CN105272256B - A kind of high heat conduction graphite foam/carbon composite and preparation method thereof - Google Patents

A kind of high heat conduction graphite foam/carbon composite and preparation method thereof Download PDF

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CN105272256B
CN105272256B CN201510633245.2A CN201510633245A CN105272256B CN 105272256 B CN105272256 B CN 105272256B CN 201510633245 A CN201510633245 A CN 201510633245A CN 105272256 B CN105272256 B CN 105272256B
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temperature
heat conduction
high heat
graphite foam
heating rate
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CN105272256A (en
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冯志海
余立琼
樊桢
宋永忠
孔清
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

The present invention relates to a kind of high heat conduction graphite foam/carbon composite and preparation method thereof, prepares the graphite foam with high heat conductance as enhancing base by precursor of mesophase pitch first；Then using mesophase pitch or coal tar pitch as matrix carbon matrix precursor, impregnated by mesohigh/carbonization technology strengthens base to graphite foam and is densified；More than 2500 DEG C of high temperature graphitization processing finally is carried out to the material of acquisition, obtains density in 1.3g/cm3More than, thermal conductivity is more than 300W/mK, and compressive strength can reach more than 9MPa high heat conduction graphite foam/carbon composite, and its thermal conductivity and compressive strength are 2 times and more than 3 times of foam material of graphite, compared to high heat conduction carbon/carbon compound material, prepare cost and the cycle also greatly reduces.

Description

A kind of high heat conduction graphite foam/carbon composite and preparation method thereof
Technical field
The present invention relates to a kind of high heat conduction graphite foam/carbon composite and preparation method thereof, it is carbon-based multiple to belong to high heat conduction Condensation material manufacturing technology field.
Background technology
With the fast development of science and technology, heat management and heat dissipation turn into the key technology that many fields are developed.It is various Accurate electronic device control system is required in re-entry space vehicle (aircraft, guided missile, satellite and all kinds of spacecrafts), to realize certainly Dynamicization and accurate control and guidance to empty day weapon, these electronic equipments, which need to work under certain temperature conditions, to expire The requirement used enough.Also, with the development of microelectric technique and guidance technology, electronic equipment degree of integration more and more higher, energy Density is increasing, and caused heat is more and more, to ensure equipment steady operation, it is necessary to using high performance highly heat-conductive material Effective heat management is carried out to it.Localized hyperthermia's part application environment of re-entry space vehicle is harsh, and temperature is high, thermal stress protrudes, Need lightweight, resistant to elevated temperatures highly heat-conductive material to play complement heat conduction function, so as to simplify anti-thermal design, lift the reliable of aircraft Property.Traditional metal (aluminium, copper) Heat Conduction Material is because itself density is larger, thermal coefficient of expansion is higher, trace impurity causes heat The defects of conductance declines to a great extent, it is difficult to meet growth requirement.Therefore, the research and development to new highly heat-conductive material are most important.
Highly-conductive hot carbon based composites have low-density, high heat conductance, low thermal coefficient of expansion, certain structural strength, resistance to The excellent properties such as high temperature, corrosion-resistant, the high heat conduction candidate material for most having application prospect at present is become, is widely used in empty day The fields such as the heat management of aircraft, complement heat conduction, high energy electron, such as electronic device cooling system, heat-exchange system, space low temperature System, thermal energy storage system etc., realize that miniaturization, device lightweight, compact-sizedization and the operation of corresponding thermal management component are high Effectization.
Existing high heat conducting foam material of graphite, due to its graphite platelet structure high development, and its porous structure And the characteristics of high opening rate determines that the mechanical property of graphite foam is not high, while the raising of its heat conductivility is limited, it is difficult to meets The application demand of the management device of higher energy density.High heat conduction carbon/carbon compound material is carbon-based multiple as new high heat conduction Condensation material, there is high temperature resistance and high strength, but it is high heat conduction fibrage precast body that it, which strengthens base, high heat conduction fiber is former Material can only import, and expensive, cycle length costly plus weaving textile, it is difficult to batch application, and face key at any time The problem of raw material high heat conduction fiber entrance is limited.How a kind of density is provided, thermal conductivity meets to require and raw suitable for batch The composite of production, it is this area urgent problem to be solved.
