CN1872677A - High heat conducting foam material of graphite, and fabricating method - Google Patents
High heat conducting foam material of graphite, and fabricating method Download PDFInfo
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- CN1872677A CN1872677A CN 200510073394 CN200510073394A CN1872677A CN 1872677 A CN1872677 A CN 1872677A CN 200510073394 CN200510073394 CN 200510073394 CN 200510073394 A CN200510073394 A CN 200510073394A CN 1872677 A CN1872677 A CN 1872677A
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- high heat
- heat conducting
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000010439 graphite Substances 0.000 title claims abstract description 41
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 41
- 239000006261 foam material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 29
- 239000010426 asphalt Substances 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000013022 venting Methods 0.000 claims description 26
- 238000010792 warming Methods 0.000 claims description 25
- 239000011302 mesophase pitch Substances 0.000 claims description 24
- 239000006260 foam Substances 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 239000011280 coal tar Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000003208 petroleum Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000011800 void material Substances 0.000 claims description 7
- 239000011294 coal tar pitch Substances 0.000 claims description 3
- 235000019628 coolness Nutrition 0.000 claims description 3
- 239000011301 petroleum pitch Substances 0.000 claims description 3
- 238000007669 thermal treatment Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000005187 foaming Methods 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000011295 pitch Substances 0.000 description 4
- 230000000740 bleeding effect Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
This invention discloses a method for manufacturing high heat-conductive graphite foam material. The method comprises: (1) heating asphalt in a reactor at 1-5 deg.C/min to 260-400 deg.C; (2) pressurizing to 2-6 MPa; (3) heating at 1-2 deg.C/min to 350-550 deg.C; (4) keeping the temperature for 15-120 min, and discharging the gas to obtain asphalt foam material; (5) heating to 950-1100 deg.C under nitrogen protection to obtain carbonized asphalt foam material; (6) heating to 2600-3000 deg.C under nitrogen protection for carbonization, and cooling naturally to obtain high heat-conductive graphite foam material. The pore sizes are 80-800 mum, the density is 0.28-0.75 g/cu cm, the porosity is 55-85%, and the heat conductivity is 68-140 W/mK. The high heat-conductive graphite foam material can be widely used in radiator, heat exchanger, automobile, airplane brake block, catalyst carrier, gas adsorbent and composite material.
Description
Technical field
The present invention relates to a kind of high conductive graphite foam (graphite foam) and high conductive graphite foamy manufacture method.
Background of invention
The charcoal foam uses in various application, and described application comprises as thermal insulation/lagging material, the conductive filler material that is used for polymkeric substance or plastics, electrode and structured material etc.Charcoal foam with high surface area and high porosity obtains embodying in a lot of these application and other application.
Known have make charcoal foamy the whole bag of tricks, comprise and use coal or pitch high pressure nitriding foaming, or use raw materials such as coal, pitch, polyethylene by the whipping agent foaming etc., then this porous form is at high temperature solidified, so that obtain the charcoal foam.
The charcoal foamy thermal conductivity extreme difference that above charcoal foam and preparation method obtain generally can only be used as lagging material or structured material.
People such as U.S. Oak Ridge laboratory James.Klett announced that the method for the volatilization autoreaction foaming that utilizes low molecular compound in the mesophase pitch heat-processed prepared graphited Carbon foam in 1997, the aperture average out to 300um of Carbon foam, and have the higher specific tenacity and the capacity of heat transmission (US Patent 6033506).What they adopted is that temperature and pressure is reduced to room temperature and non-pressurized method simultaneously, and the Carbon foam void content of preparation is lower, and density is higher.
People such as the mound Jieshan of Dalian University of Technology had applied for utilizing coal tar mid-temperature pitch and petroleum pitch to prepare the patent of Carbon foam method in 2003, but raw materials usedly all must adopt the metal-salt upgrading, adopt the method for naturally cooling to prepare Carbon foam, specifically do not put the pressure mode and announce.The Yu Ming of Donghua University virtues etc. were applied for a kind of method of utilizing mechanical expressing technique to prepare Carbon foam in 2004, but preparation process need be added whipping agent.
