CN107022345A - Preparation method, composite and the application of graphene/graphite powder composite material - Google Patents
Preparation method, composite and the application of graphene/graphite powder composite material Download PDFInfo
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- CN107022345A CN107022345A CN201710202806.2A CN201710202806A CN107022345A CN 107022345 A CN107022345 A CN 107022345A CN 201710202806 A CN201710202806 A CN 201710202806A CN 107022345 A CN107022345 A CN 107022345A
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Abstract
The present invention relates to preparation method, composite and the application of graphene/graphite powder composite material, using graphene oxide dispersion liquid and graphite powder as raw material, graphene oxide surface is with functional groups such as hydroxyl, carboxyls, there is good dispersiveness in water equal solvent, can also improve its interface fusion with graphite powder.Both are mutually mixed by high-speed stirred, ultrasonic disperse is uniform, spray-dried, preexpanding and high-temperature process, graphene oxide is reduced to graphene, obtain graphene/graphite powder composite material.Using this composite as heat filling, composite is formed with the cubical array of orientation in the base by structure control, prepare anisotropic high thermal conductivity composite.Fully overlapped between high filler loading capacity graphene composite material, reduce interface resistance, its heat conductivility exceedes some common alloys, has great potential in heat conduction application field.
Description
Technical field
The invention belongs to technical field of material, and in particular to the preparation method of graphene/graphite powder composite material, multiple
Condensation material and application.
Background technology
Graphene (graphene), is the tightly packed carbonaceous material into individual layer bi-dimensional cellular shape lattice structure of sp2 carbon atoms
Material, can be regarded as other dimension carbon materials, such as fullerene (0 dimension), the elementary cell of CNT (1 dimension) graphite (3-dimensional).By
Possessing in it has numerous excellent performances, such as excellent carrier mobility (10000cm-2s-1) and thermal conductivity (5000Wm-1K-1), as one of current material of greatest concern, substantial amounts of research is put in the application of graphene.Graphene goes out
It is existing, bring hope to high dielectric and high heat conduction field.
Composite, is with two or more material of different nature, by method physically or chemically, grand
Sight/microcosmic upper material of the composition with new capability.Various materials make up for each other's deficiencies and learn from each other in performance, produce cooperative effect, make multiple
The combination property of condensation material is better than former composition material, so as to meet various requirement.
Graphene and graphite powder all have good heat conductivility, but two kinds of materials are differed due to structure, its heat conduction
There is also larger difference for principle.Graphene and graphite powder are the carbon material of excellent thermal conductivity, in order to further enhance difference
A little, the present invention combines graphene and graphite powder to material, prepares the composite wood that a kind of performance is better than any homogenous material
Material.But graphene is insoluble in water and conventional organic solvent, this also causes pole to the preparation and application of graphene composite material
It is big difficult.
The content of the invention
First purpose of the present invention is the preparation method for providing graphene/graphite powder composite material.
Technical scheme is as follows:
The preparation method of a kind of graphene/graphite powder composite material, using graphene oxide dispersion liquid and graphite powder as original
Material, graphene oxide surface has good dispersiveness in water equal solvent, can also changed with functional groups such as hydroxyl, carboxyls
It is apt to its interface fusion with graphite powder.Both are mutually mixed by high-speed stirred, ultrasonic disperse is uniform, spray-dried,
Preexpanding and high-temperature process, graphene oxide are reduced to graphene, obtain graphene/graphite powder composite material.
The graphene oxide aqueous dispersions concentration is 1mg/mL~10mg/mL.
The particle diameter of the graphite powder is more than 300nm.
The high-speed stirred speed is 2000~20000r/min.
The ultrasonic time is 1~10h.
The inlet temperature of the spray drying device is 90 DEG C, and outlet temperature is 200 DEG C.
The protective gas used in the high-temperature process is one kind in ammonia, nitrogen, argon gas.
The calcining heat is 400~1000 DEG C.
Second object of the present invention uses the composite of above method preparation to provide.
Third object of the present invention is the application for providing above-mentioned material in field of radiating.
The beneficial effects of the invention are as follows:When the heat conduction carbon material of two kinds of different-grain diameters of graphene and graphite powder is mixed, lead
The collocation of hot material has a significant effect to improving heat conductivility, during Heat Conduction Material different-grain diameter changes in distribution, system heat conductivility
Development pattern changes, and the composite of high thermal conductivity is can obtain when particle diameter distribution is appropriate.Using this composite
As heat filling, composite is formed with the cubical array of orientation in the base by structure control, prepare anisotropy
High thermal conductivity composite.Fully overlapped between high filler loading capacity graphene composite material, reduce interface resistance, its thermal conductivity
Some common alloys are can exceed that, there is great potential in heat conduction application field.
