CN102924736A - Preparation of carbon fiber/ carbon nano tube/ epoxy resin composite material and assisted by freezing and drying - Google Patents
Preparation of carbon fiber/ carbon nano tube/ epoxy resin composite material and assisted by freezing and drying Download PDFInfo
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- CN102924736A CN102924736A CN2012104245418A CN201210424541A CN102924736A CN 102924736 A CN102924736 A CN 102924736A CN 2012104245418 A CN2012104245418 A CN 2012104245418A CN 201210424541 A CN201210424541 A CN 201210424541A CN 102924736 A CN102924736 A CN 102924736A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 107
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 107
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 87
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 87
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 37
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000007710 freezing Methods 0.000 title description 8
- 230000008014 freezing Effects 0.000 title description 8
- 238000001035 drying Methods 0.000 title description 3
- 238000002360 preparation method Methods 0.000 title description 3
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000805 composite resin Substances 0.000 claims abstract 4
- 239000004593 Epoxy Substances 0.000 claims description 19
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 11
- 238000007669 thermal treatment Methods 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 229920002430 Fibre-reinforced plastic Polymers 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- -1 glycidyl ester Chemical class 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 3
- 235000013824 polyphenols Nutrition 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000006735 epoxidation reaction Methods 0.000 claims description 2
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 13
- 238000004108 freeze drying Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000009417 prefabrication Methods 0.000 abstract 2
- 239000007900 aqueous suspension Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 9
- 241000446313 Lamella Species 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000004402 polyphenol group Chemical group 0.000 description 1
- 241000894007 species Species 0.000 description 1
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Abstract
本发明公开了一种冷冻干燥辅助制备碳纤维/碳纳米管/环氧树脂复合材料的方法。工艺为：先向碳纳米管水系悬浮液中添加去离子水予以稀释，得到碳纳米管水溶液；再将碳纤维样条浸渍到该水溶液中并抽真空；随后进行冷冻干燥处理，得到碳纤维/碳纳米管预制体；再将预制体于Ar气、500℃下处理30min～60min，充分浸渍液态树脂并固化，即可制得碳纤维/碳纳米管/树脂复合材料。本发明工艺简单、能耗较低，并且使碳纳米管在复合材料中具有更好的分布形态，进一步改善了复合材料的性能。
The invention discloses a method for preparing carbon fiber/carbon nanotube/epoxy resin composite material aided by freeze-drying. The process is as follows: first add deionized water to the carbon nanotube aqueous suspension to dilute to obtain a carbon nanotube aqueous solution; then impregnate the carbon fiber sample into the aqueous solution and vacuumize; then perform freeze-drying treatment to obtain carbon fiber/carbon nanotube Tube prefabrication; then treat the prefabrication in Ar gas at 500°C for 30min to 60min, fully impregnate the liquid resin and solidify, and then the carbon fiber/carbon nanotube/resin composite material can be obtained. The invention has simple process, low energy consumption, better distribution form of carbon nanotubes in the composite material, and further improves the performance of the composite material.
Description
Technical field
The invention relates to epoxy resin-base composite material preparation, particularly a kind of auxiliary method for preparing carbon fiber/carbon nano tube/epoxy resin composite material of Freeze Drying Technique of utilizing.
Background technology
It is better that Resins, epoxy has mechanical property, the base materials such as metal, pottery, concrete had stronger sticking power, cure shrinkage is little, be easy to control moulding, electrical insulating property is good, and to acid, caustic corrosion is insensitive, and satisfy the advantages such as usually temperature service requirements (thermotolerance of Resins, epoxy is generally 80 ℃ ~ 100 ℃, and the thermotolerance of individual species can reach more than 200 ℃).By the epoxy resin composite material that carbon fiber and carbon nanotube improve, its performance, especially mechanical property are greatly improved; In addition, the character of the aspects such as the special electricity that has based on carbon fiber, carbon nanotube self, heat, sound, light, carbon fiber/carbon nano tube/epoxy resin composite material has also possessed some new characteristics that are different from Resins, epoxy itself, and is expected to be widely used in the fields such as space flight and aviation, traffic and sports equipment.