The present invention utilizes coal tar mesophase pitch, oil mesophase pitch or synthetic asphalts to be raw material, does not need to carry out upgrading, does not also need to add whipping agent, utilizes under the high pressure to prepare high conductive graphite foam from the principle that foams.By different gas release modes, realize that hole bubble size and pore wall thickness are controlled, finally obtain the graphite foam of controlled density, porosity, product density and porosity ranges are wide, can better adapt to the requirement of different purposes.
Summary of the invention
The purpose of this invention is to provide a kind of high heat conducting foam material of graphite, this high heat conducting foam material of graphite has large surface area, higher mechanical strength, particularly has high thermal conductivity;
Another purpose of the present invention provides a kind of preparation method of high heat conducting foam material of graphite, and this method does not need that raw material is added catalyzer and carries out upgrading, and foaming process also need not whipping agent, low cost of manufacture; Put pressure by different venting modes, realize density and controlled porosity, the plain foaming properties wide ranges of the charcoal that finally obtains, purposes is wide.
Technical scheme of the present invention is as follows:
High heat conducting foam material of graphite provided by the invention is characterized in that, uses following step preparation:
(1) petroleum asphalt based mesophase pitch powder, synthetic mesophase asphalt phase particle or coal tar mesophase pitch powder are put into the high-temperature high-voltage reaction device, temperature rise rate with 1-5 ℃/min is warming up to 260-400 ℃, be pressurized to 2-6.0Mpa, continuation is warming up to 350-550 ℃ with 1-2 ℃/min temperature rise rate, after constant temperature 15min-2 hour, cool off and venting obtains bituminous froth;
Described cooling and venting mode are three kinds, first kind the cooling and the venting mode be: after being cooled to room temperature with 1-2 ℃/min rate of temperature fall, at the uniform velocity bleed off gas to normal pressure; Second kind the cooling and the venting mode be: when being cooled to room temperature, at the uniform velocity bleeding off gas and make temperature reduce to the softening temperature of raw material up to normal pressure with 1-2 ℃/min rate of temperature fall; The third cooling and venting mode are: exit fast in the time of 1-5min to normal pressure, be cooled to room temperature with 1-2 ℃/min rate of temperature fall again;
(2) the gained bituminous froth is warming up to 950-1100 ℃ with the temperature rise rate that is not more than 1 ℃/min, carries out charing under the omnidistance nitrogen protection, the charing bituminous froth that obtains;
(3) with gained charing bituminous froth again under argon shield, be warming up to 2600-3000 ℃ with the temperature rise rate that is not more than 1 ℃/min, through naturally cooling, just obtain high heat conducting foam material of graphite.
Described petroleum asphalt based mesophase pitch powder in the described step (1) or synthetic mesophase asphalt phase powder or coal tar mesophase pitch powder are put into after the high-temperature high-voltage reaction device, are evacuated to 0.08-0.1Mpa earlier, heat up again.The density of described high heat conducting foam material of graphite is 0.28-0.75g/cm
3, void content is 55-85%, thermal conductivity is 68-140W/mk.
High heat conducting foam material of graphite provided by the invention and preparation method thereof has following advantage: do not need that raw material is added catalyzer and carry out upgrading, foaming process also need not whipping agent, low cost of manufacture; Put pressure by different venting modes, realize density and controlled porosity, technology is simple; The foam material of graphite performance range that finally obtains is wide, and purposes is wide.
Description of drawings
Fig. 1 is the light micrograph of the high heat conducting foam material of graphite for preparing of the present invention;
Fig. 2, Fig. 3 are the scanning electron photomicrographs of high heat conducting foam material of graphite of the present invention.
Embodiment
Further describe the present invention below in conjunction with drawings and Examples:
Petroleum asphalt based mesophase pitch, synthetic mesophase asphalt phase or coal tar mesophase pitch are put into the high-temperature high-voltage reaction device, temperature rise rate with 1-5 ℃/min is warming up to 260-400 ℃, be pressurized to 2-6.0Mpa, continuation is warming up to 350-550 ℃ with 1-2 ℃/min temperature rise rate, after constant temperature 15min-2 hour, cool off and venting obtains bituminous froth;
The raw material of putting into the high-temperature high-voltage reaction device can be Powdered, also can be particulate state.
After raw material is put into the high-temperature high-voltage reaction device, need earlier reactor to be sealed, and be evacuated to 0.08-0.1Mpa, heat up again.
