CN104986754A - Graphene-based thermal conductive film preparing method - Google Patents
Graphene-based thermal conductive film preparing method Download PDFInfo
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Abstract
The invention provides a graphene-based thermal conductive film preparing method which includes the steps that biological materials are stirred and squeezed broken, and a solvent is added to the biological materials to dilute the materials; ultrasonic suction filtration is conducted on the obtained biological material pulp, and filter liquor of the biological material pulp is obtained and sealed for use; ultrasound is conducted on a graphite oxide solution, and oxidized graphene sol is obtained; the biological material filter liquid is mixed with the oxidized graphene sol, the mixed solution is made to react, and a reduced graphene film is obtained; the thermal annealing is conducted on the obtained film under the conditions of the inert atmosphere and low temperature, and the high-thermal-conductive graphene film is obtained. The graphene film prepared through the method has the advantages of being thermal conductive, electric conductive, good in mechanical property, controllable in thickness, wide in raw material source and capable of achieving batch production easily.
Description
Technical field
The invention belongs to a kind of preparation method of heat conduction film, particularly a kind of method preparing graphene-based heat conduction film.
Background technology
In recent years along with the fast development of science and technology, the design of instrument, equipment is made more and more significantly to present feature that is light, thin, short, little and high efficiency.But simultaneously adjoint one important problem is that plant and instrument creates a large amount of heats in operational process, if these heats are got rid of not in time, will badly influence job stability and the safe reliability of electron device.Graphene oxide reduces by gordian technique exactly that prepare graphene-based heat conduction film, the method of current redox graphene mainly comprises: (1) thermal reduction, but this kind of requirement of method to stove is higher, because general processing sample needs at 1000 DEG C, even up to 2000 DEG C, and and power consumption; (2) solution chemical reduction, the reagent of the reduction that this kind of method is used is generally sodium borohydride, hydrazine hydrate, hydrogen iodide, and these reagent have strong toxicity or strong corrodibility; (3) hydrothermal reduction, this kind of method needs to carry out at high temperature under high pressure, and prepared sample is and easily reunites, once can reunite, the heat conductivility of graphene-based film will be greatly affected.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, provide one to have nontoxic, energy-saving and cost-reducing, good heat conductivity, the method for the graphene-based heat conduction film of the preparation that can produce in enormous quantities.
In order to solve the technical problem of above-mentioned existence, technical scheme of the present invention is as follows:
(1) prepare graphite oxide, graphite oxide is made into the water-sol that concentration is 0.5-6mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol;
(2) biomaterial is stirred squeezing broken, itself and solvent are diluted and obtain biomaterial slurry, the concentration of slurry is 1-20mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain biomaterial filtrate;
(3) be 1:5-10 by the mass ratio of graphite oxide and biological slurry, biomaterial filtrate mixed with the graphene oxide water-sol, at room temperature-100 DEG C of temperature, carries out 10min-48h reaction, reacted the graphene film of rear preparation reduction;
(4) by gained graphene film at argon gas atmosphere thermal anneal process 0.5-1h, obtain high thermal conductivity graphene film.
Described biomaterial is the one in wild jujube, Kiwifruit, Herba lespedezae virgatae, Semen Cassiae, fresh jujube, sea-buckthorn, Herba amaranthi ascendentis, capsicum, big capsicums, clover, vicia unijuga, Herba Commelinae Bengalensis, concentrated orange juice, cabbage mustard, green pepper, leaf mustard leaf, Herba Houttuyniae, pea seedlings, rape a kind of sedge
Described solvent is deionized water, ethanol or the mixing solutions of the two;
The graphene film of described preparation reduction is that spontaneous evaporation is dry, the mode of vacuum-drying and cooked beans Beancurd sheet obtains.
Described spontaneous evaporation drying flat has in the open container of certain depth for the graphene oxide solution of reduction being poured into one, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, this method can reach the effect controlling film size and thickness further by the amount controlling solution.