The content of the invention
It is an object of the invention to overcome the above-mentioned deficiency of prior art, there is provided a kind of high heat conduction graphite foam/carbon is compound The preparation method of material, suitable for batch material, the density of the material is in 1.3g/cm3More than, thermal conductivity can reach 300W/m More than K.
The above-mentioned purpose of the present invention is mainly achieved through the following technical solutions：
A kind of preparation method of high heat conduction graphite foam/carbon composite, is comprised the following steps that：
Step (1), using mesophase pitch as presoma prepare high heat conduction graphite foam as strengthen base, the high heat conduction The density of graphite foam enhancing base is 0.5~0.9g/cm3, thermal conductivity is more than 100W/mK, and porosity is 39~77%, perforate Rate is more than 85%；
Step (2), the graphite foam enhancing base for preparing step (1) carries out mesophase pitch or coal tar pitch impregnates；Its Middle mesophase pitch dipping temperature is 280-370 DEG C, and coal tar pitch dipping temperature is 160-240 DEG C, impregnation pressure 15-70MPa, Dwell time is 1-5h；
Step (3), step (2) is impregnated to the graphite foam progress carbonization treatment after mesophase pitch or coal tar pitch；
Step (4), by the C-base composte material obtained after step (3) carbonization treatment be put into high temperature furnace carry out high temperature at Reason；
Step (5), judge whether composite density exceedes given threshold, be not above given threshold then return to step (2) impregnation pressure when mesophase pitch or coal tar pitch dipping, is increased；Composite density exceedes given threshold, performs step (6)；
Step (6), by C-base composte material carry out superhigh temperature graphitization processing, high heat conduction graphite foam/carbon is prepared Composite.
In the preparation method of above-mentioned high heat conduction graphite foam/carbon composite, carbonization treatment technique curve in step (3) For：Room temperature~350 DEG C, heating rate are 5~15 DEG C/min；350~500 DEG C, heating rate is 1~5 DEG C/min；500 DEG C, protect 1~10h of temperature；500~650 DEG C, heating rate is 1~5 DEG C/min；650 DEG C, it is incubated 1~10h；650~900 DEG C, heating rate For 3~5 DEG C/min, 900 DEG C, 1~5h is incubated；Freely cool.
In the preparation method of above-mentioned high heat conduction graphite foam/carbon composite, step (4) high temperature handling process curve For：Room temperature~900 DEG C, heating rate are 10~20 DEG C/min；900~1200 DEG C, heating rate is 5~10 DEG C/min；1200 DEG C insulation 1~5h；1200 DEG C~target process temperature, heating rate is 3~5 DEG C/min；Under target process temperature insulation 1~ 5h；Control rate of temperature fall for 5~15 DEG C/min until temperature is down to less than 900 DEG C；Less than 900 DEG C freely cool；The target Treatment temperature is 1800 DEG C~2500 DEG C.
In the preparation method of above-mentioned high heat conduction graphite foam/carbon composite, superhigh temperature graphitization processing in step (6) Process curve is：More than 2500 DEG C are warming up to 1~15 DEG C/min speed and is incubated 1~10h, are freely cooled.
Preferably, given threshold 1.3g/cm3。
Preferably, the thermal conductivity of high heat conduction graphite foam/carbon composite is more than 300W/mK.
Preferably, it is specific as enhancing base by presoma preparation high heat conduction graphite foam of mesophase pitch in step (1) For：Softening point is used to prepare high heat conduction stone by carbonization and graphitization processing for 220-300 DEG C of mesophase pitch foaming Black foam is as enhancing base.
Preferably, composite density is not above given threshold then return to step (two) in the step (5), increase Impregnation pressure when mesophase pitch or coal tar pitch impregnate, and heighten the temperature that high-temperature process is carried out in high temperature furnace.
A kind of high heat conduction graphite foam/carbon composite simultaneously, using high heat conduction graphite foam as enhancing base, mesophase pitch Or coal tar pitch is matrix carbon matrix precursor, is impregnated, is carbonized by 15-70MPa, 1800 DEG C~2500 DEG C high-temperature heat treatments and 2500 DEG C Above superhigh temperature graphitization is prepared.