Lyophilize claims that again liter change is dry.Refer under high vacuum state, it is the water vapour of gaseous state that the moisture in the material is directly distilled by solid-state ice, to reach the purpose of dried material.Concrete technical process comprises freezing and dry two portions, namely is being lower than under 0 ℃ the temperature water-containing materials freezing so that liquid water wherein is frozen into ice fully first, again material is carried out drying on lyophilizer.Its most significant advantage is: freezing dry process can make the particle in the material be fixed up by original position, has kept the original microscopic pattern of material (such as vesicular structure).
Summary of the invention
Purpose of the present invention, to prepare comparatively complexity of carbon fiber/carbon nano tube/epoxy resin composite material technique for prior art, and be difficult to can so that carbon nanotube can be dispersed in preferably on the interface between Resins, epoxy/carbon fiber (playing the effect that strengthens interface bond strength), can be distributed in preferably again simultaneously the deficiency that (in matrix, hinders dislocation moving and crack propagation) in the resin matrix, provide a kind of both technique simple, can significantly optimize again the distribution of carbon nanotube in matrix material so that it brings into play the carbon fiber/carbon nano tube/epoxy resin composite material of its own advantages better.
The present invention utilizes the auxiliary method for preparing carbon fiber/carbon nano tube/epoxy resin composite material of Freeze Drying Technique, has following steps:
(1) weighing carbon nanotube water system suspension is diluted to wherein adding deionized water, and stirring obtains carbon nano-tube aqueous solutions; Wherein, the mass ratio of the quality of the deionized water of interpolation and carbon nanotube water system suspension is 0:1 ~ 10:1;
(2) the carbon fiber batten is impregnated in the carbon nano-tube aqueous solutions that obtains in the step (1), and vacuumizes;
(3) the carbon fiber batten behind the dipping carbon nano-tube aqueous solutions that step (2) is obtained carries out lyophilize at lyophilizer subsequently in being frozen into solid-state block below 0 ℃, obtains carbon fiber/carbon nanotube precast body;
(4) carbon fiber that step (3) is obtained/carbon nanotube precast body is in Ar gas, 500 ℃ of lower thermal treatment 30min～60min; Then in carbon fiber/carbon nanotube precast body, introduce Resins, epoxy by the VARTM method, and solidify, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
The carbon nanotube water system suspension of described step (1) is carbon nanotube aqueous slurry or carbon nanotube aqueous dispersion.
The carbon fiber batten of described step (2) is any one in the unidirectional polyacrylonitrile carbon fiber bundle polyacrylonitrile carbon fiber cloth of arranging the carbon cloth that forms, two dimension, the three-dimensional polyacrylonitrile carbon fiber knitted body.
The resin of described step (4) is any one in bisphenol A type epoxy resin, bisphenol f type epoxy resin, polyphenol type tetraglycidel ether epoxy resin, aliphatic glycidyl ether Resins, epoxy, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, the epoxidation of olefins compound.
The invention has the beneficial effects as follows, with respect to the method for preparing fiber/carbon nano tube/epoxy resin composite material commonly used at present, technical process of the present invention is simple, energy consumption is lower, the more important thing is and make carbon nanotube at the interface with in the resin matrix preferably distribution arranged all, reach the effect of optimizing carbon nanotube distribution in matrix material, be conducive to obtain the more excellent material of performance.
Description of drawings
Fig. 1 is the SEM image of the carbon fiber that lyophilize obtains in the embodiment of the invention 1/carbon nanotube precast body;
Fig. 2 is the SEM image after carbon fiber/the carbon nanotube precast body is heat-treated that in the embodiment of the invention 1 lyophilize is obtained;
Fig. 3 is the carbon fiber that makes in the embodiment of the invention 1/carbon nano tube/epoxy resin composite material photo.
Embodiment
Below in conjunction with specific embodiment the present invention is done further specific description.
