CN109763209A - A method of manufacture high thermal conductivity asphalt base carbon fiber - Google Patents
A method of manufacture high thermal conductivity asphalt base carbon fiber Download PDFInfo
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- CN109763209A CN109763209A CN201910097323.XA CN201910097323A CN109763209A CN 109763209 A CN109763209 A CN 109763209A CN 201910097323 A CN201910097323 A CN 201910097323A CN 109763209 A CN109763209 A CN 109763209A
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Abstract
The present invention relates to a kind of methods for manufacturing high thermal conductivity asphalt base carbon fiber, comprising: (1) powder containing boron element is added into pitch, stirs evenly, spinning material is made；(2) spun is made through spinning in spinning material made from step (1)；(3) spun made from step (2) is oxidation-treated；Then carbonization treatment；Again through graphitization processing to get.Present invention firstly discloses the powder containing boron element is added into asphalt stock, it then will be handled under a series of specified conditions such as pitch spinning, oxidation, carbonization, graphitization, obtain high thermal conductivity type asphalt base carbon fiber；The addition of boron element directly results in the variation of the arrangement of carbon atom, and then the carbon fiber made from ensuring significantly reduces the requirement such as temperature condition in production process, significantly reduce production cost under the premise of with excellent heat conductivity performance.
Description
Technical field
The present invention relates to a kind of methods for manufacturing high thermal conductivity asphalt base carbon fiber, belong to asphalt-based carbon fiber technology of preparing neck
Domain.
Background technique
High thermal conductivity asphalt-based carbon fiber is a kind of dual-use industrial materials of unique energy, the army of being widely used in
The reinforcement of the advanced composite materials such as work, space flight, aviation, sports equipment, high-grade civilian goods.It should be noted that highly-conductive hot carbon fiber
In addition to the characteristic superpower with heating conduction, also there are the characteristics such as lightweight, high-strength, superelevation mould, highly conductive, low thermal coefficient of expansion,
It is best suited for the big space environment of day and night temperature, the various structures that thermal expansion coefficient is zero can be prepared by using it as reinforcement
Type and functional material, it has also become solve the indispensable reinforcement of outer space structural and functional composite materials.It is external
It has been achieved with and commercially produces, China is also in development and trial production stage；Beauty, Deng developed country are classified as strategic materials
Control is carried out, international market stops selling to China, the serious development for restricting China's national defense related fields.Therefore, accelerate high
The development and production of thermally conductive carbon fiber are extremely urgent challenges.
But since the C atomic arrangement inside asphalt-based carbon fiber is mixed and disorderly, the thermal conductivity of general asphalt-based carbon fiber is only 70W/
M K or so, the prior art are to improve its heating conduction, generally use the method for improving treatment temperature and make internal carbon atom row
What is arranged is more regular, to improve its thermal conductivity.Plain asphalt carbon fiber is handled system by domestic generally use under 2800 degree of high temperature
Heat-conducting type carbon fiber is obtained, this method and process is complicated, and energy consumption is high, and the fiber thermal conductivity prepared is general, usually in 400W/
M K or so (the thermally conductive of copper is 401W/m K) close with copper, to continue to improve thermal conductivity, it is necessary to increase temperature, this is not only right
Relevant device proposes harsher requirement, and energy consumption height, complex process, yield rate are low, and cost is caused to significantly rise.
Chinese patent literature TW200420647A(application number TW092127823) it discloses B4C powder and divinyl four
After amine, 6101 epoxy resin, acetone are mixed and are sufficiently stirred with the ratio of 1:1:10:10, the pitch coated on carbonization treatment is fine
Dimension table face adds tension 11g in 2500 degree, 2800 degree of graphitization processings respectively after solidification.Although the technology can be improved part and lead
Hot property, but still it is unable to reach expected requirement, and product length is unable to satisfy use demand.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of methods for manufacturing high thermal conductivity asphalt base carbon fiber.This method
It can solve domestic asking using conventional method production high thermal conductivity asphalt-based carbon fiber low efficiency, the high requirements on the equipment and complex process
Topic.