Described vacuum-drying is pour in filter flask by the graphene oxide solution of reduction, utilize vacuum filtration or high pressure press filtration, or film suction filtration is done by the way taking the two to combine, and then the film of the moisture that is invisible to the naked eye at room temperature is carried out drying.
Described cooked beans Beancurd sheet is that the graphene oxide solution of the reduction of 4-8mg/mL is at 80-95 DEG C of thermostatically heating 1.5-3 hour by concentration, then the thing of film can be there is at the liquid level of solution, then the liquid below film is slowly toppled over away, film at room temperature drying gets final product film forming, and its thickness is by controlling strength of solution, Heating temperature and controlling heat-up time.
The temperature of described thermal anneal process is 200-400 DEG C.
Graphene film prepared by the present invention is a kind of brand-new functional materials, can conduct heat as one, dispel the heat, equal hot materials, for eliminating local pyrexia point, smoothed temperature gradient, it is lightweight, thickness is thin, good toughness, can with various gum and the good compound of insulation paper, and be die-cut to easily and variously need shape and size, thus well fit together with various metal, plastics.The fields such as smart mobile phone, panel computer, LED illumination device, intelligent television, pick up camera, digital camera, semiconductor manufacturing facility, vehicle electronics can be widely used in.
The present invention compared with prior art tool has the following advantages:
1. raw material sources used is extensive, natural environmental-protective;
2. moulding process is simply controlled, is easy to scale operation;
3. equipment used is extremely simple, and production cost is extremely low;
4. do not have the generation of toxic substance in preparation process, be beneficial to the health of operator.
Embodiment
Embodiment 1
Graphite oxide is made into the water-sol that concentration is 0.5mg/mL, through ultrasonic, obtains graphene oxide (GO) water-sol, squeeze broken by wild jujube stoning, itself and deionized water mixed diluting are obtained biomaterial slurry, and the concentration of slurry is 1mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:5, its mixing solutions is allowed to carry out reaction 48h at 25 DEG C, react rear spontaneous evaporation drying and forming-film, concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:66.Wherein by the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 8 μm, and thermal conductivity is 600Wm
-1k
-1, specific conductivity is 250Scm
-1, tensile strength is 20MPa, and tensile modulus is 4GPa.
Embodiment 2
Graphite oxide is made into the water-sol that concentration is 1.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Kiwifruit broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 2mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 800Wm
-1k
-1, specific conductivity is 300Scm
-1, tensile strength is 30MPa, and tensile modulus is 3.8GPa.
Embodiment 3
Graphite oxide is made into the water-sol that concentration is 1.5mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Herba lespedezae virgatae broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 3.5mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:7, allows its mixing solutions carry out reaction 40h at 60 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:26.4.By the film of gained thermal annealing 0.5h under 350 DEG C of argon gas atmosphere, gained film thickness is 20 μm, and thermal conductivity is 502Wm
-1k
-1, specific conductivity is 210Scm
-1, tensile strength is 21MPa, and tensile modulus is 3.9GPa.
Embodiment 4
Graphite oxide is made into the water-sol that concentration is 2.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Semen Cassiae broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 4.6mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:7, allows its mixing solutions carry out reaction 32h at 75 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:26.4.By the film of gained thermal annealing 0.5h under 280 DEG C of argon gas atmosphere, gained film thickness is 20 μm, and thermal conductivity is 600Wm
-1k
-1, specific conductivity is 260Scm
-1, tensile strength is 26MPa, and tensile modulus is 4.1GPa.
Embodiment 5
Graphite oxide is made into the water-sol that concentration is 2.5mg/mL, through ultrasonic, obtains graphene oxide (GO) water-sol, squeeze broken by fresh jujube, itself and deionized water mixed diluting are obtained biomaterial slurry, and the concentration of slurry is 6.4mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:8, allows its mixing solutions carry out reaction 5h at 85 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:25.1.By the film of gained thermal annealing 0.8h under 250 DEG C of argon gas atmosphere, gained film thickness is 21 μm, and thermal conductivity is 618Wm
-1k
-1, specific conductivity is 280Scm
-1, tensile strength is 28MPa, and tensile modulus is 3.7GPa.
