CN101134675A - Preparation method of graphite radical composite material - Google Patents
Preparation method of graphite radical composite material Download PDFInfo
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- CN101134675A CN101134675A CNA2007100726210A CN200710072621A CN101134675A CN 101134675 A CN101134675 A CN 101134675A CN A2007100726210 A CNA2007100726210 A CN A2007100726210A CN 200710072621 A CN200710072621 A CN 200710072621A CN 101134675 A CN101134675 A CN 101134675A
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Abstract
The present invention provides preparation process of graphite-base composite material. The preparation process includes the following steps: mixing expandable graphite powder and coke powder and pressing at pressure of 5-50 MPa to form base board with graphite as main component; dissolving asphalt in organic solvent, adding reinforcing material and graphitization catalyzing stuffing, mixing, and eliminating solvent to obtain adhesive mixture; smelting the adhesive mixture at 110-140 deg.c, and soaking the base board at gas pressure of 1-50MPa for 10-120 min; taking out the base board, cooling to room temperature and crushing; and molding the crushed mixture. The graphite-base composite material has excellent electric performance, excellent heat performance, excellent mechanical performance and low cost.
Description
(1) technical field
That the present invention relates to is a kind of preparation method of matrix material, specifically is that saying so a kind of is the preparation method of the graphite-base composite material of main raw material with the expanded graphite.
(2) background technology
Graphite material has good electrical conductivity, low thermal expansivity, resistance to sudden heating and thermostability.Thereby be widely used in fields such as chemical industry, space flight, nuclear energy.Present high strength, high-heat conductivity graphite material adopt generally that refinery coke or pitch coke mix with caking agent and toughener, prepare after the moulding, high temperature graphitization.Natural graphite is compared with other refinery coke, pitch coke, has high thermal stability, low resistivity, fugitive constituent and thermal expansivity.Yet the strength of materials that with the natural graphite is feedstock production is lower, therefore is mainly used in the various brushes of electric charcoal industry production, high-abrasive material and plumbago crucible etc.For the higher graphite material of service requirements intensity, it has been generally acknowledged that should not be with natural graphite as raw material.U.S. Pat 3140190 is to mix with a kind of ceramic additive (molybdenum silicide, titanium boride) and liquid carbonaceous binder with Graphite Powder 99 to prepare refractory materials, although its intensity increases to some extent, is two times of pure graphite intensity, and its intensity is still very low as can be seen.
Natural graphite can make the expanded graphite of 200～600 times of volume growths behind intercalation, washing, high temperature puffing, will can make the flexible graphite plate of the high heat conduction with definite shape and intensity after expanded graphite and the certain caking agent compound compressed moulding.Therefore, natural graphite made expanded graphite after, its adhesiveproperties and intensity all can significantly improve.
(3) summary of the invention
The object of the present invention is to provide a kind of is the method for the graphite-base composite material of feedstock production high strength, high heat conductance, low-resistivity with the expanded graphite, and this method technological operation is simple, easy to operate, help preparing the special high-performance graphite composite material.
The object of the present invention is achieved like this:
(1) the expanded graphite powder is mixed with coke powder and compress and form the graphite cake of matrix based on graphite, pressing pressure is 5～50MPa;
(2) with organic solvent for example benzene, toluene, tetrahydrofuran (THF) or propylene carbonate ester pitch is dissolved, add reinforcing filler and catalyzed graphitization filler, mix, removing desolvates obtains binder mixtures;
(3) by weight percentage the made mixture 20%～40% of made graphite cake 60%～80%, the step 2 of step 1 with the prepared mixture of step 2 110～140 ℃ of fusions, put into the prepared graphite cake of step 1, the gaseous tension that applies is 1～50MPa, floods 10～120 minutes;
(4) take out the graphite cake that floods, be cooled to room temperature, cut or be broken into small-particle;
(5) mixture after the described fragmentation of step 4 is put into mould compression moulding.
The present invention can also comprise:
1, the expansion multiplying power of described expanded graphite is 100～600mL/g, preferred 200～500mL/g.
2, the weight percent of described expanded graphite and coke powder is 10: 1～1: 1.
3, described coke powder is refinery coke or pitch coke.
4, described catalyzed graphitization filler is Ti powder, TiO
2Powder, Si powder, Zr powder, ZrO
2The mixture of one or more any ratios in the compound of powder, organic titanium, silicon and zirconium compounds or inorganic titanium, silicon, zirconium, add-on are 1～15% of pitch weight.
5, described pitch is high softening point bitumen, and softening temperature is 105～200 ℃.
6, described filler is the mixture of one or more any ratios in carbon nanotube, carbon fiber and the silicon carbide fiber, and filling adding amount is 0.1～60% of a pitch weight.
7, described compression moulding is with the mixture after the fragmentation at room temperature, and pressure is 10～80MP
aFollowing coldmoulding, 600～800 ℃ of following charings, impregnated with adhesive mixture again, and then 600～800 ℃ of following charings, charing one impregnation cycles several times after, 1000～3000 ℃ of following greyings.