Preferably, prepared using the preparation method of described high heat conduction graphite foam/carbon composite.
The present invention has the advantages that compared with prior art：
(1) present invention uses mesophase pitch as precursor, and being prepared by foaming-carbonization-graphitization has high fever The graphite foam of conductance is as enhancing base；Then using mesophase pitch or coal tar pitch as matrix carbon matrix precursor, soaked by mesohigh Stain/carbonization technology is densified to graphite foam enhancing base；More than 2500 DEG C of high fire stons finally is carried out to the material of acquisition Blackization processing, is prepared density in 1.3g/cm3More than, thermal conductivity is more than 300W/mK, compressive strength can reach 9MPa with On high heat conduction graphite foam/carbon composite, its thermal conductivity and compressive strength are 2 times and more than 3 times of foam material of graphite, Compared to high heat conduction carbon/carbon compound material, prepare cost and the cycle also greatly reduces, the technique can also realize that large scale height is led simultaneously The preparation of hot graphite foam/carbon composite.
(2) present invention uses density as 0.5~0.9g/cm3, thermal conductivity is more than 100W/mK, porosity 39~ 77%, high heat conduction graphite foam of the percent opening more than 85% has preferably as enhancing base, the graphite foam of this density range Mechanical property, ensure that enhancing base can be compound with matrix carbon and not easy to crack under the conditions of mesohigh, the high hole of enhancing base Gap rate and percent opening can lift pickling efficiency, while strengthening base, there is high thermal conductivity to contribute to final composite thermal conductivity The lifting of rate.
(3) present invention use mesophase pitch as high heat conduction presoma, its excellent orientation be easy to graphited knot The thermal conductivity of final composite can be substantially improved in structure；Coal tar pitch is used as matrix carbon matrix precursor, it is low on cost is prepared In mesophase pitch presoma, while it can also meet part actual demand；Relative to resinae presoma, using mesophase pitch Or coal tar pitch is matrix carbon matrix precursor, it is easier to prepares the C-base composte material of high heat conductance.
(4) slower carbonization heating rate and specific high temperature perforate treatment temperature are employed in the present invention, can avoided Material is carbonized and problem of Cracking caused by light component release in part in high-temperature process, while discharges stress；Using superelevation stone Inkization temperature and slower graphitization heating rate, contribute to the ordered orientation of graphite flake layer and growing up for graphite grains, carry The high thermal conductivity of final composite.
(5) present invention according to different application demands, can select the graphite foam of different densities, pore structure and performance Enhancing base materials material, adjust matrix carbon matrix precursor species and dipping/carbonization technique, it is possible to achieve different densities, heat conductivility and knot The preparation of high heat conduction graphite foam/carbon composite of structure intensity.By adjusting impregnation pressure, high-temperature process temperature, repetition time Number can obtain the composite of different density, be required to determine number of repetition, the party according to actually required composite density Method is flexibly effective, can be applied to heat management, the complement heat conduction system of varying environment demand, and practicality is stronger.
(6) present invention can apply to the preparation of large scale high heat conduction graphite foam/carbon composite, with traditional heat management The metal material that system uses is compared, and has the characteristics that light, high heat conductance, linear expansion coefficient are low, can be applied to empty day flight The heat management of device, survey of deep space, satellite and high energy laser weapon etc., complement heat conduction system, promote higher energy density electronic devices Application, realize equipment lightweight and it is long when high efficient and reliable run.
(7) present invention prepared by high heat conduction graphite foam/carbon composite due to its density it is relatively low, be also used as increasing Strong basis is further compound with other materials, assigns its new 26S Proteasome Structure and Function, expands its application field.
Brief description of the drawings
Fig. 1 is high heat conduction graphite foam/carbon composite preparation method flow chart of the present invention.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings：
The present invention uses mesophase pitch as precursor, and being prepared by foaming-carbonization-graphitization has high heat conductance Graphite foam as enhancing base；Then using mesophase pitch or coal tar pitch as matrix carbon matrix precursor ,/carbon is impregnated by mesohigh Change technology is densified to graphite foam enhancing base；Finally the material of acquisition is carried out at more than 2500 DEG C of high temperature graphitization Reason, is prepared density in 1.3g/cm3More than, thermal conductivity is more than 300W/mK high heat conduction graphite foam/carbon composite. Comprise the following steps that：
Step (1), using mesophase pitch as presoma, pass through foaming-carbonization-graphitization and prepare high heat conduction graphite For foam as enhancing base, its density is 0.5~0.9g/cm3, thermal conductivity is more than 100W/mK, and porosity is opened 39~77% Porosity is more than 85%.