Embodiment 6
Graphite oxide is made into the water-sol that concentration is 3.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by sea-buckthorn broken, itself and ethanol mixed diluting are obtained biomaterial slurry, the concentration of slurry is 7.5mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:10, allows its mixing solutions carry out reaction 1h at 90 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:24.By the film of gained thermal annealing 0.5h under 300 DEG C of argon gas atmosphere, gained film thickness is 22 μm, and thermal conductivity is 509Wm
-1k
-1, specific conductivity is 240Scm
-1, tensile strength is 24MPa, and tensile modulus is 4.3GPa.
Embodiment 7
Graphite oxide is made into the water-sol that concentration is 3.5mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Herba amaranthi ascendentis broken, itself and ethanol mixed diluting are obtained biomaterial slurry, the concentration of slurry is 8mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:9, allows its mixing solutions carry out reaction 10min at 100 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:24.Gained film thickness is 22 μm, and thermal conductivity is 240Wm
-1k
-1, specific conductivity is 180Scm
-1, tensile strength is 35MPa, and tensile modulus is 4.0GPa.
Embodiment 8
Graphite oxide is made into the water-sol that concentration is 4.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by capsicum broken, itself and ethanol mixed diluting are obtained biomaterial slurry, the concentration of slurry is 9.3mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:5, allows its mixing solutions carry out reaction 3.min at 88 DEG C, has reacted final vacuum suction filtration drying and forming-film.Concrete grammar is: pour in filter flask by the graphene oxide solution of reduction, utilizes vacuum filtration to be done by film suction filtration, then the film of the moisture that is invisible to the naked eye at room temperature is carried out drying.Wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of filter flask
2)=1:22.9.By the film of gained thermal annealing 0.7h under 350 DEG C of argon gas atmosphere, gained film thickness is 23 μm, and thermal conductivity is 300Wm
-1k
-1, specific conductivity is 190Scm
-1, tensile strength is 25MPa, and tensile modulus is 3.0GPa.
Embodiment 9
Graphite oxide is made into the water-sol that concentration is 4.5mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by big capsicums broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 11.5mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:9, allows its mixing solutions carry out reaction 2h at 78 DEG C, has reacted rear high pressure pressure-filteration drying film forming.Concrete grammar is: pour in filter flask by the graphene oxide solution of reduction, utilizes high pressure press filtration to be done by film suction filtration, then the film of the moisture that is invisible to the naked eye at room temperature is carried out drying.Wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of filter flask
2)=1:29.3.Gained film thickness is 18 μm, and thermal conductivity is 300Wm
-1k
-1, specific conductivity is 170Scm
-1, tensile strength is 29MPa, and tensile modulus is 3.0GPa.
Embodiment 10
Graphite oxide is made into the water-sol that concentration is 5.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by clover broken, itself and ethanol mixed diluting are obtained biomaterial slurry, the concentration of slurry is 12.4mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:9, allows its mixing solutions carry out reaction 6h at 65 DEG C, and combine vacuum filtration and high pressure press filtration after having reacted drying and forming-film.Concrete grammar is as follows: pour in filter flask by the graphene oxide solution of reduction, and film suction filtration is done by the way utilizing vacuum filtration and high pressure press filtration to combine, and then the film of the moisture that is invisible to the naked eye at room temperature is carried out drying.Wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of filter flask
2)=1:35.2.By the film of gained thermal annealing 0.7h under 210 DEG C of argon gas atmosphere, gained film thickness is 15 μm, and thermal conductivity is 300Wm
-1k
-1, specific conductivity is 198Scm
-1, tensile strength is 18MPa, and tensile modulus is 4.6GPa.
Embodiment 11
Graphite oxide is made into the water-sol that concentration is 5.5mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by vicia unijuga broken, itself and ethanol mixed diluting are obtained biomaterial slurry, the concentration of slurry is 13.6mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:8, allows its mixing solutions carry out reaction 15h at 44 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:35.2.By the film of gained thermal annealing 0.9h under 300 DEG C of argon gas atmosphere, gained film thickness is 18 μm, and thermal conductivity is 250Wm
-1k
-1, specific conductivity is 180Scm
-1, tensile strength is 15MPa, and tensile modulus is 4.7GPa.