8, described moulding is to be 10～80MP with the mixture after the fragmentation at 1400～3000 ℃, pressure
aHot-forming down, constant temperature time 10～90min.
Method of the present invention is compared with existing technology has following advantage:
A) natural graphite is made expanded graphite after, therefore its adhesiveproperties can significantly improve, and can it prepare the graphite composite material of high strength, high heat conductance for the raw material coke for replacing, its bending strength is all greater than 30MP
a, thermal conductivity is greater than 250W/m.K, and cost significantly reduces.
B) owing to added filler carbon nanotube, carbon fiber or the silicon carbide fiber with enhancement in raw material, the intensity of the graphite composite material of feasible preparation significantly improves.
C) owing in raw material, added the catalyzed graphitization constituent element, therefore improved the degree of graphitization of graphite composite material, and then improved its thermal conductivity.
D) technological operation of the present invention is simple, easy to operate, helps preparing the special high-performance graphite composite material.
(4) embodiment
For example the present invention is done in more detail below and describes:
Embodiment 1
With expansion multiplying power is to be compressed into film after the expanded graphite of 200mL/g and petroleum coke powder mix with weight ratio at 10: 1, and pressing pressure is 5MPa.Binding agent is a petroleum pitch, and softening temperature is 200 ℃, and adding reinforcing filler is carbon fiber, and content is 0.1% of pitch weight, and the catalyzed graphitization filler of adding is the Zr powder, and add-on is 15% of a pitch weight.With toluene pitch is dissolved, add carbon fiber and Zr powder, mix the back and remove the preparation asphalt mixture that desolvates.With expanded graphite and the coke powder laminated film impregnating pitch mixture that suppresses; Pressure is 10MPa during dipping, and temperature is 110 ℃, and the time is 120 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 60%, and asphalt mixture content is 40%.Under 1400 ℃, pressure is hot-forming under the 80MPa, constant temperature time 90min with said mixture.The room-temperature property of the matrix material of preparation is: bending strength is 30MPa, and thermal conductivity is 260W/m.K.
Embodiment 2
With expansion multiplying power is to be compressed into film after the expanded graphite of 300mL/g and petroleum coke powder mix with weight ratio at 1: 1, and pressing pressure is 10MPa.Binding agent is a coal-tar pitch, and softening temperature is 105 ℃, and adding reinforcing filler is carbon nanotube, and content is 30% of pitch weight, and the catalyzed graphitization filler of adding is the Ti powder, and add-on is 1% of a pitch weight.With toluene pitch is dissolved, add carbon nanotube and Ti powder, mix the back and remove the preparation asphalt mixture that desolvates.With expanded graphite and the coke powder laminated film impregnating pitch mixture that suppresses; Pressure is 50MPa during dipping, and temperature is 140 ℃, and the time is 30 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 80%, and asphalt mixture content is 20%.Under 3000 ℃, pressure is hot-forming under the 10MPa, constant temperature time 10min with said mixture.The room-temperature property of the matrix material of preparation is: bending strength is 34MPa, and thermal conductivity is 365W/m.K.
Embodiment 3
With expansion multiplying power is to be compressed into film after the expanded graphite of 300mL/g and petroleum coke powder mix with weight ratio at 5: 1, and pressing pressure is 30MPa.Binding agent is a coal-tar pitch, and softening temperature is 105 ℃, and adding reinforcing filler is carbon nanotube, and content is 30% of pitch weight, and the catalyzed graphitization filler of adding is the Ti powder, and add-on is 1% of a pitch weight.With propylene carbonate ester pitch is dissolved, add carbon nanotube and Ti powder, mix the back and remove the preparation asphalt mixture that desolvates.With expanded graphite and the coke powder laminated film impregnating pitch mixture that suppresses; Pressure is 30MPa during dipping, and temperature is 140 ℃, and the time is 30 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 75%, and asphalt mixture content is 25%.Under 2400 ℃, pressure is hot-forming under the 40MPa, constant temperature time 60min with said mixture.The room-temperature property of the matrix material of preparation is: bending strength is 32MPa, and thermal conductivity is 315W/m.K.
Embodiment 4
With the expanded graphite is raw material, and expansion multiplying power is 500mL/g, and binding agent is a coal-tar pitch, and softening temperature is 120 ℃, and adding reinforcing filler is carbon nanotube, and content is 60% of pitch weight, and the catalytic filler of adding is a silica flour, and add-on is 5% of a pitch weight.It is 20MPa that expanded graphite is pressed into diaphragm pressure; Pressure is 10MPa during dipping, and temperature is 130 ℃, and the time is 50 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 70%, and asphalt mixture content is 30%.Above-mentioned compound mixes, and moulding process adopts common process, and pressure is coldmoulding under the 80MPa, 800 ℃ of following charings, again through the binder mixtures dipping, and then 800 ℃ of following charings, after charing one impregnation cycles 2 times, 1000 ℃ of following greyings.The room-temperature property of the matrix material of preparation is: bending strength is 32MPa, and thermal conductivity is 260W/m.K.
