CN102659095A - Preparation method of high heat conduction and high strength graphite - Google Patents
Preparation method of high heat conduction and high strength graphite Download PDFInfo
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- CN102659095A CN102659095A CN2012101226307A CN201210122630A CN102659095A CN 102659095 A CN102659095 A CN 102659095A CN 2012101226307 A CN2012101226307 A CN 2012101226307A CN 201210122630 A CN201210122630 A CN 201210122630A CN 102659095 A CN102659095 A CN 102659095A
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- natural flake
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011302 mesophase pitch Substances 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000010426 asphalt Substances 0.000 claims description 26
- 239000003610 charcoal Substances 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 11
- 239000002657 fibrous material Substances 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000007770 graphite material Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000011268 mixed slurry Substances 0.000 abstract 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 abstract 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 abstract 1
- 239000004917 carbon fiber Substances 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 238000003825 pressing Methods 0.000 description 8
- 238000010907 mechanical stirring Methods 0.000 description 7
- 238000012856 packing Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- 239000011329 calcined coke Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
一种高导热高强度石墨的制备方法是按重量百分比组成天然鳞片石墨的含量为63%–71%，中间相沥青的含量为24%-30%，短切中间相沥青炭纤维的含量为4%-8%，将天然鳞片石墨、中间相沥青及短切中间相沥青纤维在含有0.7-1.0wt%的羟乙基纤维素的水溶液中机械混合,得到混合均匀的浆料。将混合均匀的浆料真空干燥，然后装模热压处理，温度≤300℃时，以120-180℃/h，温度＞300℃时，以300-600℃/h的升温速率，将温度从室温升至2200-2700℃，并在最终温度下加压至20-25MPa,自然降温后制得最终产品。本发明具有制备质轻、导热性能和力学性能良好石墨材料的优点。A preparation method of high thermal conductivity and high strength graphite is composed of 63%-71% of natural flake graphite by weight, 24%-30% of mesophase pitch, and 4% of chopped mesophase pitch carbon fiber. %-8%, mechanically mix natural flake graphite, mesophase pitch and chopped mesophase pitch fibers in an aqueous solution containing 0.7-1.0wt% hydroxyethyl cellulose to obtain a uniformly mixed slurry. Vacuum-dry the uniformly mixed slurry, and then heat and press in a mold. When the temperature is ≤300°C, the temperature is 120-180°C/h; when the temperature is >300°C, the temperature is increased from 300-600°C/h. The room temperature is raised to 2200-2700°C, and the pressure is increased to 20-25MPa at the final temperature, and the final product is obtained after natural cooling. The invention has the advantages of preparing graphite materials with light weight, good thermal conductivity and mechanical properties.
Description
Technical field
The invention belongs to a kind of preparation method of high conductive high strength graphite.
Background technology
Carbon/graphite material is owing to light weight and have advantages such as good heat-conductivity conducting, mechanical behavior under high temperature, and in aspect extensive application such as aerospace, high power density heat dissipation element, nuclear fusion device first wall materials.At present, the research for high-heat conductivity graphite material mainly concentrates on high heat conducting fiber C/C matrix material and the adulterated charcoal/ceramic composite material of catalysis constituent element two aspects.But the preparation of C/C matrix material often need be with fiber premolding; Then precast body is carried out repeatedly solvent impregnated resin or pitch or realizes densification (Carbon-carbon composites:a summary of recent developments and applications. T. Windhorst through high temperature chemical vapor deposition; Mater Des; 1997,18 (1): 11-15).Because its preparation cycle is long, cost is high, thereby the further application of this material is restricted.For charcoal/ceramic composite material, common preparation technology adopts calcined coke as aggregate, and coal-tar pitch makes the finished product as sticker after mixing moulding, charing, greying.Though an amount of catalytic ceramics constituent element mix the graphite regularity that can improve the raw material of wood-charcoal material; Improve the conductive performance of matrix, but it increases the proportion of material to a certain extent, influenced the mechanical property of material; As increased fragility (the Properties and microstructure of graphitised ZrC/C or SiC/C composites. H.P. Qiu of matrix; Carbon, 2005,43 (5): 1021-25).And these drawbacks limit the application of high conductive graphite at aspects such as aerospace fields.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the graphite material of light weight, heat conductivility and good mechanical properties.