Embodiment 12
Graphite oxide is made into the water-sol that concentration is 6.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Herba Commelinae Bengalensis broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 14.8mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, and allow its mixing solutions carry out reaction 3h at 80 DEG C, period obtains film by the mode of cooked beans Beancurd sheet, has reacted rear drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:35.2.Gained film thickness is 15 μm, and thermal conductivity is 300Wm
-1k
-1, specific conductivity is 150Scm
-1, tensile strength is 18MPa, and tensile modulus is 4.5GPa.
Embodiment 13
Graphite oxide is made into the water-sol that concentration is 6.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, orange juice will be concentrated and squeeze broken, the mixing solutions mixed diluting of itself and deionized water and ethanol is obtained biomaterial slurry, and the concentration of slurry is 16.7mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, and allow its mixing solutions carry out reaction 1.5h at 95 DEG C, period obtains film by the mode of cooked beans Beancurd sheet, has reacted rear drying and forming-film.Concrete grammar is as follows: the thing that can occur film between the mixing solutions reaction period at the liquid level of solution, then slowly toppled over away by the liquid below film, film at room temperature drying gets final product film forming.Gained film thickness is 16 μm, and thermal conductivity is 33.Wm
-1k
-1, specific conductivity is 160Scm
-1, tensile strength is 17MPa, and tensile modulus is 4.0GPa.
Embodiment 14
Graphite oxide is made into the water-sol that concentration is 6.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, cabbage mustard is squeezed broken, the mixing solutions mixed diluting of itself and deionized water and ethanol is obtained biomaterial slurry, and the concentration of slurry is 19.0mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, and allow its mixing solutions carry out reaction 3h at 90 DEG C, period obtains film by the mode of cooked beans Beancurd sheet, has reacted rear drying and forming-film.Concrete grammar is as follows: the thing that can occur film between the mixing solutions reaction period at the liquid level of solution, then slowly toppled over away by the liquid below film, film at room temperature drying gets final product film forming.Gained film thickness is 16 μm, and thermal conductivity is 200Wm
-1k
-1, specific conductivity is 120Scm
-1, tensile strength is 19MPa, and tensile modulus is 3.9GPa.
Embodiment 15
Graphite oxide is made into the water-sol that concentration is 6.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by green pepper broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 20.0mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 600Wm
-1k
-1, specific conductivity is 280Scm
-1, tensile strength is 3.3MPa, and tensile modulus is 2.3GPa.
Embodiment 16
Graphite oxide is made into the water-sol that concentration is 1.0mg/mL, through ultrasonic, obtains graphene oxide (GO) water-sol, squeeze broken by leaf mustard leaf, itself and deionized water mixed diluting are obtained biomaterial slurry, and the concentration of slurry is 2mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 700Wm
-1k
-1, specific conductivity is 280Scm
-1, tensile strength is 31MPa, and tensile modulus is 3.7GPa.
Embodiment 17
Graphite oxide is made into the water-sol that concentration is 1.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by Herba Houttuyniae broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 2mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 710Wm
-1k
-1, specific conductivity is 310Scm
-1, tensile strength is 31MPa, and tensile modulus is 3.8GPa.
Embodiment 18
Graphite oxide is made into the water-sol that concentration is 1.0mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol, squeezed by pea seedlings broken, itself and deionized water mixed diluting are obtained biomaterial slurry, the concentration of slurry is 2mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 600Wm
-1k
-1, specific conductivity is 280Scm
-1, tensile strength is 32MPa, and tensile modulus is 3.4GPa.
