a kind of hot three-dimensional grapheme heat sink material of high-strength highly-conductive and its
Construction method.
Background technique
The miniaturization of integrated circuit and highly integrated, continues to increase the packing density of electronic component, strong providing
While big use function, increased dramatically for its operating power consumption and calorific value is also resulted in.High temperature will be to electronic component
Stability, reliability and service life generate harmful influence.The result of study of Mithal 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 failure rate can subtract 4%；If increasing by 10~20 DEG C, therefore
Barrier rate improves 100%.It 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 fever electronics member device
Heat caused by part can timely be discharged.
Since heat dissipation is a comprehensive problem, so scholar's brainstrust of academia and industry has been put into largely
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 the key that solve heat dissipation problem.There is " a weight in traditional heat sink material (copper, aluminium, artificial graphite, heat pipe etc.)
Two is low " the drawbacks of, i.e., density is big, thermal conductivity is low, heat emissivity coefficient is low.Be no longer satisfied present electronic product and aerospace
Requirement of the field to heat sink material.Graphene is as a kind of New Two Dimensional crystalline material, except with mechanical property and electric property
Except, individual layer thermal conductivity rate is up to~5300W/ (mK), provides rare opportunity to the development of heat sink material of new generation.Though
Right single-layer graphene has the thermal conductivity of superelevation, but (thickness is received only less than 1 since the size of graphene itself is very small
Rice, two-dimensional directional size is at several microns to tens microns), receiving, sight scale is uncontrollable, therefore commercial applications are difficult to break through.
It how to be the hot spot studied both at home and abroad using this advantage of graphene, one of strategy is exactly that graphene is assembled into macroscopical material
Material.If graphene can be assembled into some way macroscopic view structure or material, and can give full play to graphene receive see ruler
The thermal property of degree, realize from receive see scale to macro-scale leap, so that it may so that the thermal property of graphene is had
Effect utilizes.
Graphene, which is made into mainly graphene heat dissipation film, thermal conductivity that macroscopic material is applied to radiate, at present to reach
To 2000W/m.K or more, preparation process is also relatively mature.But there are an intrinsic disadvantages for graphene heat dissipation film
End, i.e., the preparation method of current graphene heat dissipation film, with the increase of thickness, compactness is difficult to ensure that bedding void is larger
It causes the phon scattering of interlayer to increase, results in its thermal conductivity and sharply 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,
Problem existing for graphene radiation material is that not can be implemented simultaneously high heat conductance and big thickness (three-dimensional block), i.e., can not obtain big
Heat flux.But the heat dissipation effect to realize must have big heat flux, i.e., to do thick film even three-dimensional material.It causes
This is contradictory the reason is that the preparation method of current graphene heat dissipation film increases with thickness, and the compactness of film not can guarantee, this
The application of the graphene heat dissipation film of limitation.And the graphene sheet layer directionality of prior art preparation is low, and interface resistance is big, in turn
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.
Summary of the invention
Be to solve above-mentioned current graphene heat dissipation film with the increase of thickness, compactness is difficult to ensure, bedding void compared with
It causes the phon scattering of interlayer to increase greatly, its thermal conductivity is caused sharply to decline, problem existing for graphene radiation material is can not
It realizes high heat conductance and big thickness (three-dimensional block) simultaneously, i.e., can not obtain the stone of big heat flux and prior art preparation
Black alkene lamella directionality is low, and interface resistance is big, and then leads to problems such as the thermal conductivity for prolonging lamella direction low, and the present invention provides a kind of high
The construction method of strong high thermal conductivity three-dimensional grapheme heat sink material, specifically follows the steps below:
1) graphene oxide dispersion is prepared；
2) the highly directional processing of graphene oxide；
3) it is freeze-dried: obtaining graphene oxide foam；
4) the graphene oxide foam that step 4) obtains hydrazine hydrate reduction: is obtained into grapheme foam with hydrazine hydrate reduction；
5) preforming: multiple grapheme foams being put into graphite jig, is pressurizeed with constant rate, makes grapheme material
It is preforming.