After being heated to outlet temperature, system needs constant temperature 15min-2 hour, and the performance of the material that different constant temperature times obtains is also inequality.
Adopt different coolings and venting mode, the bituminous froth performance difference that obtains.Adopt first kind of cooling and venting mode, promptly be cooled to room temperature with 1-2 ℃/min rate of temperature fall after, at the uniform velocity bleed off gas to normal pressure, the hole communicates (as shown in Figure 2) around each Kong Douyu of the foams that obtain.Adopt second kind of cooling and venting mode, when promptly being cooled to room temperature with 1-2 ℃/min rate of temperature fall, at the uniform velocity bleeding off gas and make softening temperature that temperature reduces to raw material up to normal pressure, the foams hole wall that obtains is thinner, and density is bigger, and through hole is more.Adopt the third cooling and venting mode, promptly exit fast in the time of 1-5min to normal pressure, 1-2 ℃/min rate of temperature fall is cooled to room temperature again, and the foams hole wall that obtains is thin, and through hole is big, and density is little.
The gained bituminous froth is warming up to 950-1100 ℃ with the temperature rise rate that is not more than 1 ℃/min, carries out charing under the omnidistance nitrogen protection, the charing bituminous froth that obtains; Again with gained charing bituminous froth under argon shield, be warming up to 2600-3000 ℃ with the temperature rise rate that is not more than 1 ℃/min and carry out greying, through naturally cooling, just obtain high heat conducting foam material of graphite.
The density of gained high heat conducting foam material of graphite is 0.28-0.75g/cm
3, void content is 55-85%, thermal conductivity is 68-140W/mk.
Embodiment 1
A certain amount of oil mesophase pitch powder is put into the high-temperature high-voltage reaction device, be evacuated to 0.1Mpa, heat-up rate with 4 ℃/min is heated to 260 ℃, be pressurized to 6.0Mpa, be warming up to 350 ℃ of temperature with 2 ℃/min again, constant temperature 15min, be cooled to room temperature after, at the uniform velocity bleed off gas to normal pressure, obtain bituminous froth;
The gained bituminous froth is warming up to 950 ℃ with the heat-up rate of 1 ℃/min, under the omnidistance nitrogen protection, carries out charing and handle, the charing bituminous froth;
Gained charing bituminous froth again under argon shield, is warming up to 2600 ℃ with the heat-up rate of 1 ℃/min,, just obtains high heat conducting foam material of graphite as shown in Figure 2 through naturally cooling; After measured, the density of the prepared high heat conducting foam material of graphite of present embodiment is 0.75g/cm
3, void content is 55%, thermal conductivity is 68W/mk.
Embodiment 2
Get a certain amount of coal-tar pitch powder after high-temperature heat treatment and put into the high-temperature high-voltage reaction device, be evacuated to 0.08Mpa, temperature rise rate with 5 ℃/min is heated to 350 ℃, be pressurized to 4Mpa, temperature rise rate with 1 ℃/min is warming up to 450 ℃ again, behind the constant temperature 1h, when being cooled to room temperature, at the uniform velocity bleeding off gas and make temperature reduce to the softening temperature of raw material (promptly finishing for 300 ℃) up to normal pressure with 1-2 ℃/min rate of temperature fall; Obtain bituminous froth;
The gained bituminous froth is warming up to 1050 ℃ with the heat-up rate of 1 ℃/min, under the omnidistance nitrogen protection, carries out charing and handle, the plain foam of charing pitch,
Gained charing bituminous froth again under argon shield, is warming up to 2800 ℃ with the heat-up rate of 1 ℃/min,, just obtains high heat conducting foam material of graphite as shown in Figure 1 through naturally cooling; The density of measuring this graphite foam of gained is 0.57g/cm
3, void content is 68%, thermal conductivity is 120W/mk.
