CN102897753B - Preparation method for graphite with high thermal conductivity - Google Patents
Preparation method for graphite with high thermal conductivity Download PDFInfo
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- CN102897753B CN102897753B CN201210335389.6A CN201210335389A CN102897753B CN 102897753 B CN102897753 B CN 102897753B CN 201210335389 A CN201210335389 A CN 201210335389A CN 102897753 B CN102897753 B CN 102897753B
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- graphite
- preparation
- high conductive
- thermal conductivity
- conductive graphite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 97
- 239000010439 graphite Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000000138 intercalating agent Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 230000002687 intercalation Effects 0.000 claims description 20
- 238000009830 intercalation Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000007493 shaping process Methods 0.000 claims description 8
- 238000009417 prefabrication Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011302 mesophase pitch Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000011280 coal tar Substances 0.000 claims description 2
- 239000011294 coal tar pitch Substances 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000002893 slag Substances 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000005087 graphitization Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000007770 graphite material Substances 0.000 description 14
- 241000611009 Nematalosa come Species 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method for graphite with high thermal conductivity. The preparation method is characterized by comprising the following steps: weighing natural crystalline flake graphite with a size of no less than 400 meshes and mixing the crystalline flake graphite with an intercalator to obtain intercalated graphite; subjecting the intercalated graphite to expansion at a temperature of 200 to 1100 DEG C to obtain expanded graphite, wherein an expansion ratio is set to be 1.5 to 2.0 times; soaking the expanded graphite with a liquid carbon source, taking the expanded graphite out, heating the expanded graphite to a temperature of 500 to 1000 DEG C in a manner of hot pressing with pressure controlled to be 5 to 100 MPa and taking the heated graphite out from a kettle after cooling so as to obtain intermediate graphite; and placing the intermediate graphite in a graphitization furnace, heating the intermediate graphite to a temperature of 2000 to 3000 DEG C in inert gas flow and taking the heated intermediate graphite out after cooling so as to obtain finished graphite. According to the invention, the prepared graphite has high thermal conductivity (350 to 650 W/mK); and after slight expansion, the crystalline flake graphite has a small particle size and a firm structure, so the phenomenon of slag falling of graphite with high thermal conductivity can be well overcome.
Description
Technical field
The present invention relates to a kind of graphite its preparation method with high heat conduction feature.
Background technology
Along with the development of electronic technology and Aeronautics and Astronautics technology, the miniaturization of electronics trend, Highgrade integration, for ensureing the steady-state operation of high power density electronic equipment and miniature/small-sized integrated functionality system, to the heat strengthening derivation that its operational process produces, higher requirement will inevitably be proposed.Therefore various countries researchist has carried out large quantity research for thermally conductive material.Graphite material as a kind of there is high thermal conductivity, the material of lightweight is studied widely, is a kind of material in this field with very large potentiality.But at present, general complex process in the preparation process of high-heat conductivity graphite material, and its material structure and the more difficult control of performance, thus need to research and develop new preparation path further.
Existing solution has use natural flake graphite as starting material to prepare high conductive graphite, because natural flake graphite itself has high thermal conductivity.But the particle sintering the material of rear preparation due to crystalline flake graphite under the effect of binding agent is larger, the phenomenon of the slag that comes off, falls is there will be in further use procedure, its heat conductivility so can be caused to decline and even lost efficacy, so this defect use that natural flake graphite prepares high conductive graphite technique limits its widespread use.With regard to this kind of technique, overcoming the slag-off phenomenon of goods, thus widen the range of application of high conductive graphite while how keeping the high heat conduction of natural flake graphite, is be problem demanding prompt solution.
Summary of the invention
For the above-mentioned technique utilizing natural flake graphite to prepare high conductive graphite in conjunction with insecure, easy fall the defect of slag, inefficacy, the present invention proposes a kind of preparation method of high conductive graphite, and its technical scheme is as follows:
A preparation method for high conductive graphite, comprises the following steps:
Intercalation: get particle and be not less than 400 object natural flake graphites, be mixed into intercalator, obtain intercalated graphite;
Expand: carry out expansion process under this intercalated graphite being placed in 200-1100 ° of C, setting its expansion multiple is 1.5-20 times, obtains expanded graphite;
Prefabricated: to take out after this expanded graphite is soaked into liquid carbon source, be heated to 500-1000 ° of C by the mode of hot pressing, pressure-controlling, in 5-100MPa, then goes out still after cooling, obtains middle graphite; And
Shaping: this middle graphite is placed in a graphitizing furnace, and under inert gas flow, be heated to 2000-3000 ° of C, finally cooling is come out of the stove and is namely obtained finished product graphite.
As the preferred person of the technical program, improvement can be had in following:
In preferred embodiment, in this intercalation step, this intercalator comprises: the mixture of iron(ic) chloride, cobalt chloride, nickelous chloride, the vitriol oil-concentrated nitric acid, organic intercalation agent and two or more mixture thereof.
In preferred embodiment, in this prefabrication step, this liquid carbon source comprises: coal tar, coal-tar pitch, petroleum residual oil, CONPA resin, mesophase pitch and two or more mixture thereof.