6) hot pressed sintering: by preform hot pressed sintering to get arrive the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
Above-mentioned specific steps are as follows:
1) it prepares graphene oxide dispersion: being 10KHz in frequency in deionized water by graphene oxide powder dispersion
Under~100KHz, ultrasonic treatment 30min~60min is carried out, uniform solution is formed it into, obtains graphene oxide dispersion；
2) graphene oxide dispersion the highly directional processing of graphene oxide: is put into cylindrical body or cuboid hollow mould
In, preferably metal die cools down the metal edge frame (lateral wall) of mold surrounding, then with liquid nitrogen because of mold surrounding
Degree of supercooling it is bigger, then water along the direction XY crystallize, graphene oxide layer is also along the direction XY oriented alignment；
3) be freeze-dried: it is dry at -20 DEG C that the mixture of the graphene oxide of step 2) preparation and water is put into freeze dryer
It is dry for 24 hours~48h, obtain graphene oxide foam；
4) hydrazine hydrate reduction: the highly directional structure in order to keep material, by the way of steam reduction.By graphene oxide
Foam is placed on the porose bracket in bottom, and hydrazine hydrate is placed on and is heated to reflux in device, and heating evaporates hydrazine hydrate, and oxygen will be housed
The bracket of graphite alkene foam is placed on the upper surface of hydrazine hydrate liquid, and the steam after evaporating hydrazine hydrate can just enter oxidation stone
In black alkene foam, so that graphene oxide be restored, it is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) preforming: more due to doing the grapheme foam that three-dimensional block materials need, it is unsmooth to there is exhaust in direct hot pressing
The problem of, influence the compactness of material.So multiple (2 or more) grapheme foams are overlayed graphite mo(u)ld in layer first
With the constant pre-stamped molding of rate in tool.
6) hot pressed sintering: by above-mentioned steps 5) preparation preform be put into togerther vacuum sintering funace together with mold,
Pressurize 20MPa~60MPa at 2000 DEG C, keeps the temperature 30min~120min, and vacuum environment is to get to the three-dimensional stone of high-strength highly-conductive heat
Black alkene heat sink material.
Preferably, above-mentioned steps 2) described in graphene oxide powder select large stretch of (20-30 μm) mono-layer graphite oxide
Alkene, the condition of ultrasonic treatment are that processing 30min~60min, the concentration of graphene oxide dispersion are under 10KHz~100KHz
0.1mg/mL~5mg/mL.
Preferably, above-mentioned steps 3) described in graphene oxide highly directional treatment process, by mold surrounding
Frame leads to liquid nitrogen to realize the high orientation arrangement of graphene oxide.
Preferably, above-mentioned steps 4) described in freeze-drying condition be at -20 DEG C it is dry for 24 hours~48h.
Preferably, above-mentioned steps 5) described in reduction 80% mass fraction hydrazine hydrate, using the side of steam reduction
To keep aligning for graphene, reducing condition is 118 DEG C and is heated to reflux 1h method.
Preferably, preforming condition described in step 6) is 5~15mm/min of compression rate, maximum pressure is 0.5~
1MPa, pressure maintaining 1min.
Preferably, above-mentioned steps 7) described in hot pressed sintering condition be at 2000 DEG C of temperature pressurize 20MPa~
60MPa, keeps the temperature 30min~120min, and vacuum degree is less than 0.1Pa.
Although pure graphene is difficult reality the beneficial effects of the present invention are: one, single-layer graphene has superelevation thermal conductivity
Existing single layer, so the present invention obtains the single-layer graphene of high heat conductance using large stretch of single-layer graphene oxide, by reduction, greatly
Macroscopical heat sink material interface resistance of piece graphene preparation is relatively small, realizes high heat conductance.Two, real by " ice template method "
The high orientation of existing graphene is arranged (schematic illustration is shown in Fig. 1): keeping the water in graphene oxide dispersion first in mold surrounding
Then first forming core is crystallized along degree of supercooling direction (direction XY), so that graphene oxide layer be made to take along the crystallization direction deflection of water
To, realize highly directional arrangement, mutually overlapped between graphene oxide layer, thus realize along the highly thermally conductive of graphene sheet layer direction
Rate.Three, the method that the present invention uses hydrazine hydrate steam reduction, the grapheme foam after making reduction can be very good to keep originally
Highly directional arrangement.Four, preform process eliminates the gas of grapheme foam inner most, ensure that later period hot pressing can have
The raising compactness of effect.External force is provided by hot pressing, the gap between graphene sheet layer is reduced, increases compactness, thus
Increase the thermal conductivity of material.