Embodiment 3
Get a certain amount of synthetic mesophase asphalt phase particle and put into the high-temperature high-voltage reaction device, be evacuated to 0.08Mpa, temperature rise rate with 1 ℃/min is heated to 400 ℃, be pressurized to 2Mpa, continuation is warming up to 550 ℃ with the temperature rise rate of 1 ℃/min, and constant temperature 2h at the uniform velocity exits to normal pressure fast, be cooled to room temperature with 1 ℃/min, obtain bituminous froth;
The gained bituminous froth is warming up to 1100 ℃ with the heat-up rate of 1 ℃/min, under the omnidistance nitrogen protection, carries out charing and handle, the charing bituminous froth,
Gained charing bituminous froth again under argon shield, is warming up to 3000 ℃ with the heat-up rate of 1 ℃/min,, just obtains high heat conducting foam material of graphite as shown in Figure 3 through naturally cooling; The density of gained high heat conducting foam material of graphite is 0.28g/cm after measured
3, void content is 85%, thermal conductivity is 140W/mk.
The high conductive graphite foam of manufacturing of the present invention can be used to comprise scatterer, heat exchanger, the brake facing of automobile, aircraft, support of the catalyst, adsorbent etc., also can make matrix material, be applied to boats and ships, medical, biological, nuclear industry, military project and many civilian industries etc. by compound other material.
Claims (9)
1, a kind of high heat conducting foam material of graphite is characterized in that, uses following step preparation:
(1) petroleum asphalt based mesophase pitch, synthetic mesophase asphalt phase or coal tar mesophase pitch are put into the high-temperature high-voltage reaction device, temperature rise rate with 1-5 ℃/min is warming up to 260-400 ℃, be pressurized to 2-6.0Mpa, continuation is warming up to 350-550 ℃ with 1-2 ℃/min temperature rise rate, after constant temperature 15min-2 hour, cool off and venting obtains bituminous froth;
(2) the gained bituminous froth is warming up to 950-1100 ℃ with the temperature rise rate that is not more than 1 ℃/min, carries out charing under the omnidistance nitrogen protection, the charing bituminous froth that obtains;
(3) with gained asphalt carbon foams again under argon shield, be warming up to 2600-3000 ℃ with the temperature rise rate that is not more than 1 ℃/min, through naturally cooling, just obtain high heat conducting foam material of graphite.
2, press the high heat conducting foam material of graphite of claim 1, it is characterized in that, described petroleum asphalt based mesophase pitch, synthetic mesophase asphalt phase or coal tar mesophase pitch are Powdered or particulate state, and mesophase pitch is to obtain through thermal treatment with petroleum pitch, coal-tar pitch or synthetic asphalts raw material.
3, by the described high heat conducting foam material of graphite of claim 1, it is characterized in that, described petroleum asphalt based mesophase pitch in the described step (1) or synthetic mesophase asphalt phase or coal tar mesophase pitch are put into after the high-temperature high-voltage reaction device, are evacuated to 0.08-0.1Mpa earlier, heat up again.
4, by the described high heat conducting foam material of graphite of claim 1, it is characterized in that, described cooling and venting mode are any of following three kinds of coolings and venting mode, described three kinds the cooling and the venting mode be: first kind the cooling and the venting mode be: after being cooled to room temperature with 1-2 ℃/min rate of temperature fall, at the uniform velocity bleed off gas to normal pressure; Second kind the cooling and the venting mode be: when being cooled to room temperature, at the uniform velocity bleed off gas to normal pressure with 1-2 ℃/min rate of temperature fall; The third cooling and venting mode are: abandon fast in the time of 1-5min to normal pressure, 1-2 ℃/min rate of temperature fall is cooled to room temperature again.
5, by claim 1,2,3 or 4 described high heat conducting foam material of graphite, it is characterized in that the aperture of described high heat conducting foam material of graphite is 80-800um, density is 0.28-0.75g/cm
3, void content is 55-85%, thermal conductivity is 68-140W/mk.
6, the preparation method of the described high heat conducting foam material of graphite of a kind of claim 1 is characterized in that, its preparation process is as follows:
(1) petroleum asphalt based mesophase pitch, synthetic mesophase asphalt phase or coal tar mesophase pitch are put into the high-temperature high-voltage reaction device, temperature rise rate with 1-5 ℃/min is warming up to 260-400 ℃, be pressurized to 2-6.0Mpa, continuation is warming up to 350-550 ℃ with 1-2 ℃/min temperature rise rate, after constant temperature 15min-2 hour, cool off and venting obtains bituminous froth;
(2) the gained bituminous froth is warming up to 950-1100 ℃ with the temperature rise rate that is not more than 1 ℃/min, carries out charing under the omnidistance nitrogen protection, the charing bituminous froth that obtains;
(3) with gained asphalt carbon foams again under argon shield, be warming up to 2600-3000 ℃ with the temperature rise rate that is not more than 1 ℃/min, through naturally cooling, just obtain high heat conducting foam material of graphite.