Embodiment
Technical scheme is further illustrated below by embodiment, the embodiment is only to aid in
Understand the present invention, be not construed as the concrete restriction to the present invention.
Embodiment 1
(1) graphene oxide aqueous dispersions and the blending of the mesh graphite powders of 2g 80 that 1L concentration is 1g/L are taken;
(2) high speed shear dispersion machine is utilized, regulation rotating speed is 3000r/min, and the blend of step (1) is stirred into 2h, then
Finely dispersed mixed liquor is subjected to ultrasonic disperse, ultrasonic time is 2h;
(3) ultrasonically treated mixed liquor is spray-dried, the inlet temperature for setting spray drying device is 90 DEG C, is gone out
Mouth temperature is 200 DEG C, obtains solid powder;
(4) gained powder is carried out after preexpanding process, high-temperature calcination, calcining heat is carried out under protective gas atmosphere
For 800 DEG C, after cooling, the composite that graphene/graphite powder is constituted is obtained.
Embodiment 2
(1) graphene oxide aqueous dispersions and the blending of the mesh graphite powders of 2g 100 that 1L concentration is 2g/L are taken;
(2) high speed shear dispersion machine is utilized, regulation rotating speed is 5000r/min, and the blend of step (1) is stirred into 2h, then
Finely dispersed mixed liquor is subjected to ultrasonic disperse, ultrasonic time is 2h;
(3) ultrasonically treated mixed liquor is spray-dried, the inlet temperature for setting spray drying device is 90 DEG C, is gone out
Mouth temperature is 200 DEG C, obtains solid powder;
(4) gained powder is carried out after preexpanding process, high-temperature calcination, calcining heat is carried out under protective gas atmosphere
For 800 DEG C, after cooling, the composite that graphene/graphite powder is constituted is obtained.
Embodiment 3
(1) graphene oxide aqueous dispersions and the blending of the mesh graphite powders of 2g 325 that 1L concentration is 5g/L are taken;
(2) high speed shear dispersion machine is utilized, regulation rotating speed is 5000r/min, and the blend of step (1) is stirred into 4h, then
Finely dispersed mixed liquor is subjected to ultrasonic disperse, ultrasonic time is 4h;
(3) ultrasonically treated mixed liquor is spray-dried, the inlet temperature for setting spray drying device is 90 DEG C, is gone out
Mouth temperature is 200 DEG C, obtains solid powder;
(4) gained powder is carried out after preexpanding process, high-temperature calcination, calcining heat is carried out under protective gas atmosphere
For 800 DEG C, after cooling, the composite that graphene/graphite powder is constituted is obtained.
Embodiment 4
(1) graphene oxide aqueous dispersions and the blending of the mesh graphite powders of 5g 1200 that 1L concentration is 5g/L are taken;
(2) high speed shear dispersion machine is utilized, regulation rotating speed is 5000r/min, and the blend of step (1) is stirred into 4h, then
Finely dispersed mixed liquor is subjected to ultrasonic disperse, ultrasonic time is 2h;
(3) ultrasonically treated mixed liquor is spray-dried, the inlet temperature for setting spray drying device is 90 DEG C, is gone out
Mouth temperature is 200 DEG C, obtains solid powder;
(4) gained powder is carried out after preexpanding process, high-temperature calcination, calcining heat is carried out under protective gas atmosphere
For 800 DEG C, after cooling, the composite that graphene/graphite powder is constituted is obtained.
Embodiment 5
(1) graphene oxide aqueous dispersions and the blending of the mesh graphite powders of 5g 8000 that 1L concentration is 10g/L are taken;
(2) high speed shear dispersion machine is utilized, regulation rotating speed is 10000r/min, and the blend of step (1) is stirred into 4h, then
Finely dispersed mixed liquor is subjected to ultrasonic disperse, ultrasonic time is 4h;
(3) ultrasonically treated mixed liquor is spray-dried, the inlet temperature for setting spray drying device is 90 DEG C, is gone out
Mouth temperature is 200 DEG C, obtains solid powder;
(4) gained powder is carried out after preexpanding process, high-temperature calcination, calcining heat is carried out under protective gas atmosphere
For 800 DEG C, after cooling, the composite that graphene/graphite powder is constituted is obtained.
