CN104211423A - Preparation method of graphene modified carbon/carbon composite material - Google Patents
Preparation method of graphene modified carbon/carbon composite material Download PDFInfo
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- CN104211423A CN104211423A CN201410473041.2A CN201410473041A CN104211423A CN 104211423 A CN104211423 A CN 104211423A CN 201410473041 A CN201410473041 A CN 201410473041A CN 104211423 A CN104211423 A CN 104211423A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- -1 graphene modified carbon Chemical class 0.000 title abstract 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 239000010426 asphalt Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 21
- 150000001722 carbon compounds Chemical class 0.000 claims description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 17
- 238000012986 modification Methods 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 4
- 238000006424 Flood reaction Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000005087 graphitization Methods 0.000 abstract description 7
- 239000000835 fiber Substances 0.000 abstract description 4
- 150000001721 carbon Chemical class 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract description 2
- 238000005452 bending Methods 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 20
- 239000011159 matrix material Substances 0.000 description 11
- 239000004917 carbon fiber Substances 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Abstract
The invention relates to a preparation method of a modified carbon/carbon composite material, in particular relates to a preparation method of a graphene modified carbon/carbon composite material, and is used for solving the problem of poor performance of an existing carbon/carbon composite material. The method comprises the following steps: 1, performing coating treatment on a preform by a graphene solution; 2, performing liquid-phase impregnation on the preform by asphalt; 3, repeating the step 2 for 2-3 times, heating the asphalt, soaking the treated preform in the asphalt under the normal pressure, and taking out; 4, carbonizing the soaked preform; 5, repeating the steps 2 to 4 for 4 times, putting a sample into a carbonization furnace, heating under the argon protection, keeping constant temperature, cooling, and taking out the sample to obtain the graphene modified carbon/carbon composite material. According to the method, the graphitization degree, bending strength and fiber bundle/substrate interface shear strength of the graphene modified carbon/carbon composite material can be improved; the method is used for preparing the modified carbon/carbon composite material.
Description
Technical field
The present invention relates to a kind of preparation method of modifying carbon/carbon composite material.
Background technology
Carbon/carbon compound material is a kind of is reinforcement with carbon fiber, and carbon is the heterogeneous carbon body be made up of the different states of identity element of matrix.Due to the existence of different structure form, carbon/carbon compound material is caused to there is the different interfacial layer of four parts: the fiber/matrix interface in fibrous bundle; Carbon fiber bundle/basal body interface; The interface that the different micro-song of intrinsic silicon is formed; Interface between matrix and hole or crackle.Interface is the bridge connecting the pre-matrix carbon of carbon fiber, plays transmitted load, changes the effect of direction of crack propagation.The power of interface binding power directly decides mechanical behavior under high temperature and the heat physical properties of carbon/carbon compound material.Interface bond strength easily causes carbon/carbon compound material generation brittle rupture behavior too by force, and the too weak meeting of interface bond strength makes carbon fiber unsticking from matrix extract, and weakens the enhancement of carbon fiber.In carbon/carbon compound material, because the effect connecting different structure region and transmitted load is played at interface, therefore the performance that modification can improve matrix material is well carried out to composite material interface.
Summary of the invention
The present invention is the problem of the poor performance that will solve existing carbon/carbon compound material, provides a kind of preparation method of Graphene modifying carbon/carbon composite material.
The preparation method of Graphene modifying carbon/carbon composite material of the present invention, carries out according to the following steps:
One, carbon fabric perform is immersed in the N-Methyl pyrrolidone solution of Graphene, supersound process, then carbon fabric perform taking-up is put in baking oven, in 150 DEG C of oven dry;
Two, first with pitch/N-Methyl pyrrolidone solution, precast body is flooded, carry out supersound process simultaneously, then precast body is taken out and be put in baking oven, in 120 DEG C of oven dry;
Three, repeating step 22 ~ 3 times, by asphalt heating to 260 DEG C ~ 280 DEG C, then immerse in pitch by the precast body processed, normal pressure floods, and then takes out;
Four, the precast body after bituminizing is placed in the carbide furnace under 0.1MPa argon shield, is warming up to 400 DEG C, keep temperature 2h, be then raised to 800 DEG C, keep temperature 2h, finally temperature is raised to 1200 DEG C, insulation 2h, then lower the temperature, treat that furnace temperature is down to room temperature, take out the sample after carbonization;
Five, repeating step two to step 44 times, then puts into carbide furnace by sample, under 0.1MPa argon shield, is warming up to 1900 DEG C, keeps temperature 1h, and cooling, treats the near room temperature of furnace temperature, takes out sample, i.e. the carbon/carbon compound material of obtained Graphene modification.