Detailed description of the invention
Fig. 1 is the schematic illustration 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, with a thickness of 4mm；C) profile scanning photo；
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific 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, specifically according to following step
Suddenly it carries out:
1) prepare graphene oxide dispersion: 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, ultrasonic treatment 60min is carried out, uniform solution is formed it into, obtaining concentration is 0.1mg/
ML graphene oxide dispersion；
2) the highly directional processing of graphene oxide: graphene oxide dispersion is put into metal die (100 × 100 ×
The cuboid-type mold of 50mm；The surrounding fine copper of mold, hollow structure), then carried out with metal edge frame of the liquid nitrogen to surrounding
Cooling, leading to liquid nitrogen rate is 0.5L/min；
3) be freeze-dried: it is dry at -20 DEG C that the mixture of the graphene oxide of step 2) preparation and water is put into freeze dryer
It is dry for 24 hours, obtain graphene oxide foam；
4) hydrazine hydrate reduction: graphene oxide foam is placed on the porose bracket 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 bracket equipped with graphene oxide foam is placed on hydrazine hydrate
The upper surface of liquid, the steam after evaporating hydrazine hydrate can just enter in graphene oxide foam, thus by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) preforming: the grapheme foam that the size by the preparation of 10 pieces of steps 4) is 100*100*50mm stacks in layer
In the graphite jig of 100*100mm size, the rate on subpress with 5mm/min is forced into 0.5MPa from the top down, protects
Press 1min.
6) hot pressed sintering: being put into togerther vacuum sintering funace together with mold for above-mentioned preform, adds at 2000 DEG C
20MPa is pressed, 120min is kept the temperature, vacuum degree is 1 × 10-3Pa to get arrive 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, can be with from photo with a thickness of 4mm
Find out this sample for three-dimensional block materials, can be seen that from the scanned photograph in cross section realized between graphene sheet layer it is highly directional
Arrangement.Its microstructure schematic diagram is as shown in Figure 2.
The hot three-dimensional grapheme heat sink material of high-strength highly-conductive manufactured in the present embodiment, thermal conductivity is 1712W/ (mK) in face,
With a thickness of 4mm, report that graphene heat dissipation film thermal conductivity is reduced with the increase of thickness at present, 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 heat dissipation 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, bending strength
It can reach with 68MPa and have certain toughness.In addition to this, the heat sink material of this method preparation has good processing performance,
Arbitrary shape can be processed into.Therefore the hot three-dimensional grapheme heat sink material of high-strength highly-conductive that the present invention obtains has heat dissipation effect well
Fruit and practicability.
Embodiment two:
The construction method of the hot three-dimensional grapheme heat sink material of high-strength highly-conductive described in the present embodiment, specifically according to following step
Suddenly it carries out:
1) prepare graphene oxide dispersion: 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, ultrasonic treatment 30min is carried out, uniform solution is formed it into, obtaining concentration is 5mg/mL
Graphene oxide dispersion；
2) graphene oxide dispersion the highly directional processing of graphene oxide: is put into metal die (100 × 100 × 50mm
Cuboid-type mold；The surrounding fine copper of mold, hollow structure) in, it is then carried out with metal edge frame of the liquid nitrogen to surrounding cold
But, the rate for leading to liquid nitrogen is 0.5L/min；
3) be freeze-dried: it is dry at -20 DEG C that the mixture of the graphene oxide of step 2) preparation and water is put into freeze dryer
Dry 48h obtains graphene oxide foam；
4) hydrazine hydrate reduction: graphene oxide foam is placed on the porose bracket 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 bracket equipped with graphene oxide foam is placed on hydrazine hydrate
The upper surface of liquid, the steam after evaporating hydrazine hydrate can just enter in graphene oxide foam, thus by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) preforming: the grapheme foam that the size by the preparation of 6 pieces of steps 4) is 100*100*50mm stacks in layer
In the graphite jig of 100*100mm size, 1MPa, pressure maintaining are forced into the rate of 15mm/min from top to bottom on subpress
1min。
6) hot pressed sintering: being put into togerther vacuum sintering funace together with mold for above-mentioned preform, adds at 2000 DEG C
60MPa is pressed, 30min is kept the temperature, vacuum degree is 1 × 10-3Pa to get arrive 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, with a thickness of 2.5mm, thermal conductivity is in face
1798W/ (mK), report that 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 highly directional hot three-dimensional graphite of 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, bending
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, specifically according to following step
Suddenly it carries out:
1) prepare graphene oxide dispersion: 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, ultrasonic treatment 45min is carried out, uniform solution is formed it into, obtaining concentration is 3mg/mL
Graphene oxide dispersion；
2) graphene oxide dispersion the highly directional processing of graphene oxide: is put into metal die (100 × 100 × 50mm
Cuboid-type mold；The surrounding fine copper of mold, hollow structure) in, liquid nitrogen is then passed through by the air inlet on mold, it is right
The metal edge frame of surrounding is cooled down；
3) be freeze-dried: it is dry at -20 DEG C that the mixture of the graphene oxide of step 2) preparation and water is put into freeze dryer
Dry 36h obtains graphene oxide foam；
4) hydrazine hydrate reduction: graphene oxide foam is placed on the porose bracket 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 bracket equipped with graphene oxide foam is placed on hydrazine hydrate
The upper surface of liquid, the steam after evaporating hydrazine hydrate can just enter in graphene oxide foam, thus by graphene oxide
Reduction, is heated to reflux 1h at 118 DEG C, obtains grapheme foam；
5) preforming: the grapheme foam that the size by the preparation of 8 pieces of steps 4) is 100*100*50mm stacks in layer
In the graphite jig of 100*100mm size, 0.8MPa is forced into the rate of 10mm/min from top to bottom on subpress, is protected
Press 1min.