Technical scheme is as follows:
A method of manufacture high thermal conductivity asphalt base carbon fiber includes the following steps:
(1) powder containing boron element is added into pitch by 0.2~1.0% mass percent, stirs evenly, it is former that spinning is made
Material；
(2) spinning material made from step (1) is made and is just spun through spinning under the conditions of 380~420 ms/min of draft speed
Silk；
(3) by spun made from step (2) through 25~35min of oxidation processes under 280~320 DEG C of air environments, air supply
Amount are as follows: 45~55L/min, every gram of spun applies 4.5~5.5g tension when oxidation；Then in 950 DEG C~1050 DEG C nitrogen rings
15~25min of carbonization treatment in border, every gram of oxidation silk applies 9~11g of tension when carbonization；Again through 2400~2600 DEG C of ar gas environments
Middle 8~12min of graphitization processing, when graphitization every gram of carbonization silk apply 9~11g of tension to get.
Preferred according to the present invention, in the step (1), the powder containing boron element is boron carbide powder.
Preferred according to the present invention, in the step (1), the partial size of the powder containing boron element is no more than 0.1 μm；Further
Preferably, the partial size of the powder containing boron element is 30~60nm.
Preferred according to the present invention, in the step (1), pitch is mesophase pitch；It is further preferred that the pitch
Index of correlation it is as follows: interphase content >=98%, 280~290 DEG C of softening point, quinoline insolubles 30~40%, density 1.20~
1.35g/cm3, 70~90PPM of ash content.
Preferred according to the present invention, in the step (1), the additional amount of the powder containing boron element is 0.4~0.8%；Into one
Step is preferred, and the additional amount of the powder containing boron element is 0.5%, 0.6%, 0.7% or any range between the two.
Preferred according to the present invention, in the step (2), draft speed is 390~410 ms/min；Further preferably
, draft speed is 390 ms/min, 395 ms/min, 400 ms/min, 405 ms/min, 410 ms/min or any the two
Between range.
Preferred according to the present invention, in the step (3), oxidizing temperature is 290~310 DEG C；It is further preferred that oxidation
Temperature is 290 DEG C, 295 DEG C, 300 DEG C, 305 DEG C, 310 DEG C or any range between the two.
Preferred according to the present invention, in the step (3), oxidization time is 28~32min；It is further preferred that oxidation
Temperature is 28 min, 29 min, 30min, 31min, 32min or any range between the two.
Preferred according to the present invention, in the step (3), air supply amount is 48~52L/min；It is further preferred that
The range that air supply amount is 48 L/min, 49 L/min, 50 L/min, 51 L/min, 52 L/min or any are between the two.
Preferred according to the present invention, in the step (3), the tension that when oxidation applies is 4.8~5.2g；Further preferably
, the tension that when oxidation applies is 4.8g, 4.9g, 5.0g, 5.1g, 5.2g or any range between the two.
Preferred according to the present invention, in the step (3), carburizing temperature is 980 DEG C~1020 DEG C；It is further preferred that
Carburizing temperature is 980 DEG C, 990 DEG C, 1000 DEG C, 1010 DEG C, 1020 DEG C or any range between the two.
Preferred according to the present invention, in the step (3), carbonization time is 18~22min；It is further preferred that carbonization
The range that time is 18min, 19 min, 20 min, 21min, 22 min or any are between the two.
It is preferred according to the present invention, in the step (3), carbonization apply tension be 9g, 9.5g, 10g, 10.5g, 11g or
Any range between the two.
Preferred according to the present invention, in the step (3), graphitization temperature is 2450 DEG C~2550 DEG C；Further preferably
, carburizing temperature be 2450 DEG C, 2460 DEG C, 2470 DEG C, 2480 DEG C, 2490 DEG C, 2500 DEG C, 2510 DEG C, 2520 DEG C, 2530 DEG C,
2540 DEG C, 2550 DEG C or any range between the two.
It is preferred according to the present invention, in the step (3), graphitization time 8min, 9 min, 10 min, 11min, 12
Min or any range between the two.
Preferred according to the present invention, in the step (3), it is 9g, 9.5g, 10g, 10.5g, 11g that graphitization, which applies tension,
Or any range between the two.