The present invention is the carbon fabric perform using the N-Methyl pyrrolidone solution coatings process of Graphene to weave, and then use bituminizing precast body, carbonization, greying, then repeated impregnations, carbonization, greying several times, prepare carbon/carbon compound material.
After tested, the carbon/carbon compound material degree of graphitization of Graphene modification can reach 90.56%; Flexural strength can reach 234.21MPa, improves 25.5% compared with the material without Graphene modification; Through the carbon/carbon compound material fibrous bundle/matrix interface shear strength of Graphene modification compared with non-modified, can 24.1% be improved.
Accompanying drawing explanation
Fig. 1 is the flexural strength column diagram of modifying carbon/carbon composite material obtained in test 1-4; Fig. 2 is the fibrous bundle/basal body interface average shear strength column diagram of modifying carbon/carbon composite material obtained in test 1-4; Fig. 3 is the interface SEM image of carbon fiber and matrix in test 3 fibrous bundle, and Fig. 4 is test 3 fibrous bundle port microscopic appearance SEM image.
Embodiment
Embodiment one: the preparation method of present embodiment Graphene modifying carbon/carbon composite material, carry out according to the following steps:
One, carbon fabric perform is immersed in the N-Methyl pyrrolidone solution of Graphene, supersound process, then carbon fabric perform taking-up is put in baking oven, in 150 DEG C of oven dry;
Two, first with pitch/N-Methyl pyrrolidone solution, precast body is flooded, carry out supersound process simultaneously, then precast body is taken out and be put in baking oven, in 120 DEG C of oven dry;
Three, repeating step 22 ~ 3 times, by asphalt heating to 260 DEG C ~ 280 DEG C, then immerse in pitch by the precast body processed, normal pressure floods, and then takes out;
Four, the precast body after bituminizing is placed in the carbide furnace under 0.1MPa argon shield, is warming up to 400 DEG C, keep temperature 2h, be then raised to 800 DEG C, keep temperature 2h, finally temperature is raised to 1200 DEG C, insulation 2h, then lower the temperature, treat that furnace temperature is down to room temperature, take out the sample after carbonization;
Five, repeating step two to step 44 times, then puts into carbide furnace by sample, under 0.1MPa argon shield, is warming up to 1900 DEG C, keeps temperature 1h, and cooling, treats the near room temperature of furnace temperature, takes out sample, i.e. the carbon/carbon compound material of obtained Graphene modification.
The N-Methyl pyrrolidone solution of Graphene take Graphene as solute, and N-Methyl pyrrolidone is the solution that solvent is made.
Embodiment two: present embodiment and embodiment one unlike: in step one, the concentration of the N-Methyl pyrrolidone solution of Graphene is 0.05 ~ 0.5mg/mL.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment two unlike: in step one, the concentration of the N-Methyl pyrrolidone solution of Graphene is 0.1mg/mL.Other is identical with embodiment two.
Embodiment four: one of present embodiment and embodiment one to three unlike: in step one, the time of supersound process is 1 ~ 1.5h.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the concentration of step 2 medium pitch/N-Methyl pyrrolidone solution is 0.1mg/mL.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: in step 2, the time of supersound process is 20 ~ 30min.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: by asphalt heating to 270 DEG C in step 3.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: in step 3, dipping time is 2 ~ 2.5h.Other is identical with one of embodiment one to seven.
By following verification experimental verification beneficial effect of the present invention:
Test 1:
The preparation method of this test Graphene modifying carbon/carbon composite material, carries out according to the following steps:
One, compound concentration is the N-Methyl pyrrolidone solution of 0.01mg/mL Graphene, is immersed in by carbon fabric perform in the N-Methyl pyrrolidone solution of Graphene, supersound process 1h, then is put in baking oven, in 150 DEG C of oven dry by carbon fabric perform taking-up;
Two, first with the pitch of 0.1mg/mL/N-Methyl pyrrolidone solution, precast body is flooded, carry out supersound process 30min simultaneously, then precast body is taken out and be put in baking oven, in 120 DEG C of oven dry;
Three, repeating step 23 times, by asphalt heating to 270 DEG C, then immerses in pitch by the precast body processed, and normal pressure dipping 2h, then takes out;
Four, the precast body after bituminizing is placed in the carbide furnace under 0.1MPa argon shield, is warming up to 400 DEG C, keep temperature 2h, be then raised to 800 DEG C, keep temperature 2h, finally temperature is raised to 1200 DEG C, insulation 2h, then lower the temperature, treat that furnace temperature is down to room temperature, take out the sample after carbonization;
Five, repeating step two to step 44 times, then puts into carbide furnace by sample, under 0.1MPa argon shield, is warming up to 1900 DEG C, keeps temperature 1h, and cooling, treats the near room temperature of furnace temperature, takes out sample, i.e. the carbon/carbon compound material of obtained Graphene modification.