Application examples
The composite that embodiment 1~5 is prepared is added separately in certain heat radiation coating product that (radiating efficiency is about
For 10%), coating is sprayed in tinplate sheet, it is heated to after certain temperature, radiating and cooling is carried out under closed experiment condition
Measure of merit, test result is as shown in table 1.
Comparative example 1~5
80 mesh, 100 mesh, 325 mesh, 1200 mesh, 8000 mesh graphite powders are added separately in certain heat radiation coating product, will
Coating is sprayed in tinplate sheet, is heated to after certain temperature, and radiating and cooling measure of merit is carried out under closed experiment condition, is surveyed
Test result is as shown in table 1.
The heat dispersion test result of table 1
As can be seen that graphite powder has good heat conductivility from comparative example 1-5 test result, graphite powder is added
The radiating efficiency of coating can be further improved into heat radiation coating.The test data of comparative example and comparative example, can see
Go out, with the addition of the heat radiation coating of graphene and graphite powder composite material, than the coating radiating efficiency for adding single graphite powder material
At least it is enhanced about more than once.Therefore, by the carbon material combination of both excellent thermal conductivities of graphene and graphite powder, prepare
Composite further enhancing the advantage of two kinds of materials, and its heat conductivility is better than homogenous material.
Claims (10)
1. the preparation method of a kind of graphene/graphite powder composite material, it is characterised in that with graphene oxide aqueous dispersions and stone
Ink powder is that raw material is mutually mixed both by high-speed stirred, and ultrasonic disperse is uniform, spray-dried, preexpanding and high-temperature process
Process, graphene oxide is reduced to graphene, obtains graphene/graphite powder composite material.
2. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
Graphene oxide aqueous dispersions concentration is 1mg/mL~10mg/mL.
3. the preparation method of a kind of graphene/graphite powder composite material according to claim 2, it is characterised in that described
The particle diameter of graphite powder is more than 300nm.
4. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
High-speed stirred speed is 2000~20000r/min.
5. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
Ultrasonic time is 1~10h.
6. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
The inlet temperature of spray drying device is 90 DEG C, and outlet temperature is 200 DEG C.
7. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
The protective gas used in high-temperature process is one kind in ammonia, nitrogen, argon gas.
8. the preparation method of a kind of graphene/graphite powder composite material according to claim 1, it is characterised in that described
Calcining heat is 400~1000 DEG C.
9. the composite prepared according to any methods describeds of claim 1-8.
10. composite described in claim 9 is used as the application of heat sink material.
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Cited By (4)
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CN109777372A (en) * | 2019-01-31 | 2019-05-21 | 广东思泉新材料股份有限公司 | A kind of high thermal conductivity membrane preparation method |
WO2020145298A1 (en) * | 2019-01-09 | 2020-07-16 | 日本電気株式会社 | Reduced graphene oxide-graphite composite material, method for producing same, and lithium ion secondary battery using same |
CN111960722A (en) * | 2020-09-04 | 2020-11-20 | 南通三圣石墨设备科技股份有限公司 | Graphite tube material for uniformly dispersing graphene oxide and preparation method |
CN112812534A (en) * | 2020-12-31 | 2021-05-18 | 广东墨睿科技有限公司 | Preparation method of heat-conducting graphene PC composite material |
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CN105016731A (en) * | 2015-07-09 | 2015-11-04 | 天津大学 | Expanded graphite and graphene composite material and preparation method therefor |
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CN103449423A (en) * | 2013-08-27 | 2013-12-18 | 常州第六元素材料科技股份有限公司 | Graphene heat conducting membrane and preparation method thereof |
CN104229783A (en) * | 2014-09-10 | 2014-12-24 | 浙江碳谷上希材料科技有限公司 | Preparation method of graphene film with high thermal conductivity |
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Cited By (6)
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WO2020145298A1 (en) * | 2019-01-09 | 2020-07-16 | 日本電気株式会社 | Reduced graphene oxide-graphite composite material, method for producing same, and lithium ion secondary battery using same |
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CN109777372A (en) * | 2019-01-31 | 2019-05-21 | 广东思泉新材料股份有限公司 | A kind of high thermal conductivity membrane preparation method |
CN111960722A (en) * | 2020-09-04 | 2020-11-20 | 南通三圣石墨设备科技股份有限公司 | Graphite tube material for uniformly dispersing graphene oxide and preparation method |
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Application publication date: 20170808 |