Technological principle of the invention:
This reaction is mainly the high-temperature process of fiber after oxidation reaction and oxidation respectively there are two the stage；In oxidation process, to
Appropriate air is passed through in reacting furnace, to guarantee oxidation completely, air capacity should be 80~100 times of actual requirement or so；Oxidation
After the reaction was completed, into the high-temperature process stage, need to be passed through nitrogen protection, nitrogen itself is not involved in reaction, therefore to intake
Principle be to guarantee that fire door both ends have nitrogen to escape so that air not can enter in furnace；
Pitch is after fiber is made in spinning, oxidation, carbonization, graphitization, although mode of appearance is changed, from massive transformation
Carbon atom distribution for threadiness, but inside is constantly in mixed and disorderly state, so that the hot property of fiber does not significantly improve.Invention
People is by the way that the study found that the boron element of certain content is introduced into inside asphaltene molecule, in oxidation process, boron atom is in pitch
The distribution of fiber radially makes it in pre-oxidizing stage and oxygen knot in low inside and high outside parabolic shape due to the electron deficient of boron
Symphysis is covered on fiber surface and inhibits pre-oxidation rate at B-O compound, and oxygen element is made to be easy to spread to fibrous inside,
More cyclizations have occurred, slow down the skin-core structure of preoxidized fiber, make its radial structure more homogeneous；In carbonation stage,
Partially carbonized boron thermal decomposition is with the removing of boron gas procedure, and part of boron diffuses into carbon lattice and forms substitution solid solution with carbon, i.e.,
Boron carbide.There are many kinds of the microstructures of boron carbide, and the metastable boron carbide structure in part is decomposed at a certain temperature, and be carbonized rank
Section adds B4The carbon fiber crystallite dimension of C is larger, interlamellar spacing is smaller, degree of graphitization is high, respectively reach 3.02,3.3945A,
52.9%, in contrast, at a temperature of lower 1600 DEG C, the graphite fiber degree for being not added with boron is 23.37%.With processing temperature
The raising of degree, carbon fiber and graphite degree further increase.Tested and found by Raman, add the carbon fiber core-skin of boron carbide because
Son is 0.88, and the skin-core structure for being not added with the carbon fiber of boron is 0.78, illustrates that boron can effectively weaken skin-core structure, is improved
Fibrous inside is loose, disordered structure state, reduces its inside and outside otherness, facilitates the carbon fiber for preparing high thermal conductivity.
Beneficial effect
Present invention firstly discloses into asphalt stock add the powder containing boron element, then by pitch spinning, oxidation, carbonization,
It is handled under a series of specified conditions such as graphitization, obtains high thermal conductivity type asphalt base carbon fiber；The addition of boron element directly results in
The variation of the arrangement of carbon atom, so ensure carbon fiber obtained under the premise of with excellent heat conductivity performance, it is significant to drop
Temperature condition in low production process etc. requires, and significantly reduces production cost.
Detailed description of the invention
Fig. 1 is electron microscope (SEM) figure of oxidation silk prepared by comparative example 1；
Fig. 2 is oxidation silk electron microscope (SEM) figure prepared by embodiment 1；
Fig. 3 is electron microscope (SEM) figure of carbonization silk prepared by comparative example 1；
Fig. 4 is electron microscope (SEM) figure of carbonization silk prepared by embodiment 1；
Fig. 5 is Fourier transform infrared spectroscopy (FT-IR) figure of carbon fiber prepared by embodiment 1 and comparative example 1.
Specific embodiment
Technical solution of the present invention is further elaborated below with reference to examples and drawings, but institute's protection scope of the present invention
It is without being limited thereto.
Raw material sources
B4C powder is purchased from Nano-technology Development Co., Ltd, Hefei Air China, and partial size is averaged 50nm, purity >=99.99%；
Pitch is common commercially available mesophase pitch, technical indicator are as follows:
Interphase content: >=98%
Softening point: 285 DEG C
Quinoline insolubles: 37%
Density: 1.32g/cm3
Ash content: 80PPM
Embodiment 1
A method of manufacture high thermal conductivity asphalt base carbon fiber includes the following steps:
(1) B is added into pitch by 0.2% mass percent4C powder, stirs evenly, and spinning material is made；
(2) spun is made through spinning under the conditions of 400 ms/min of draft speed in spinning material made from step (1)；
(3) by spun made from step (2) through 300 DEG C, in air supply amount 50L/min plus tension 5g oxidation processes 30min
Afterwards, under 1000 DEG C of nitrogen environments plus tension 10g carbonization treatment 20min, then through under 2500 DEG C of ar gas environments plus tension 10g stone
Inkization handle 10min to get.
The method conductometer LF467 detection that shines of gained fiber, thermal conductivity reaches 580W/m K, higher than fine copper thermal conductivity by 37%,
It is higher by 37% than the plain asphalt carbon fiber of 2800 degree of processing, and mechanical property slightly improves.Since graphitization temperature is only 2500
Degree, is significantly less than 2800 degree of conventional method, and only this item just makes energy consumption save 30%.