Test 2:
With the difference of test 1, the preparation method of this test Graphene modifying carbon/carbon composite material is only that the concentration of the N-Methyl pyrrolidone solution of Graphene is 0.05mg/mL.
Test 3:
With the difference of test 1, the preparation method of this test Graphene modifying carbon/carbon composite material is only that the concentration of the N-Methyl pyrrolidone solution of Graphene is 0.1mg/mL.
Test 4:
With the difference of test 1, the preparation method of this test Graphene modifying carbon/carbon composite material is only that the concentration of the N-Methyl pyrrolidone solution of Graphene is 0.5mg/mL.
The degree of graphitization of modifying carbon/carbon composite material obtained in test 1-4 is as shown in table 1.
The degree of graphitization of the coating modified carbon/carbon compound material of table 1 different concns graphene solution
| Graphene concentration (mg/mL) | 0 | 0.01 | 0.05 | 0.10 | 0.50 |
| Degree of graphitization (%) | 77.35 | 80.13 | 83.04 | 86.46 | 90.56 |
Learn from the result of table 1, the degree of graphitization of carbon/carbon compound material raises along with the continuous increase of graphite strength of solution, finally reaches 90.56%.Along with the increase of Graphene content, carbon (002) spacing d in carbon/carbon compound material
002interlamellar spacing progressively reduces, and degree of graphitization increases, and illustrates that the stack manner of graphite aspect progressively trends towards ordering.
The flexural strength of modifying carbon/carbon composite material obtained in test 1-4 as shown in Figure 1.
Learn from the result of Fig. 1, the carbon/carbon compound material flexural strength of Graphene modification first increases rear reduction along with the increase of Graphene concentration.Reach maximum when 0.05mg/ml, flexural strength reaches 234.21MPa, raising 25.5% compared with the material without Graphene modification.As can be seen from Figure 1, improving Graphene concentration can't make the flexural strength of carbon-carbon composite improve always simultaneously.
Fibrous bundle/basal body interface the average shear strength of modifying carbon/carbon composite material obtained in test 1-4 as shown in Figure 2.As can see from Figure 2, the interface average shear strength of fibrous bundle is between 10-12.5MPa.Non-modified, its interface average shear strength is the most weak, is about 10.07MPa.Along with the continuous increase of Graphene concentration, part Graphene has filled up the hole of fibrous bundle/basal body interface, induction matrix carbon is to greying future development, and therefore interface average shear strength constantly increases, until reach maximum value 12.50MPa when Graphene modifier concentration reaches 0.1mg/ml.And when Graphene interface modification concentration reaches 0.5mg/mL, the average shear strength at interface presents downtrending, and this mainly have impact on bituminizing to a certain extent cause the hole that a part is new to produce because the excessive Graphene of concentration forms block small-particle at fiber surface.Can reach a conclusion thus, the solution modification concentration of Graphene interface modification carbon/carbon compound material can not increase simply, and need control also can not affect within bitumen-impregnated scope can either fill up interface void.
The interface SEM testing carbon fiber and matrix in 3 fibrous bundles schemes as shown in Figure 3, tests 3 fibrous bundle port microscopic appearance SEM images as shown in Figure 4.Carbon fiber is be uniformly distributed in the composite substantially as can be seen from Fig., and has good interface cohesion between fiber and matrix, does not form obvious hole and defect and then makes material property degradation.
Claims (8)
1. a preparation method for Graphene modifying carbon/carbon composite material, is characterized in that the method is carried out according to the following steps:
One, carbon fabric perform is immersed in the N-Methyl pyrrolidone solution of Graphene, supersound process, then carbon fabric perform taking-up is put in baking oven, in 150 DEG C of oven dry;
Two, first with pitch/N-Methyl pyrrolidone solution, precast body is flooded, carry out supersound process simultaneously, then precast body is taken out and be put in baking oven, in 120 DEG C of oven dry;
Three, repeating step 22 ~ 3 times, by asphalt heating to 260 DEG C ~ 280 DEG C, then immerse in pitch by the precast body processed, normal pressure floods, and then takes out;
Four, the precast body after bituminizing is placed in the carbide furnace under 0.1MPa argon shield, is warming up to 400 DEG C, keep temperature 2h, be then raised to 800 DEG C, keep temperature 2h, finally temperature is raised to 1200 DEG C, insulation 2h, then lower the temperature, treat that furnace temperature is down to room temperature, take out the sample after carbonization;
Five, repeating step two to step 44 times, then puts into carbide furnace by sample, under 0.1MPa argon shield, is warming up to 1900 DEG C, keeps temperature 1h, and cooling, treats the near room temperature of furnace temperature, takes out sample, i.e. the carbon/carbon compound material of obtained Graphene modification.
2. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1, is characterized in that the concentration of the N-Methyl pyrrolidone solution of Graphene in step one is 0.05 ~ 0.5mg/mL.
3. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 2, is characterized in that the concentration of the N-Methyl pyrrolidone solution of Graphene in step one is 0.1mg/mL.
4. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1 and 2, is characterized in that the time of supersound process in step one is 1 ~ 1.5h.
5. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1 and 2, is characterized in that the concentration of step 2 medium pitch/N-Methyl pyrrolidone solution is 0.1mg/mL.
6. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1 and 2, is characterized in that the time of supersound process in step 2 is 20 ~ 30min.
7. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1 and 2, is characterized in that asphalt heating to 270 DEG C in step 3.
8. the preparation method of a kind of Graphene modifying carbon/carbon composite material according to claim 1 and 2, is characterized in that in step 3, dipping time is 2 ~ 2.5h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110809A (en) * | 2015-08-18 | 2015-12-02 | 河南泛锐复合材料研究院有限公司 | Preparation method for graphene-modified high thermal conductivity three-dimensional carbon/carbon composite material |
| CN105152674A (en) * | 2015-08-18 | 2015-12-16 | 河南泛锐复合材料研究院有限公司 | Preparation method of pantograph slide plate made of graphene modified carbon/carbon composite material |
| CN105235529A (en) * | 2015-10-22 | 2016-01-13 | 苏州泛珉复合材料科技有限公司 | Preparation method for pantograph slide plate made of graphene-copper modified carbon/carbon composite material |
| CN105421084A (en) * | 2015-12-04 | 2016-03-23 | 镇江奥立特机械制造有限公司 | Novel fiber liquid-immersing method |
| CN105948014A (en) * | 2016-04-27 | 2016-09-21 | 山东前昊炭素有限公司 | Coke/sulfonated graphene carbon-graphite material for sealing piece and preparation method thereof |
| CN108947557A (en) * | 2018-09-25 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of carbon/carbon compound material and preparation method thereof |
| CN109734468A (en) * | 2019-02-26 | 2019-05-10 | 航天材料及工艺研究所 | A kind of graphene paper enhancing carbon/carbon compound material and preparation method thereof |
| CN115710134A (en) * | 2022-11-25 | 2023-02-24 | 航天特种材料及工艺技术研究所 | Interface modified ceramic matrix composite and preparation method thereof |
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2014
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| 牟辰中: "石墨烯涂层对碳/碳复合材料的界面改性研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 6, 15 June 2014 (2014-06-15) * |
Cited By (11)
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| CN105110809A (en) * | 2015-08-18 | 2015-12-02 | 河南泛锐复合材料研究院有限公司 | Preparation method for graphene-modified high thermal conductivity three-dimensional carbon/carbon composite material |
| CN105152674A (en) * | 2015-08-18 | 2015-12-16 | 河南泛锐复合材料研究院有限公司 | Preparation method of pantograph slide plate made of graphene modified carbon/carbon composite material |
| CN105235529A (en) * | 2015-10-22 | 2016-01-13 | 苏州泛珉复合材料科技有限公司 | Preparation method for pantograph slide plate made of graphene-copper modified carbon/carbon composite material |
| CN105235529B (en) * | 2015-10-22 | 2017-09-01 | 巩义市泛锐熠辉复合材料有限公司 | Graphene copper is modified the preparation method of carbon/carbon composite pantograph pan |
| CN105421084A (en) * | 2015-12-04 | 2016-03-23 | 镇江奥立特机械制造有限公司 | Novel fiber liquid-immersing method |
| CN105948014A (en) * | 2016-04-27 | 2016-09-21 | 山东前昊炭素有限公司 | Coke/sulfonated graphene carbon-graphite material for sealing piece and preparation method thereof |
| CN105948014B (en) * | 2016-04-27 | 2018-01-23 | 山东恒煜石墨科技有限公司 | Seal coke/sulfonated graphene carbon graphite material and preparation method thereof |
| CN108947557A (en) * | 2018-09-25 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of carbon/carbon compound material and preparation method thereof |
| CN108947557B (en) * | 2018-09-25 | 2021-05-14 | 航天特种材料及工艺技术研究所 | Carbon/carbon composite material and preparation method thereof |
| CN109734468A (en) * | 2019-02-26 | 2019-05-10 | 航天材料及工艺研究所 | A kind of graphene paper enhancing carbon/carbon compound material and preparation method thereof |
| CN115710134A (en) * | 2022-11-25 | 2023-02-24 | 航天特种材料及工艺技术研究所 | Interface modified ceramic matrix composite and preparation method thereof |
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