Employed carbon nanotube water system suspension is the carbon nanotube aqueous slurry (massfraction of carbon nanotube is 5%, and the dispersion agent that uses is PVP) that Nanometer Port Co., Ltd., Shenzhen produces in following examples.
Embodiment 1
The used resin of the present embodiment is bisphenol A type epoxy resin (model is the D.E.R.*332 that Dow Chemical company produces), and solidifying agent is the D.E.H.*39 that the said firm produces, and the two mass ratio is 4:1.
(1) weighing 10g carbon nanotube water system suspension, and obtain carbon nano-tube aqueous solutions to wherein adding in the 50g deionized water, stirring;
(2) will shear the good 3 D weaving carbon fiber batten with regular shape and immerse in the above-mentioned aqueous solution, and vacuumize 5min;
(3) the carbon fiber batten that step (2) is exhausted after the vacuum, is soaked with carbon nano-tube aqueous solutions in refrigerator-freezer ,-19 ℃ of lower freezing 24h; With its lyophilize 24h on lyophilizer, obtain carbon fiber/carbon nanotube precast body subsequently;
(4) with carbon fiber/carbon nanotube precast body in Ar gas, behind 500 ℃ of lower thermal treatment 45min, method by VARTM is introduced Resins, epoxy (having added solidifying agent) in carbon fiber/carbon nanotube precast body, and in 60 ℃ of lower 4h that solidify, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
The SEM image of the carbon fiber that lyophilize obtains among the embodiment 1/carbon nanotube precast body, the SEM image after carbon fiber/the carbon nanotube precast body is heat-treated that lyophilize is obtained and the carbon fiber that finally obtains/carbon nano tube/epoxy resin composite material batten photo is respectively such as Fig. 1, Fig. 2, shown in Figure 3.Be not difficult to find out from Fig. 1, in the carbon fiber that lyophilize obtains/carbon nanotube precast body, the carbon nanotube lamella not only is wrapped in carbon fiber surface preferably, and also there is distribution (such as arrow indication among the figure) in the zone between carbon fiber.Through Overheating Treatment (Fig. 2), PVP in the carbon nanotube lamella is removed, final so that between the carbon fiber of some close together, form the net of carbon nanotube overlap joint, according to existing research, we can infer, after introducing Resins, epoxy, these carbon nanotubes will mainly be distributed in the epoxy resin-base; Simultaneously, owing to also having adhered to some carbon nanotubes (Fig. 2) at carbon fiber surface, these carbon nanotubes mainly are distributed on the interface of Resins, epoxy/carbon fiber after introducing Resins, epoxy.This shows, utilize the auxiliary method for preparing carbon fiber/carbon nano tube/epoxy resin composite material of lyophilize, can reach and make carbon nanotube be distributed in simultaneously effect in Resins, epoxy/carbon fiber interface and the epoxy resin-base.
Embodiment 2
The used resin of the present embodiment is bisphenol A type epoxy resin (model is the D.E.R.*332 that Dow Chemical company produces), and solidifying agent is the D.E.H.*39 that the said firm produces, and the two mass ratio is 4:1.
(1) weighing 20g carbon nanotube water system suspension, and obtain carbon nano-tube aqueous solutions to wherein adding in the 20g deionized water, stirring;
(2) will shear the good 3 D weaving carbon fiber batten with regular shape and immerse in the mentioned solution, and vacuumize 10min;
(3) the carbon fiber batten that step (2) is exhausted after the vacuum, is soaked with carbon nano-tube aqueous solutions in refrigerator-freezer ,-19 ℃ of lower freezing 24h; With its lyophilize 24h on lyophilizer, obtain carbon fiber/carbon nanotube precast body subsequently;
(4) with carbon fiber/carbon nanotube precast body in Ar gas, behind 500 ℃ of lower thermal treatment 45min, method by VARTM is introduced Resins, epoxy (having added solidifying agent) in carbon fiber/carbon nanotube precast body, and in 60 ℃ of lower 4h that solidify, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
Contain more carbon nanotube lamella in the carbon fiber that lyophilize obtains/carbon nanotube precast body, and these lamellas not only are wrapped in carbon fiber surface, distribution is also arranged in the hole between carbon fiber; After the thermal treatment, the changes in distribution of carbon nanotube is very little; In the carbon fiber/carbon nano tube/epoxy resin composite material that finally obtains, the massfraction of carbon nanotube is with respect to increasing to some extent among the embodiment 1.