7, press the preparation method of the high heat conducting foam material of graphite of claim 6, it is characterized in that, described petroleum asphalt based mesophase pitch, synthetic mesophase asphalt phase or coal tar mesophase pitch are Powdered or particulate state, and mesophase pitch is to obtain through thermal treatment with petroleum pitch, coal-tar pitch or synthetic asphalts raw material.
8, press the preparation method of the described high heat conducting foam material of graphite of claim 6, it is characterized in that, described petroleum asphalt based mesophase pitch in the described step (1) or synthetic mesophase asphalt phase or coal tar mesophase pitch are put into after the high-temperature high-voltage reaction device, be evacuated to 0.08-0.1Mpa earlier, heat up again.
9, press the preparation method of the described high heat conducting foam material of graphite of claim 6, it is characterized in that, described cooling and venting mode are any of following three kinds of coolings and venting mode, described three kinds the cooling and the venting mode be: first kind the cooling and the venting mode be: after being cooled to room temperature with 1-2 ℃/min rate of temperature fall, at the uniform velocity bleed off gas to normal pressure; Second kind the cooling and the venting mode be: when being cooled to room temperature, at the uniform velocity bleed off gas to normal pressure with 1-2 ℃/min rate of temperature fall; The third cooling and venting mode are: abandon fast in the time of 1-5min to normal pressure, 1-2 ℃/min rate of temperature fall is cooled to room temperature again.
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Cited By (10)
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| CN101164875B (en) * | 2007-10-10 | 2010-06-02 | 中国科学院山西煤炭化学研究所 | Method for preparing high heat conducting foam carbon material |
| CN101508433B (en) * | 2009-03-27 | 2011-03-30 | 上海应用技术学院 | High-heat conduction graphitized carbon material and method of manufacturing the same |
| CN102219208A (en) * | 2011-03-28 | 2011-10-19 | 航天材料及工艺研究所 | Method for enhancing heat conduction performance of foamy carbon with high aperture ratio |
| CN102530916A (en) * | 2011-12-31 | 2012-07-04 | 上海大学 | Preparation method of coal-based carbon foam |
| CN102897752A (en) * | 2012-09-11 | 2013-01-30 | 华侨大学厦门园区 | Preparation method for mesophase pitch-based high-thermal conductivity graphite material |
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| US6544491B1 (en) * | 1995-05-31 | 2003-04-08 | West Virginia University | Methods of making a carbon foam |
| US6033506A (en) * | 1997-09-02 | 2000-03-07 | Lockheed Martin Engery Research Corporation | Process for making carbon foam |
| US6315974B1 (en) * | 1997-11-14 | 2001-11-13 | Alliedsignal Inc. | Method for making a pitch-based foam |
| CN100374367C (en) * | 2003-11-07 | 2008-03-12 | 大连理工大学 | Technical method and schedule for preparation of foam carbon material used asphalt as raw material |
| CN1587033A (en) * | 2004-09-10 | 2005-03-02 | 东华大学 | Process for preparing asphalt foam material |
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| CN101508433B (en) * | 2009-03-27 | 2011-03-30 | 上海应用技术学院 | High-heat conduction graphitized carbon material and method of manufacturing the same |
| CN102219208A (en) * | 2011-03-28 | 2011-10-19 | 航天材料及工艺研究所 | Method for enhancing heat conduction performance of foamy carbon with high aperture ratio |
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| CN102897752B (en) * | 2012-09-11 | 2014-09-24 | 华侨大学厦门园区 | Preparation method for mesophase pitch-based high-thermal conductivity graphite material |
| CN102897752A (en) * | 2012-09-11 | 2013-01-30 | 华侨大学厦门园区 | Preparation method for mesophase pitch-based high-thermal conductivity graphite material |
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| CN108793152A (en) * | 2018-07-03 | 2018-11-13 | 中国科学院金属研究所 | A kind of preparation method of the annealed state pyrolytic graphite with super-high heat-conductive performance |
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