Embodiment 5
With the expanded graphite is raw material, and expansion multiplying power is 400mL/g, and binding agent is a petroleum pitch, softening temperature is 120 ℃, and adding reinforcing filler is silicon carbide fiber, and content is 20% of pitch weight, the catalytic filler that adds is an organosilane, and add-on is designated as 10% of pitch weight with silicon.It is 20MPa that expanded graphite is pressed into diaphragm pressure; Pressure is 10MPa during dipping, and temperature is 130 ℃, and the time is 70 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 70%, and asphalt mixture content is 30%.Above-mentioned compound mixes, and moulding process adopts common process, and pressure is coldmoulding under the 10MPa, 600 ℃ of following charings, again through the binder mixtures dipping, and then 800 ℃ of following charings, after charing one impregnation cycles 5 times, 3000 ℃ of following greyings.The room-temperature property of the matrix material of preparation is: bending strength is 34MPa, and thermal conductivity is 280W/m.K.
Embodiment 6
With the expanded graphite is raw material, and expansion multiplying power is 300mL/g, and binding agent is a petroleum pitch, softening temperature is 120 ℃, and adding reinforcing filler is carbon nanotube, and content is 20% of pitch weight, the catalytic filler that adds is an organic zirconate, and add-on is designated as 10% of pitch weight with zirconium.It is 40MPa that expanded graphite is pressed into diaphragm pressure; Pressure is 20MPa during dipping, and temperature is 130 ℃, and the time is 70 minutes; Be broken into small-particle after the cooling, wherein the content of expanded graphite and coke powder is 75%, and asphalt mixture content is 25%.Above-mentioned compound mixes, and moulding process adopts common process, and pressure is coldmoulding under the 60MPa, 800 ℃ of following charings, again through the binder mixtures dipping, and then 800 ℃ of following charings, after charing one impregnation cycles 4 times, 2400 ℃ of following greyings.The room-temperature property of the matrix material of preparation is: bending strength is 36MPa, and thermal conductivity is 300W/m.K.
Claims (9)
1. the preparation method of a graphite-base composite material is characterized in that comprising the steps:
(1) the expanded graphite powder is mixed with coke powder and compress and form the graphite cake of matrix based on graphite, pressing pressure is 5～50MPa;
(2) with organic solvent for example benzene, toluene, tetrahydrofuran (THF) or propylene carbonate ester pitch is dissolved, add reinforcing filler and catalyzed graphitization filler, mix, removing desolvates obtains binder mixtures;
(3) by weight percentage the made mixture 20%～40% of made graphite cake 60%～80%, the step 2 of step 1 with the prepared mixture of step 2 110～140 ℃ of fusions, put into the prepared graphite cake of step 1, the gaseous tension that applies is 1～50MPa, floods 10～120 minutes;
(4) take out the graphite cake that floods, be cooled to room temperature, cut or be broken into small-particle;
(5) mixture after the described fragmentation of step 4 is put into mould compression moulding.
2. according to the preparation method of claims 1 described a kind of graphite-base composite material, the expansion multiplying power that it is characterized in that described expanded graphite is 100～600mL/g, preferred 200～500mL/g.
3. according to the preparation method of claims 1 described a kind of graphite-base composite material, the weight percent that it is characterized in that described expanded graphite and coke powder is 10: 1～1: 1.
4. according to the preparation method of claims 1 described a kind of graphite-base composite material, it is characterized in that described coke powder is refinery coke or pitch coke.
5. according to the preparation method of claims 1 described a kind of graphite-base composite material, it is characterized in that described catalyzed graphitization filler is Ti powder, TiO
2Powder, Si powder, Zr powder, ZrO
2The mixture of one or more any ratios in the compound of powder, organic titanium, silicon and zirconium compounds or inorganic titanium, silicon, zirconium, add-on are 1～15% of pitch weight.
6. according to the preparation method of claims 1 described a kind of graphite-base composite material, it is characterized in that described pitch is high softening point bitumen, softening temperature is 105～200 ℃.
7. according to the preparation method of claims 1 described a kind of graphite-base composite material, it is characterized in that described filler is the mixture of one or more any ratios in carbon nanotube, carbon fiber and the silicon carbide fiber, filling adding amount is 0.1～60% of a pitch weight.
8. according to the preparation method of the described a kind of graphite-base composite material of claims 1-7, it is characterized in that described compression moulding is with the mixture after the fragmentation at room temperature, pressure is coldmoulding under 10～80MPa, 600～800 ℃ of following charings, impregnated with adhesive mixture again, and then 600～800 ℃ of following charings, charing-impregnation cycles several times after, 1000～3000 ℃ of following greyings.
9. according to the preparation method of the described a kind of graphite-base composite material of claims 1-7, it is characterized in that described compression moulding is is hot-forming under 10～80MPa with the mixture after the fragmentation at 1400～3000 ℃, pressure, constant temperature time 10～90min.
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