In preferred embodiment, this rare gas element is argon gas.
In preferred embodiment, in this prefabrication step, after hot pressing heating, the mode of naturally cooling is taked to go out still.
In preferred embodiment, in this forming step, the mode of naturally cooling after heating, is taked to come out of the stove.
In preferred embodiment, in this prefabrication step, its heat-processed has atmosphere of inert gases.
In preferred embodiment, in this forming step, the uniform rate of 1-50 ° of C/min is adopted to heat up to the heating of this middle graphite.
The beneficial effect of the technical program is:
1. the process of intercalation and expansion step, regulate the expansion multiple of natural flake graphite, regulate the arrangement behavior of graphite microcrystal, and under hot pressing function, binding agent and expanded graphite chip array regular, in forming step, after further greying, there is higher thermal conductivity (350-650W/mK).
2. crystalline flake graphite is through microdilatancy, and its particle diameter is less, sound construction, thus can overcome the slag-off phenomenon of high conductive graphite preferably.
3. from above-mentioned material used in steps, the advantages such as it is extensive that the present invention has raw material sources, cheap, with short production cycle.
Accompanying drawing explanation
Below in conjunction with accompanying drawing embodiment, the invention will be further described:
Fig. 1 is the schema of the embodiment of the present invention 1 to embodiment 6.
Embodiment
Embodiment 1
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: after at 200-1100 DEG C expansion process, obtain the microdilatancy graphite that expansion multiple is 1.5 times.
Prefabricated 30: expanded graphite is immersed liquid charcoal source mesophase pitch.Be placed on after soaking into taking-up in hot pressing furnace, under an inert atmosphere, with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains prefabricated graphite.
Shaping 40: prefabricated graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 2.20g/cm3, and thermal conductivity is 650W/mK.
Embodiment 2
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: after at 200-1100 DEG C expansion process, obtain the expanded graphite that expansion multiple is 3 times.
Prefabricated 30: take out after expanded graphite being immersed liquid charcoal source and obtain initial goods.Initial goods are placed in hot pressing furnace under an inert atmosphere, and with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains the prefabricated graphite of intermediate.
Shaping 40: prefabricated for intermediate graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 2.12g/cm3, and thermal conductivity is 542W/mK.
Embodiment 3
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: expansion process at 200-1100 DEG C, obtains the microdilatancy crystalline flake graphite that expansion multiple is 5 times.
Prefabricated 30: take out after microdilatancy crystalline flake graphite is immersed liquid charcoal source and obtain initial goods.Afterwards initial goods are placed in hot pressing furnace under an inert atmosphere by initial goods, with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains the prefabricated graphite of intermediate.
Shaping 40: prefabricated for intermediate graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 2.04g/cm3, and thermal conductivity is 485W/mK.
Embodiment 4
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: expansion process at 200-1100 DEG C, obtains the expanded graphite that expansion multiple is 8 times.
Prefabricated 30: will: take out after expanded graphite immerses liquid charcoal source and obtain initial goods.Afterwards initial goods are placed in hot pressing furnace under an inert atmosphere by initial goods, with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains the prefabricated graphite of intermediate
Shaping 40: prefabricated for intermediate graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 1.94g/cm3, and thermal conductivity is 448W/mK.
Embodiment 5
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: after at 200-1100 DEG C expansion process, obtain the expanded graphite that expansion multiple is 10 times.
Prefabricated 30: take out after expanded graphite being immersed liquid charcoal source and obtain initial goods.Afterwards initial goods are placed in hot pressing furnace under an inert atmosphere by initial goods, with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains the prefabricated graphite of intermediate.
Shaping 40: prefabricated for intermediate graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 1.92g/cm3, and thermal conductivity is 415W/mK.
Embodiment 6
Intercalation 10: get particle diameter and be not less than 400 object natural flake graphite 200g, be mixed into the vitriol oil-concentrated nitric acid mixture as intercalator, intercalation processing;
Expand 20: after at 200-1100 DEG C expansion process, obtain the expanded graphite that expansion multiple is 20 times.
Prefabricated 30: take out after microdilatancy crystalline flake graphite is immersed liquid charcoal source and obtain initial goods.Afterwards initial goods are placed in hot pressing furnace under an inert atmosphere by initial goods, with the heat-up rate of 0.1 ~ 100 DEG C/min, pressure is 5-100MPa, initial goods is heated to 600 DEG C ~ 2000 DEG C and obtains the prefabricated graphite of intermediate.
Shaping 40: prefabricated for intermediate graphite is placed in a graphitizing furnace under argon gas stream, with the heat-up rate of 1 ~ 50 DEG C/min, intermediate is heated to 2000 DEG C ~ 3000 DEG C.Come out of the stove after naturally cooling and namely obtain high-heat conductivity graphite material.The density of the graphite material obtained is at 1.90g/cm3, and thermal conductivity is 354W/mK.