Step (2), graphite foam prepared by step (1) is put into bituminizing tank carries out mesophase pitch or coal and drip Green grass or young crops dipping；Wherein mesophase pitch dipping temperature is 280-370 DEG C, and coal tar pitch dipping temperature is 160-240 DEG C, and impregnation pressure is 15-70MPa, dwell time 1-5h.
Step (3), step (2) is impregnated to the graphite foam after mesophase pitch or coal tar pitch be put into carbide furnace and carry out Carbonization treatment.
The process curve of carbonization treatment is：Room temperature~350 DEG C, heating rate are 5~15 DEG C/min；350~500 DEG C, rise Warm speed is 1~5 DEG C/min；500 DEG C, it is incubated 1~10h；500~650 DEG C, heating rate is 1~5 DEG C/min；650 DEG C, protect 1~10h of temperature；650~900 DEG C, heating rate is 3~5 DEG C/min, 900 DEG C, is incubated 1~5h；Freely cool.
Step (4), by the C-base composte material obtained after step (3) carbonization treatment be put into high temperature furnace carry out high temperature open Hole is handled；
High-temperature processing technology curve is：Room temperature~900 DEG C, heating rate are 10~20 DEG C/min；900~1200 DEG C, rise Warm speed is 5~10 DEG C/min；1200 DEG C of 1~5h of insulation；1200 DEG C~target process temperature, heating rate be 3~5 DEG C/ min；1~5h is incubated under target process temperature；Control rate of temperature fall for 5~15 DEG C/min until temperature is down to less than 900 DEG C； Less than 900 DEG C freely cool；The target process temperature is 1800 DEG C~2500 DEG C.
Step (5), according to materials application demand, repeat step (two)~step (4), by adjust mesophase pitch or Impregnation pressure when coal tar pitch impregnates, the C-base composte material of different densities can be obtained.
Step (6), by C-base composte material carry out more than 2500 DEG C superhigh temperature graphitization processings, density is prepared and exists 1.3g/cm3More than, thermal conductivity is more than 300W/mK high heat conduction graphite foam/carbon composite.
Superhigh temperature graphitization processing process curve is：More than 2500 DEG C and insulation 1 are warming up to 1~15 DEG C/min speed ~10h, freely cools.
Embodiment 1
(1), use softening point as 275 DEG C of mesophase pitch, pressure be 7.0MPa, temperature be that 330 DEG C of conditions issue Type is soaked, preparing high heat conduction graphite foam by 900 DEG C of carbonizations and 3000 DEG C of graphitizations is used as enhancing base, prepared graphite foam Enhancing base density is 0.60g/cm3, thermal conductivity 138W/mK, porosity 73%, percent opening is more than 90%.
(2), the graphite foam enhancing base prepared in step (1) is put into coal tar pitch impregnating autoclave, used around graphite foam Coal tar pitch embeds, and closing lid is warming up to 200 DEG C and is evacuated to -0.1MPa, and 15MPa, heat-insulation pressure keeping 4 are pressurized to after heat-insulation pressure keeping 1h Freely cool after hour.
(3) sample after dipping coal tar pitch in step (2), is put into progress normal pressure carbonization in carbide furnace, carbonization technique is bent Line is：Room temperature~350 DEG C, 10 DEG C/min of heating rate；350~500 DEG C, 1 DEG C/min of heating rate；500 DEG C, it is incubated 3h；500 ~650 DEG C, 1 DEG C/min of heating rate；650 DEG C, it is incubated 5h；650~900 DEG C, 3 DEG C/min of heating rate, 900 DEG C, it is incubated 3h； Freely cool.