Embodiment 19
Graphite oxide is made into the water-sol that concentration is 1.0mg/mL, through ultrasonic, obtains graphene oxide (GO) water-sol, squeeze broken by rape a kind of sedge, itself and deionized water mixed diluting are obtained biomaterial slurry, and the concentration of slurry is 2mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain its filtrate, seal stand-by; Mix with graphene oxide colloidal sol with above-mentioned biomaterial filtrate, wherein the mass ratio of slurry and graphite oxide is 1:6, allows its mixing solutions carry out reaction 46h at 40 DEG C, has reacted rear spontaneous evaporation drying and forming-film.Concrete grammar is as follows: the graphene oxide solution of reduction being poured into one flat has in the open container of certain depth, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film, wherein comprise the amount (mg) of graphene oxide in solution: the floorage (mm of container
2)=1:52.8.By the film of gained thermal annealing 0.5h under 400 DEG C of argon gas atmosphere, gained film thickness is 10 μm, and thermal conductivity is 600Wm
-1k
-1, specific conductivity is 290Scm
-1, tensile strength is 35MPa, and tensile modulus is 3.0GPa.
Claims (8)
1. prepare a method for graphene-based heat conduction film, it is characterized in that comprising the steps:
(1) prepare graphite oxide, graphite oxide is made into the water-sol that concentration is 0.5-6mg/mL, through ultrasonic, obtain graphene oxide (GO) water-sol;
(2) biomaterial is stirred squeezing broken, itself and solvent are diluted and obtain biomaterial slurry, the concentration of slurry is 1-20mg/mL; By the ultrasonic suction filtration of biomaterial slurry obtained, obtain biomaterial filtrate;
(3) be 1:5-10 by the mass ratio of graphite oxide and biological slurry, biomaterial filtrate is mixed with the graphene oxide water-sol, in room temperature-100
ocarry out 10min-48h reaction at C temperature, react the graphene film of rear preparation reduction;
(4) by gained graphene film at argon gas atmosphere thermal anneal process 0.5-1h, obtain high thermal conductivity graphene film.
2. a kind of method preparing graphene-based heat conduction film as claimed in claim 1, is characterized in that described biomaterial is the one in wild jujube, Kiwifruit, Herba lespedezae virgatae, Semen Cassiae, fresh jujube, sea-buckthorn, Herba amaranthi ascendentis, capsicum, big capsicums, clover, vicia unijuga, Herba Commelinae Bengalensis, concentrated orange juice, cabbage mustard, green pepper, leaf mustard leaf, Herba Houttuyniae, pea seedlings, rape a kind of sedge.
3. a kind of method preparing graphene-based heat conduction film as claimed in claim 1, is characterized in that described solvent is deionized water, ethanol or the mixing solutions of the two.
4. a kind of method preparing graphene-based heat conduction film as claimed in claim 1, is characterized in that the graphene film of described preparation reduction is that spontaneous evaporation is dry, the mode of vacuum-drying or cooked beans Beancurd sheet obtains.
5. a kind of method preparing graphene-based heat conduction film as claimed in claim 4, it is characterized in that described spontaneous evaporation drying flat has in the open container of certain depth for the graphene oxide solution of reduction being poured into one, and then under room temperature condition, allow it evaporate, make the graphene oxide lamella be left be assembled into film.
6. a kind of method preparing graphene-based heat conduction film as claimed in claim 4, it is characterized in that described vacuum-drying is pour in filter flask by the graphene oxide solution of reduction, utilize vacuum filtration or high pressure press filtration, or film suction filtration is done by the way taking the two to combine, and then the film of the moisture that is invisible to the naked eye at room temperature is carried out drying.
7. a kind of method preparing graphene-based heat conduction film as claimed in claim 4, it is characterized in that described cooked beans Beancurd sheet is is that the graphene oxide solution of the reduction of 4-8 mg/mL is at 80-95 DEG C of thermostatically heating 1.5-3 hour by concentration, then the thing of film can be there is at the liquid level of solution, then slowly toppled over away by the liquid below film, film at room temperature drying gets final product film forming.
8. a kind of method preparing graphene-based heat conduction film as claimed in claim 1, is characterized in that the temperature of described thermal anneal process is 200-400
oc.
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