Embodiment 2
A method of manufacture high thermal conductivity asphalt base carbon fiber includes the following steps:
(1) B is added into pitch by 0.5% mass percent4C powder, stirs evenly, and spinning material is made；
(2) spun is made through spinning under the conditions of 380 ms/min of draft speed in spinning material made from step (1)；
(3) by spun made from step (2) through 320 DEG C, in air supply amount 45L/min plus tension 4.5g oxidation processes
After 30min, under 1000 DEG C of nitrogen environments plus tension 11g carbonization treatment 20min, then through under 2400 DEG C of ar gas environments plus tension
11g graphitization processing 10min to get.
The method conductometer LF467 detection that shines of gained fiber, thermal conductivity 596W/m K.
Embodiment 3
A method of manufacture high thermal conductivity asphalt base carbon fiber includes the following steps:
(1) B is added into pitch by 1.0% mass percent4C powder, stirs evenly, and spinning material is made；
(2) spun is made through spinning under the conditions of 420 ms/min of draft speed in spinning material made from step (1)；
(3) by spun made from step (2) through 280 DEG C, in air supply amount 55L/min plus tension 5.5g oxidation processes
After 30min, under 1000 DEG C of nitrogen environments, plus tension 9g carbonization treatment 20min, then through under 2600 DEG C of ar gas environments plus tension
9g graphitization processing 19min to get.
The method conductometer LF467 detection that shines of gained fiber, thermal conductivity are 575W/m K.
Embodiment 4
A method of manufacture high thermal conductivity asphalt base carbon fiber includes the following steps:
(1) B is added into pitch by 0.2% mass percent4C particle, stirs evenly by 0.1 μm of partial size, and spinning material is made；
(2) spun is made through spinning under the conditions of 400 ms/min of draft speed in spinning material made from step (1)；
(3) by spun made from step (2) through under 300 DEG C of air environments, in air supply amount 50L/min, plus tension 5g oxygen
After changing processing 30min, under 1000 DEG C of nitrogen environments, plus tension 10g carbonization treatment 20min, then through under 2500 DEG C of ar gas environments,
Add tension 10g graphitization processing 10min to get.
The method conductometer LF467 detection that shines of gained fiber, thermal conductivity are 508W/m K.
Can be seen that the two by the result of embodiment 1 and embodiment 4 is only B4The partial size of C particle is different, but leads to two
Person's thermal conductivity has significant difference.This may be since partial size difference leads to B4The degree difference that is uniformly dispersed of C particle, Jin Erying
The microstructure of fiber is rung, the thermal conductivity so as to cause embodiment 4 is remarkably decreased.
Comparative example 1
Method as described in Example 1, graphitization temperature point ratio are 2500 degree and 2800 degree, the difference is that, in pitch not
Add B4C powder.
Gained fiber carries out coherent detection, with the method conductometer LF467 detection that shines, testing result: after 2500 degree of processing
Fiber thermal conductivity is 320 W/m K, and fiber thermal conductivity is 423 W/m K after 2800 degree of processing.
Table 1 is not added with B4C and it is added to B4The degree of graphitization of the carbon fiber of C compares
| g/% | 1200℃ | 1300℃ | 1400℃ | 1500℃ | 1600℃ |
| Embodiment 1 | — | 3.60 | 23.48 | 40.58 | 52.90 |
| Comparative example 1 | — | — | — | — | 23.37 |
From table 1, it is apparent that being not added with the carbon fiber of boron carbide at 1600 degree or less substantially without graphite-structure, and add
Add the carbon fiber of boron carbide to produce graphite-structure at 1300 degree, has equally been 1600 degree, the degree of graphitization of the latter reaches
52.90%, it is far longer than the carbon fiber for being not added with boron carbide.Therefore, we can make the inside of carbon fiber with lower temperature
Molecules align is to graphite transition.
The fiber in comparative example 1 and 1 step of embodiment (3) after oxidation and after carbonization is detected respectively, as a result such as Fig. 1 to Fig. 2
Shown, comparative example 1 is not added with B4The oxidized fibre (Fig. 1) of C, the hole that section generates are apparently higher than embodiment 1 and are added to B4C
Oxidized fibre (Fig. 2), which results in generating more holes (Fig. 3) when continuing high-temperature process, and (Fig. 4) is by being added to
B4It is obtained after the fiber high temperature processing of C, the hole of section is considerably less than (Fig. 3).Fiber cross-sectional hole is fewer, illustrates fiber
Internal Char Residues Structure is more regular, and heating conduction also can be better.