(4), the sample after being carbonized in step (3) is put into high temperature furnace and carries out high-temperature process, high-temperature processing technology curve For：Room temperature~900 DEG C, 10 DEG C/min of heating rate；900~1200 DEG C, 5 DEG C/min of heating rate；1200 DEG C of insulation 3h；1200 DEG C~2000 DEG C, 3 DEG C/min of heating rate；2000 DEG C, it is incubated 3h；Control 10 DEG C/min of rate of temperature fall is down to 900 until temperature Below DEG C；Less than 900 DEG C freely cool.
(5), repeat step (2) and step (3), impregnation pressure reach 50MPa, freely cooled after heat-insulation pressure keeping 3h.
(6), repeat step (4), maximum heat treatment temperature are adjusted to 2300 DEG C, and now density of material reaches 1.38g/cm3。
(7) material in step (6), is put into superhigh temperature graphitizing furnace progress superhigh temperature graphitization processing, with 1~5 DEG C/ Min speed is warming up to 3000 DEG C and is incubated 10h, then freely cools, and completes graphitization processing, that is, high heat conduction stone is prepared Black foam/carbon composite.
High heat conduction graphite foam/carbon composite final densities are 1.35g/cm3, thermal conductivity 304W/mK, compression is by force Spend for 9.0MPa.
Embodiment 2
(1), use softening point as 275 DEG C of mesophase pitch, pressure be 7.5MPa, temperature be that 330 DEG C of conditions issue Type is soaked, preparing high heat conduction graphite foam by 900 DEG C of carbonizations and 3000 DEG C of graphitizations is used as enhancing base, prepared graphite foam Enhancing base density is 0.65g/cm3, thermal conductivity 152W/mK, porosity 71%, percent opening is more than 90%.
(2), the graphite foam enhancing base prepared in step (1) is put into mesophase pitch impregnating autoclave, graphite foam week To enclose and embedded with mesophase pitch, closing lid is warming up to 330 DEG C and is evacuated to -0.1MPa, and 25MPa is pressurized to after heat-insulation pressure keeping 1h, Heat-insulation pressure keeping freely cools after 4 hours.
(3) sample after dipping mesophase pitch in step (2), is put into progress normal pressure carbonization, carbonizer in carbide furnace Skill curve is：Room temperature~350 DEG C, 10 DEG C/min of heating rate；350~500 DEG C, 3 DEG C/min of heating rate；500 DEG C, insulation 5h；500~650 DEG C, 1 DEG C/min of heating rate；650 DEG C, it is incubated 5h；650~900 DEG C, heating rate 3 DEG C/min, 900 DEG C, It is incubated 3h；Freely cool.
(4), the sample after being carbonized in step (3) is put into high temperature furnace and carries out high-temperature process, high-temperature processing technology curve For：Room temperature~900 DEG C, 10 DEG C/min of heating rate；900~1200 DEG C, 5 DEG C/min of heating rate；1200 DEG C of insulation 2h；1200 DEG C~2300 DEG C, 3 DEG C/min of heating rate；2300 DEG C, it is incubated 4h；Control 10 DEG C/min of rate of temperature fall is down to 900 until temperature Below DEG C；Less than 900 DEG C freely cool.
(5), repeat step (2) and step (3), impregnation pressure reach 50MPa, freely cooled after heat-insulation pressure keeping 3h.
(6), repeat step (4), maximum heat treatment temperature are adjusted to 2500 DEG C, and now density of material reaches 1.45g/cm3。
(7) material, is put into progress superhigh temperature graphitization processing in superhigh temperature graphitizing furnace, with 1~5 DEG C/min speed It is warming up to 3000 DEG C and is incubated 10h, then freely cool, complete graphitization processing, that is, it is compound that high heat conduction graphite foam/carbon is made Material.
High heat conduction graphite foam/carbon composite final densities are 1.42g/cm3, thermal conductivity 351W/mK, compression is by force Spend for 9.5MPa.
It is described above, it is only the optimal embodiment of the present invention, but protection scope of the present invention is not limited thereto, Any one skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in, It should all be included within the scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.