Embodiment 3
The used resin of the present embodiment is bisphenol A type epoxy resin (model is the D.E.R.*332 that Dow Chemical company produces), and solidifying agent is the D.E.H.*39 that the said firm produces, and the two mass ratio is 4:1.
(1) weighing 10g carbon nanotube water system suspension, and obtain carbon nano-tube aqueous solutions to wherein adding in the 50g deionized water, stirring;
(2) carbon cloth (the T700 fiber that toray company produces) with unidirectional array immerses in the mentioned solution, and vacuumizes 5min;
(3) unidirectional lamination that step (2) is exhausted after the vacuum, is soaked with carbon nano-tube aqueous solutions in refrigerator-freezer ,-19 ℃ of lower freezing 24h; With its lyophilize 24h on lyophilizer, obtain carbon fiber/carbon nanotube precast body subsequently;
(4) with carbon fiber/carbon nanotube precast body in Ar gas, behind 500 ℃ of lower thermal treatment 45min, method by VARTM is introduced Resins, epoxy (having added solidifying agent) in carbon fiber/carbon nanotube precast body, and in 60 ℃ of lower 4h that solidify, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
The carbon nanotube lamella that forms in the carbon fiber that lyophilize obtains/carbon nanotube precast body not only is wrapped in carbon fiber surface, and distribution is also arranged in the hole between carbon fiber; After the thermal treatment, the changes in distribution of carbon nanotube is very little; Determined by carbon cloth, the carbon fiber/carbon nano tube/epoxy resin composite material that finally obtains is the tabular sample, and carbon fiber becomes unidirectional distribution.
Embodiment 4
The used resin of the present embodiment is polyphenol type tetraglycidel ether epoxy resin (model is the still SK-0430 that produces of section's speciality polymer Materials Co., Ltd of Changzhou), and solidifying agent is the DDS that the said firm produces, and the two mass ratio is 5:2.
(1) weighing 10g carbon nanotube water system suspension, and obtain carbon nano-tube aqueous solutions to wherein adding in the 50g deionized water, stirring;
(2) will shear in the carbon cloth immersion mentioned solution of good control of two-dimensional braided, and vacuumize 5min;
(3) the carbon fiber batten that step (2) is exhausted after the vacuum, is soaked with carbon nano-tube aqueous solutions in refrigerator-freezer ,-19 ℃ of lower freezing 24h; With its lyophilize 24h on lyophilizer, obtain carbon fiber/carbon nanotube precast body subsequently;
(4) with carbon fiber/carbon nanotube precast body in Ar gas, behind 500 ℃ of lower thermal treatment 30min, in carbon fiber/carbon nanotube precast body, introduce Resins, epoxy (having added solidifying agent) by the VARTM method, and according to: finish curing under 120 ℃ 1h+160 ℃ 4h+200 ℃ of 4h condition, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
The carbon nanotube lamella that forms in the carbon fiber that lyophilize obtains/carbon nanotube precast body not only is wrapped in carbon fiber surface, and distribution is also arranged in the hole between carbon fiber; After the thermal treatment, the changes in distribution of carbon nanotube is very little; Determined by carbon cloth, the carbon fiber/carbon nano tube/epoxy resin composite material that finally obtains is the tabular sample, and carbon fiber is only becoming bivariate distribution in the plane.
Above-mentioned description to embodiment is to be convenient to those skilled in the art can understand and apply the invention.The person skilled in the art easily makes various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of raw material, interval value can both realize the present invention, and this is not illustrated one by one again.