Product prepared by embodiment 1 and comparative example 1 is detected by Fourier transform infrared spectroscopy, as a result as shown in Figure 5.By
Fig. 5 can be seen that in the infrared spectrogram of the embodiment 1 of addition boron carbide carbon fiber in 1380 cm-1There is the feature of B-N key
Absorption peak, what this 1600 DEG C of explanation was truly has BN compound to exist.In addition, 1600cm-1The absorption peak that place represents B-C appears in carbon
In fiber infrared spectrum, it is not added with B4The peak intensity of the comparative example 1 of the carbon fiber of C here is higher than embodiment 1 and adds boron carbide
Peak intensity, illustrate to be added to B under identical heat treatment temperature4The carbon fiber cyclisation structural rearrangement of C simultaneously discharges the reaction of nitrogen more
Sufficiently, the phosphorus content of carbon fiber will it is higher, performance is more preferable.
Comparative example 2
According to the content that TaiWan, China patent (TW200420647A) is recorded, it is prepared as follows:
By B4After C powder and divinyl tetramine, 6101 epoxy resin, acetone are mixed and are sufficiently stirred with the ratio of 1:1:10:10,
Pitch fibers surface coated on carbonization treatment adds tension 11g in 2500 degree, 2800 degree of graphitization processings respectively after solidification.
Gained fiber carries out coherent detection, and with the method conductometer LF467 detection that shines, fiber thermal conductivity is respectively 390W/m K
With 480W/m K.
Interpretation of result
It can be seen that by the comparison of embodiment 1 and the product-related data of comparative example 2 since embodiment 1 manufactures high thermal conductivity drip
Green base carbon fibre is boron carbide powder to be mixed in asphalt stock to carry out spinning, through peroxidating, carbonization and graphitization processing, manufacture
The internal asphalt base carbon fiber containing boron element out, this differs markedly from 2 TaiWan, China patent (TW200420647A) of comparative example
The surface spraying method of use, surface coat B4The purpose of C powder is not thermally conductive in order to improve, but heat-resisting in order to improve
Property and electric conductivity, therefore, which is simultaneously not concerned with fibrous inner structure.In addition, embodiment 1 manufactures high thermal conductivity asphalt base carbon fiber
It is that long fibre is obtained by spinning, it is possible to produce long fibre tow is woven into two dimension or three-dimensional carbon fibre fabric, is used as carbon
The reinforcement of fiber/resin composite material and carbon/carbon compound material prepares highly heat-conductive material, and prepared by comparative example 1 is
Staple fiber.
Claims (10)
1. a kind of method for manufacturing high thermal conductivity asphalt base carbon fiber, which comprises the steps of:
(1) powder containing boron element is added into pitch by 0.2~1.0% mass percent, stirs evenly, it is former that spinning is made
Material；
(2) spinning material made from step (1) is made and is just spun through spinning under the conditions of 380~420 ms/min of draft speed
Silk；
(3) by spun made from step (2) through 25~35min of oxidation processes under 280~320 DEG C of air environments, air supply
Amount are as follows: 45~55L/min, every gram of spun applies 4.5~5.5g tension when oxidation；Then in 950 DEG C~1050 DEG C nitrogen rings
15~25min of carbonization treatment in border, every gram of oxidation silk applies 9~11g of tension when carbonization；Again through 2400~2600 DEG C of ar gas environments
Middle 8~12min of graphitization processing, when graphitization every gram of carbonization silk apply 9~11g of tension to get.
2. the method as described in claim 1, which is characterized in that in the step (1), the powder containing boron element is boron carbide powder
End.
3. the method as described in claim 1, which is characterized in that in the step (1), the partial size of the powder containing boron element does not surpass
Cross 0.1 μm；It is further preferred that the partial size of the powder containing boron element is 30~60nm.
4. the method as described in claim 1, which is characterized in that in the step (1), pitch is mesophase pitch；Further
Preferably, the index of correlation of the pitch is as follows: interphase content >=98%, and 280~290 DEG C of softening point, quinoline insolubles 30~
40%, 1.20~1.35g/cm of density3, 70~90PPM of ash content.