Claims (4)

  1. A kind of 1. preparation method of high heat conduction graphite foam/carbon composite, it is characterised in that：Comprise the following specific steps that：
    Step (1), using mesophase pitch as presoma prepare high heat conduction graphite foam as strengthen base, the high heat conduction graphite The density of foam enhancing base is 0.5~0.9g/cm3, thermal conductivity is more than 100W/mK, and for porosity 39~77%, percent opening is big In 85%；
    Step (2), the graphite foam enhancing base for preparing step (1) carries out mesophase pitch or coal tar pitch impregnates；In wherein Between asphalt phase dipping temperature be 280-370 DEG C, impregnation pressure 15-70MPa, dwell time 1-5h；Coal tar pitch dipping temperature For 160-240 DEG C, impregnation pressure 15-70MPa, dwell time 1-5h；
    Step (3), step (2) is impregnated to the graphite foam progress carbonization treatment after mesophase pitch or coal tar pitch；
    Step (4), the C-base composte material obtained after step (3) carbonization treatment is put into high temperature furnace carries out high-temperature process；
    Step (5), judge whether the composite density after high-temperature process exceedes given threshold, be not above given threshold then Return to step (two), increase impregnation pressure when mesophase pitch or coal tar pitch dipping；Composite density exceedes given threshold, Perform step (6)；
    Step (6), by C-base composte material carry out superhigh temperature graphitization processing, it is compound that high heat conduction graphite foam/carbon is prepared Material；
    Carbonization treatment technique curve is in the step (3)：Room temperature~350 DEG C, heating rate are 5~15 DEG C/min；350~ 500 DEG C, heating rate is 1~5 DEG C/min；500 DEG C, it is incubated 1~10h；500~650 DEG C, heating rate is 1~5 DEG C/min； 650 DEG C, it is incubated 1~10h；650~900 DEG C, heating rate is 3~5 DEG C/min, 900 DEG C, is incubated 1~5h；Freely cool；
    Superhigh temperature graphitization processing process curve is in the step (6)：3000 DEG C are warming up to 1~15 DEG C/min speed Above and 1~10h is incubated, freely cooled；
    Given threshold is 1.3g/cm3；
    The thermal conductivity of high heat conduction graphite foam/carbon composite is more than 300W/mK.
  2. A kind of 2. preparation method of high heat conduction graphite foam/carbon composite according to claim 1, it is characterised in that： The step (4) high temperature handling process curve is：Room temperature~900 DEG C, heating rate are 10~20 DEG C/min；900~1200 DEG C, heating rate is 5~10 DEG C/min；1200 DEG C of 1~5h of insulation；1200 DEG C~target process temperature, heating rate is 3~5 ℃/min；1~5h is incubated under target process temperature；Control rate of temperature fall for 5~15 DEG C/min until temperature be down to 900 DEG C with Under；Less than 900 DEG C freely cool；The target process temperature is 1800 DEG C~2500 DEG C.
  3. A kind of 3. preparation method of high heat conduction graphite foam/carbon composite according to claim 1, it is characterised in that： Prepare high heat conduction graphite foam as presoma using mesophase pitch in step (1) is specially as enhancing base：Use softening point for 220-300 DEG C of mesophase pitch foaming, high heat conduction graphite foam is prepared as enhancing by carbonization and graphitization processing Base.
  4. A kind of 4. preparation method of high heat conduction graphite foam/carbon composite according to claim 1, it is characterised in that： Composite density is not above given threshold then return to step (two) in the step (5), increases mesophase pitch or coal drip Impregnation pressure during green grass or young crops dipping, and heighten the temperature that high-temperature process is carried out in high temperature furnace.
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CN107651671B (en) * 2017-10-13 2019-10-15 杭州高烯科技有限公司 A kind of method and a kind of preparation method of super flexible high thermal conductivity graphene film of catalyzed graphitization
CN108314458B (en) * 2018-02-09 2020-07-21 陕西天策新材料科技有限公司 Preparation method of high-thermal-conductivity carbon/carbon composite material
CN110357076A (en) * 2019-07-17 2019-10-22 常州富烯科技股份有限公司 A kind of grapheme foam and preparation method thereof, graphene carbon composite material and preparation method
CN111154458A (en) * 2020-01-19 2020-05-15 中国科学院上海应用物理研究所 Graphite foam erythritol phase-change heat storage material and preparation method thereof
CN113149649A (en) * 2021-03-29 2021-07-23 湖南长宇科技发展有限公司 Mesophase-like asphalt and preparation method and application thereof

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