In above-described embodiment, by the process of intercalation and expansion step, regulate the expansion multiple of natural flake graphite, regulate the arrangement behavior of graphite microcrystal, and under hot pressing function, binding agent and expanded graphite chip array regular, in forming step, after further greying, there is higher thermal conductivity (350-650W/mK).Because crystalline flake graphite is through microdilatancy, its particle diameter is less, sound construction, thus can overcome the slag-off phenomenon of high conductive graphite preferably.On the other hand, from above-mentioned material used in steps, the advantages such as it is extensive that the present invention has raw material sources, cheap, with short production cycle.
The above, be only present pre-ferred embodiments, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (8)
1. a preparation method for high conductive graphite, is characterized in that: comprise the following steps:
Intercalation: get particle and be not less than 400 object natural flake graphites, be mixed into intercalator, obtain intercalated graphite;
Expand: carry out expansion process under this intercalated graphite being placed in 200-1100 ° of C, setting its expansion multiple is 1.5-20 times, obtains expanded graphite;
Prefabricated: to take out after this expanded graphite is soaked into liquid carbon source, be heated to 500-1000 ° of C by the mode of hot pressing, pressure-controlling, in 5-100MPa, then goes out still after cooling, obtains middle graphite; And
Shaping: this middle graphite is placed in a graphitizing furnace, and under inert gas flow, be heated to 2000-3000 ° of C, finally cooling is come out of the stove and is namely obtained finished product graphite.
2. the preparation method of a kind of high conductive graphite according to claim 1, it is characterized in that: in this intercalation step, this intercalator comprises: the mixture of iron(ic) chloride, cobalt chloride, nickelous chloride, the vitriol oil-concentrated nitric acid, organic intercalation agent and two or more mixture thereof.
3. the preparation method of a kind of high conductive graphite according to claim 1, it is characterized in that: in this prefabrication step, this liquid carbon source comprises: coal tar, coal-tar pitch, petroleum residual oil, CONPA resin, mesophase pitch and two or more mixture thereof.
4. a kind of preparation method of high conductive graphite according to any one of claims 1 to 3, is characterized in that: this rare gas element is argon gas.
5. the preparation method of a kind of high conductive graphite according to claim 1, is characterized in that: in this prefabrication step, takes the mode of naturally cooling to go out still after hot pressing heating.
6. the preparation method of a kind of high conductive graphite according to claim 1, is characterized in that: in this forming step, takes the mode of naturally cooling to come out of the stove after heating.
7. the preparation method of a kind of high conductive graphite according to claim 1, it is characterized in that: in this prefabrication step, its heat-processed has atmosphere of inert gases.
8. the preparation method of a kind of high conductive graphite according to claim 1, is characterized in that: in this forming step, adopts the uniform rate of 1-50 ° of C/min to heat up to the heating of this middle graphite.
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| CN201210335389.6A CN102897753B (en) | 2012-09-11 | 2012-09-11 | Preparation method for graphite with high thermal conductivity |
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| CN201210335389.6A CN102897753B (en) | 2012-09-11 | 2012-09-11 | Preparation method for graphite with high thermal conductivity |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104003373B (en) * | 2013-02-21 | 2016-06-29 | 海洋王照明科技股份有限公司 | A kind of grapheme material and preparation method thereof |
| CN103450857A (en) * | 2013-09-05 | 2013-12-18 | 中国科学院青岛生物能源与过程研究所 | Composite graphite heat-conducting membrane material with controllable heat conductivity and preparation process thereof |
| CN104943223B (en) * | 2015-06-17 | 2016-09-07 | 天津大学 | There is graphite flake and the preparation method of high thermal conductivity coefficient along plane and thickness direction simultaneously |
| CN110265850B (en) * | 2019-07-23 | 2021-06-25 | 自贡恒基电碳厂 | Preparation method of electric brush for motor and obtained electric brush |
| CN116081616B (en) * | 2022-12-30 | 2024-06-11 | 湛江市聚鑫新能源有限公司 | Low-sulfur high-expansion-temperature expandable graphite and preparation method and application thereof |
| CN116534854B (en) * | 2023-04-25 | 2024-05-10 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
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| CN101538036B (en) * | 2009-04-28 | 2011-01-05 | 中国科学院山西煤炭化学研究所 | Method for preparing high thermal conductivity graphite material |
| CN102516952A (en) * | 2011-11-14 | 2012-06-27 | 苏州市达昇电子材料有限公司 | Method for preparing composite film sheet material from organic silicon and graphite |
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| CN100387517C (en) * | 2005-06-03 | 2008-05-14 | 中国矿业大学（北京校区） | High heat conducting foam material of graphite, and fabricating method |
| CN101456553B (en) * | 2007-12-11 | 2011-12-28 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
| WO2010079291A2 (en) * | 2009-01-12 | 2010-07-15 | Centre National De La Recherche Scientifique | Method for preparing graphenes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101538036B (en) * | 2009-04-28 | 2011-01-05 | 中国科学院山西煤炭化学研究所 | Method for preparing high thermal conductivity graphite material |
| CN102516952A (en) * | 2011-11-14 | 2012-06-27 | 苏州市达昇电子材料有限公司 | Method for preparing composite film sheet material from organic silicon and graphite |
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