5. the method as described in claim 1, which is characterized in that in the step (1), the additional amount of the powder containing boron element is
0.4~0.8%；It is further preferred that the additional amount of the powder containing boron element is 0.5%, 0.6%, 0.7% or any the two
Between range.
6. the method as described in claim 1, which is characterized in that in the step (2), draft speed is 390~410 ms/min
Clock；It is further preferred that draft speed be 390 ms/min, 395 ms/min, 400 ms/min, 405 ms/min, 410 meters/
Minute or any range between the two.
7. the method as described in claim 1, which is characterized in that in the step (3), oxidizing temperature is 290~310 DEG C；Into
One step is preferred, and oxidizing temperature is 290 DEG C, 295 DEG C, 300 DEG C, 305 DEG C, 310 DEG C or any range between the two；
Preferably, in the step (3), oxidization time is 28~32min；It is further preferred that oxidizing temperature is 28 min, 29
Min, 30min, 31min, 32min or any range between the two；
Preferably, in the step (3), air supply amount is 48~52L/min；It is further preferred that air supply amount is 48
L/min, 49 L/min, 50 L/min, 51 L/min, 52 L/min or any range between the two；
Preferably, in the step (3), the tension that when oxidation applies is 4.8~5.2g；It is further preferred that applying when oxidation
Tension be 4.8g, 4.9g, 5.0g, 5.1g, 5.2g or any range between the two；
Preferably, in the step (3), carburizing temperature is 980 DEG C~1020 DEG C；It is further preferred that carburizing temperature is 980
DEG C, 990 DEG C, 1000 DEG C, 1010 DEG C, 1020 DEG C or any range between the two；
Preferably, in the step (3), carbonization time is 18~22min；It is further preferred that carbonization time is 18min, 19
Min, 20 min, 21min, 22 min or any range between the two；
Preferably, in the step (3), it is that 9g, 9.5g, 10g, 10.5g, 11g or any are between the two that carbonization, which applies tension,
Range.
8. the method as described in claim 1, which is characterized in that in the step (3), graphitization temperature is 2450 DEG C~2550
℃；It is further preferred that carburizing temperature be 2450 DEG C, 2460 DEG C, 2470 DEG C, 2480 DEG C, 2490 DEG C, 2500 DEG C, 2510 DEG C,
2520 DEG C, 2530 DEG C, 2540 DEG C, 2550 DEG C or any range between the two.
9. the method as described in claim 1, which is characterized in that in the step (3), graphitization time 8min, 9 min,
10 min, 11min, 12 min or any range between the two.
10. the method as described in claim 1, which is characterized in that in the step (3), graphitization apply tension be 9g,
9.5g, 10g, 10.5g, 11g or any range between the two.
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| CN110157476A (en) * | 2019-06-13 | 2019-08-23 | 北京化工大学 | A method of manufacture highly-conductive hot carbon fiber mesophase pitch |
| CN110983491A (en) * | 2019-12-17 | 2020-04-10 | 北京研韵新材料科技有限公司 | Method for manufacturing high-thermal-conductivity mesophase pitch-based carbon fibers at low temperature |
| CN114232215A (en) * | 2021-12-20 | 2022-03-25 | 西安工程大学 | Preparation method and application of asphalt-based carbon nanofiber multistage non-woven fabric with three-dimensional cavity structure |
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| CN110144643A (en) * | 2019-05-21 | 2019-08-20 | 湖南东映碳材料科技有限公司 | A kind of preparation method of high-performance intermediate phase pitch-based graphite fibre |
| CN110144643B (en) * | 2019-05-21 | 2021-05-25 | 湖南东映碳材料科技有限公司 | Preparation method of high-performance mesophase pitch-based graphite fiber |
| CN110157476A (en) * | 2019-06-13 | 2019-08-23 | 北京化工大学 | A method of manufacture highly-conductive hot carbon fiber mesophase pitch |
| CN110157476B (en) * | 2019-06-13 | 2020-04-28 | 北京化工大学 | Method for manufacturing mesophase pitch for high-thermal-conductivity carbon fibers |
| CN110983491A (en) * | 2019-12-17 | 2020-04-10 | 北京研韵新材料科技有限公司 | Method for manufacturing high-thermal-conductivity mesophase pitch-based carbon fibers at low temperature |
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