6) hot pressed sintering: being put into togerther vacuum sintering funace together with mold for above-mentioned preform, adds at 2000 DEG C
40MPa is pressed, 60min is kept the temperature, vacuum degree is 1 × 10-3Pa to get arrive 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 is with a thickness of 3.2mm, and thermal conductivity is in 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, bending strength is
79MPa.It can be seen from the above embodiments that the present invention can obtain the high starch breeding alkene cooling fin with superelevation thermal conductivity,
And cooling fin intensity with higher and excellent machining property.Therefore the three-dimensional stone of high-strength highly-conductive heat that the present invention obtains
Black alkene heat sink material has good practicability, is expected to substitute traditional heat sink material, thoroughly solves heat dissipation problem.
Claims (7)
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: the following steps are included:
1) it prepares graphene oxide dispersion: the single-layer graphene oxide powder of 20 ~ 30 micron-scales is passed through into ultrasonic treatment point
It dissipates in deionized water, forms it into uniform graphene oxide dispersion；
2) the highly directional processing of graphene oxide: graphene oxide dispersion is put into cylindrical body or cuboid hollow mould, is used
Liquid nitrogen mold lateral wall frame is cooled down, and leading to liquid nitrogen rate is 0.5L/min;
3) it is freeze-dried: the mixture of the graphene oxide of step 2 preparation and water being put into freeze dryer freeze-drying, obtains oxygen
Graphite alkene foam；
4) hydrazine hydrate reduction: the graphene oxide foam that hydrazine hydrate reduction step 3) obtains obtains grapheme foam；
5) preforming: two or more grapheme foams are put into graphite jig, are pressurizeed with the rate of 5 ~ 15mm/min,
Pressure maintaining 1min when pressure reaches 0.5 ~ 1MPa, keeps grapheme material preforming；
6) hot pressed sintering: by above-mentioned steps 5) preparation preform be put into togerther vacuum sintering funace together with graphite jig,
Under vacuum environment, hot pressed sintering to get arrive the hot three-dimensional grapheme heat sink material of high-strength highly-conductive.
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: step
It is rapid 1) described in graphene oxide powder be large stretch of single-layer graphene oxide, maximum two-dimensional directional is super having a size of 20-30 micron
The condition of sonication is processing 30min ~ 60min under 10KHz ~ 100KHz, and the concentration of graphene oxide dispersion is 0.1mg/mL
~5mg/mL。
3. 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: step
It is rapid 3) described in freeze-drying condition be at -20 DEG C it is dry for 24 hours ~ 48h.
4. 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: step
It is rapid 4) described in hydrazine hydrate be 80% mass fraction hydrazine hydrate, using the method for steam reduction, reducing condition is 118
DEG C it is heated to reflux 1h.
5. 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: step
It is rapid 5) described in preforming condition be 5 ~ 15mm/min of compression rate, pressure maintaining 1min when pressure reaches 0.5 ~ 1MPa.
6. 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: step
It is rapid 6) described in hot pressed sintering condition be at 2000 DEG C of temperature pressurization 20MPa ~ 60MPa, keep the temperature 30min ~ 120min, vacuum
Environment.
7. a kind of hot three-dimensional grapheme heat sink material of high-strength highly-conductive according to any the method preparation of claim 1-6.
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| CN115490520A (en) * | 2022-08-23 | 2022-12-20 | 清华大学深圳国际研究生院 | Low-temperature preparation method of high-strength graphite or layered transition metal carbide densified macroscopic body |
| CN115353867A (en) * | 2022-08-25 | 2022-11-18 | 江苏斯迪克新材料科技股份有限公司 | Preparation method of graphene-based composite heat-conducting film |
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