Claims (4)
1. the method for preparing carbon fiber/carbon nano tube/epoxy resin composite material is assisted in a lyophilize, has following steps:
(1) weighing carbon nanotube water system suspension is diluted to wherein adding deionized water, and stirring obtains carbon nano-tube aqueous solutions; Wherein, the mass ratio of the quality of the deionized water of interpolation and carbon nanotube water system suspension is 0:1 ~ 10:1;
(2) the carbon fiber batten is impregnated in the carbon nano-tube aqueous solutions that obtains in the step (1), and vacuumizes;
(3) the carbon fiber batten behind the dipping carbon nano-tube aqueous solutions that step (2) is obtained carries out lyophilize at lyophilizer subsequently in being frozen into solid-state block below 0 ℃, obtains carbon fiber/carbon nanotube precast body;
(4) carbon fiber that step (3) is obtained/carbon nanotube precast body is in Ar gas, 500 ℃ of lower thermal treatment 30min～60min; Then in carbon fiber/carbon nanotube precast body, introduce Resins, epoxy by the VARTM method, and solidify, can obtain carbon fiber/carbon nano tube/epoxy resin composite material.
2. according to claim 1 the auxiliary method for preparing carbon fiber/carbon nanotube/resin composite materials of lyophilize is characterized in that, the carbon nanotube water system suspension of described step (1) is carbon nanotube aqueous slurry or carbon nanotube aqueous dispersion.
3. according to claim 1 the auxiliary method for preparing carbon fiber/carbon nanotube/resin composite materials of lyophilize, it is characterized in that, the carbon fiber batten of described step (2) is any one in the unidirectional polyacrylonitrile carbon fiber bundle polyacrylonitrile carbon fiber cloth of arranging the carbon cloth that forms, two dimension, the three-dimensional polyacrylonitrile carbon fiber knitted body.
4. according to claim 1 the auxiliary method for preparing carbon fiber/carbon nanotube/resin composite materials of lyophilize, it is characterized in that, the resin of described step (4) is any one in bisphenol A type epoxy resin, bisphenol f type epoxy resin, polyphenol type tetraglycidel ether epoxy resin, aliphatic glycidyl ether Resins, epoxy, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, the epoxidation of olefins compound.
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Cited By (16)
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| CN103275525A (en) * | 2013-05-28 | 2013-09-04 | 天津大学 | Preparation method of fiber/carbon nano tube conductive network for modifying polymers |
| CN103951455A (en) * | 2014-04-09 | 2014-07-30 | 天津大学 | Method for preparing dense carbon nanotube-fiber-precursor ceramic composite material with the assistance of freeze drying |
| CN104389167A (en) * | 2014-11-03 | 2015-03-04 | 哈尔滨工业大学 | Coating solution containing nanoparticles and application thereof |
| CN104558650A (en) * | 2014-12-17 | 2015-04-29 | 天津大学 | Preparation method of carbon nano-tube/chopped carbon fiber/epoxy resin composite material |
| CN105272330A (en) * | 2015-10-22 | 2016-01-27 | 苏州泛珉复合材料科技有限公司 | Method for quickly preparing carbon/carbon composite with high thermal conductivity |
| CN106149357A (en) * | 2015-03-27 | 2016-11-23 | 国家电网公司 | A kind of method of carbon fiber surface load CNT |
| CN106479112A (en) * | 2016-09-30 | 2017-03-08 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method of phenolic impregnated carbon ablating body material |
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| CN103275525A (en) * | 2013-05-28 | 2013-09-04 | 天津大学 | Preparation method of fiber/carbon nano tube conductive network for modifying polymers |
| CN103951455A (en) * | 2014-04-09 | 2014-07-30 | 天津大学 | Method for preparing dense carbon nanotube-fiber-precursor ceramic composite material with the assistance of freeze drying |
| CN103951455B (en) * | 2014-04-09 | 2015-07-15 | 天津大学 | Method for preparing dense carbon nanotube-fiber-precursor ceramic composite material with the assistance of freeze drying |
| CN104389167A (en) * | 2014-11-03 | 2015-03-04 | 哈尔滨工业大学 | Coating solution containing nanoparticles and application thereof |
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