The high conductive high strength graphite material that the present invention proposes, its preparation method mainly comprises the steps:
(1) content of forming natural flake graphite by weight percentage is 63% – 71%; The content of mesophase pitch is 24%-30%; A short content of asphalt phase charcoal fiber that hits is 4%-8%; With natural flake graphite, mesophase pitch and the short asphalt phase fiber mechanically mixing in the aqueous solution of the Natvosol that contains 0.7-1.0wt% of hitting; The slurry that obtains mixing, wherein, he carries out mechanically mixing by weight 1:2.5-3 by the aqueous solution of short hit an asphalt phase fibrous material sum and Natvosol natural flake graphite, mesophase pitch;
(2) with the slurry vacuum-drying that mixes, adorn the mould hot-pressing processing then, during temperature≤300 ℃; With 120-180 ℃/h; During temperature＞300 ℃,, temperature is risen to 2200-2700 ℃ from room temperature with the temperature rise rate of 300-600 ℃/h; And under outlet temperature, be forced into 20-25MPa, make the finished product after the cooling naturally.
As stated, the granularity of natural flake graphite is at 150-380 μ m, and carbon content is 95-98wt.%; The softening temperature of mesophase pitch is 263.5-289.1 ℃, and carbon yield is 85.7-89.2 wt.%, and granularity is below 150 μ m; A short length of asphalt phase charcoal fiber of hitting is 3-6mm, and diameter is 13-17 μ m, and resistivity is 10-15 μ Ω m, and tensile strength is greater than 0.8GPa; The Natvosol granularity is 75-150 μ m, and viscosity is 1500-2500mp.s.
Advantage of the present invention is following:
The used raw material of the present invention is easy to get, and is with low cost; Material adopts the heat pressing process once shaped, and need not to flood repeatedly, heat deposition etc. realized the loaded down with trivial details process of densification, and preparation technology's cycle is short, has reduced manufacturing cost; Product light weight, heat conduction and good mechanical performance.
Embodiment
Embodiment 1
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.7wt% Natvosol according to the ratio of 71:25:4 (wt%).The aqueous solution weight ratio 1:2.5 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, the granularity of natural flake graphite is 380 μ m, and carbon content is 96wt%; The softening temperature of mesophase pitch is 283.1 ℃, and carbon yield is 88.9wt%, and granularity is 150 μ m; A short length of asphalt phase charcoal fiber of hitting is 3mm, and diameter is 17 μ m, and resistivity is 15 μ Ω m, and tensile strength is 0.8GPa; The Natvosol granularity is 150 μ m, and viscosity is 2000mp.s.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 120 ℃/h in the past, the temperature rise rate with 300 ℃/h rises to 2500 ℃ afterwards, and under outlet temperature, is forced into 20MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 2
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.7wt% Natvosol according to the ratio of 70:24:6 (wt%).The aqueous solution weight ratio 1:2.5 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, the granularity of natural flake graphite is 270 μ m, and carbon content is 98wt%; The softening temperature of mesophase pitch is 275.6 ℃, and carbon yield is 87.4wt%, and granularity is 150 μ m; A short length of asphalt phase charcoal fiber of hitting is 6mm, and diameter is 15 μ m, and resistivity is 13 μ Ω m, and tensile strength is 1.0GPa.The Natvosol granularity is 150 μ m, and viscosity is 1500mp.s.。In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 140 ℃/h in the past, the temperature rise rate with 400 ℃/h rises to 2500 ℃ afterwards, and under outlet temperature, is forced into 23MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 3
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.8wt% Natvosol according to the ratio of 67:25:8 (wt%).The aqueous solution weight ratio 1:2.7 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, the softening temperature of mesophase pitch is 263.5 ℃, and carbon yield is 85.7 wt%, and granularity is 105 μ m, and the essential property of all the other raw materials is shown in example 2.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 180 ℃/h in the past, the temperature rise rate with 600 ℃/h rises to 2500 ℃ afterwards, and under outlet temperature, is forced into 23MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 4
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.8wt% Natvosol according to the ratio of 68:28:4 (wt%).The aqueous solution weight ratio 1:2.7 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, the granularity of natural flake graphite is 150 μ m, and carbon content is 95wt%; The softening temperature of mesophase pitch is 277.3 ℃, and carbon yield is 86.3 wt%, and granularity is 75 μ m; A short length of asphalt phase charcoal fiber of hitting is 4mm, and diameter is 17 μ m, and resistivity is 15 μ Ω m, and tensile strength is 0.8GPa.The Natvosol granularity is 105 μ m, and viscosity is 2000mp.s.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 160 ℃/h in the past, the temperature rise rate with 500 ℃/h rises to 2500 ℃ afterwards, and under outlet temperature, is forced into 25MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 5
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.9wt% Natvosol according to the ratio of 65:28:7 (wt%).The aqueous solution weight ratio 1:2.8 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, the granularity of natural flake graphite is 250 μ m, and carbon content is 97wt%; The softening temperature of mesophase pitch is 289.1 ℃, and carbon yield is 89.2 wt%, and granularity is 105 μ m; A short length of asphalt phase charcoal fiber of hitting is 5mm, and diameter is 13 μ m, and resistivity is 10 μ Ω m, and tensile strength is 1.1GPa.The Natvosol granularity is 105 μ m, and viscosity is 2500mp.s.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 140 ℃/h in the past, the temperature rise rate with 600 ℃/h rises to 2500 ℃ afterwards, and under outlet temperature, is forced into 25MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 6
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 0.9wt% Natvosol according to the ratio of 63:30:7 (wt%).The aqueous solution weight ratio 1:2.9 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, each raw material properties is shown in example 5.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 140 ℃/h in the past, the temperature rise rate with 500 ℃/h rises to 2200 ℃ afterwards, and under outlet temperature, is forced into 25MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
Embodiment 7
At first natural flake graphite, mesophase pitch, a short asphalt phase charcoal fiber that hits are joined in the aqueous solution that contains the 1.0wt% Natvosol according to the ratio of 63:30:7 (wt%).The aqueous solution weight ratio 1:3 of natural flake graphite, mesophase pitch he short hit an asphalt phase fibrous material sum and Natvosol.Mechanical stirring is carried out thorough mixing.Wherein, each raw material properties is shown in example 5.In the graphite jig of packing into after the slurry vacuum-drying that mixes, carry out hot-pressing processing.300 ℃ of temperature rise rates of pressing 120 ℃/h in the past, the temperature rise rate with 600 ℃/h rises to 2700 ℃ afterwards, and under outlet temperature, is forced into 25MPa.Naturally come out of the stove after the cooling, the performance that records final material is seen table 1.
The Main physical performance perameter of table 1 material
Claims (5)
1. the preparation method of a high conductive high strength graphite is characterized in that comprising the steps:
(1) content of forming natural flake graphite by weight percentage is 63% – 71%; The content of mesophase pitch is 24%-30%; A short content of asphalt phase charcoal fiber that hits is 4%-8%; With natural flake graphite, mesophase pitch and the short asphalt phase fiber mechanically mixing in the aqueous solution of the Natvosol that contains 0.7-1.0wt% of hitting; The slurry that obtains mixing, wherein, he carries out mechanically mixing by weight 1:2.5-3 by the aqueous solution of short hit an asphalt phase fibrous material sum and Natvosol natural flake graphite, mesophase pitch;
(2) with the slurry vacuum-drying that mixes, adorn the mould hot-pressing processing then, during temperature≤300 ℃; With 120-180 ℃/h; During temperature＞300 ℃,, temperature is risen to 2200-2700 ℃ from room temperature with the temperature rise rate of 300-600 ℃/h; And under outlet temperature, be forced into 20-25MPa, make the finished product after the cooling naturally.
2. the preparation method of a kind of high conductive high strength graphite as claimed in claim 1, the granularity that it is characterized in that described natural flake graphite is at 150-380 μ m, and carbon content is 95-98wt%.
3. the preparation method of a kind of high conductive high strength graphite as claimed in claim 1, the softening temperature that it is characterized in that described mesophase pitch is 263.5-289.1 ℃, and carbon yield is 85.7-89.2 wt.%, and granularity is below 150 μ m.
4. the preparation method of a kind of high conductive high strength graphite as claimed in claim 1 is characterized in that a described weak point length of asphalt phase charcoal fiber of hitting is 3-6mm, and diameter is 13-17 μ m, and resistivity is 10-15 μ Ω m, and tensile strength is greater than 0.8GPa.
5. the preparation method of a kind of high conductive high strength graphite as claimed in claim 1 is characterized in that described Natvosol granularity is 75-150 μ m, and viscosity is 1500-2500mp.s.
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| CN2012101226307A CN102659095A (en) | 2012-04-25 | 2012-04-25 | Preparation method of high heat conduction and high strength graphite |
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| CN2012101226307A CN102659095A (en) | 2012-04-25 | 2012-04-25 | Preparation method of high heat conduction and high strength graphite |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446587A (en) * | 2014-11-24 | 2015-03-25 | 天津大学 | Preparation method of carbon-based composite material with high heat conductivity coefficients in both plane direction and thickness direction |
| CN105884357A (en) * | 2016-04-13 | 2016-08-24 | 湖南省长宇新型炭材料有限公司 | Graphite die material for hot-press molding and preparation method of graphite die material |
| CN108706973A (en) * | 2018-08-22 | 2018-10-26 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of high intensity high-heat conductivity graphite material |
| CN110550955A (en) * | 2019-09-24 | 2019-12-10 | 中国科学院山西煤炭化学研究所 | Ultrahigh-heat-conductivity and high-strength graphite block material and preparation method thereof |
| CN113307646A (en) * | 2021-06-28 | 2021-08-27 | 湖南兴晟新材料科技有限公司 | High-heat-conductivity and high-purity graphite-based composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1678447A (en) * | 2002-08-27 | 2005-10-05 | 尤卡碳工业有限公司 | Process of making graphite product |
-
2012
- 2012-04-25 CN CN2012101226307A patent/CN102659095A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1678447A (en) * | 2002-08-27 | 2005-10-05 | 尤卡碳工业有限公司 | Process of making graphite product |
Non-Patent Citations (2)
| Title |
|---|
| GUANMING YUAN，ET AL.: "Graphite blocks with preferred orientation and high thermal conductivity", 《CARBON》, vol. 50, 18 August 2011 (2011-08-18) * |
| ZHANJUN LIU, ET AL.: "Graphite blocks with high thermal conductivity derived from natural graphite flake", 《CARBON》, vol. 46, 28 January 2008 (2008-01-28) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446587A (en) * | 2014-11-24 | 2015-03-25 | 天津大学 | Preparation method of carbon-based composite material with high heat conductivity coefficients in both plane direction and thickness direction |
| CN105884357A (en) * | 2016-04-13 | 2016-08-24 | 湖南省长宇新型炭材料有限公司 | Graphite die material for hot-press molding and preparation method of graphite die material |
| CN108706973A (en) * | 2018-08-22 | 2018-10-26 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of high intensity high-heat conductivity graphite material |
| CN108706973B (en) * | 2018-08-22 | 2021-04-06 | 中国科学院山西煤炭化学研究所 | Preparation method of high-strength high-thermal-conductivity graphite material |
| CN110550955A (en) * | 2019-09-24 | 2019-12-10 | 中国科学院山西煤炭化学研究所 | Ultrahigh-heat-conductivity and high-strength graphite block material and preparation method thereof |
| CN110550955B (en) * | 2019-09-24 | 2021-08-13 | 中国科学院山西煤炭化学研究所 | A kind of ultra-high thermal conductivity, high-strength graphite block material and preparation method thereof |
| CN113307646A (en) * | 2021-06-28 | 2021-08-27 | 湖南兴晟新材料科技有限公司 | High-heat-conductivity and high-purity graphite-based composite material and preparation method thereof |
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Application publication date: 20120912 |