CN102617982B - Carbon nanotube/nylon fiber modified epoxy resin composite material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 117
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 117
- 229920001778 nylon Polymers 0.000 title claims abstract description 105
- 239000002131 composite material Substances 0.000 title claims abstract description 91
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 80
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 80
- 239000004677 Nylon Substances 0.000 claims abstract description 78
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000012528 membrane Substances 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims description 47
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 36
- 229920002292 Nylon 6 Polymers 0.000 claims description 35
- 239000002048 multi walled nanotube Substances 0.000 claims description 22
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 18
- 235000019253 formic acid Nutrition 0.000 claims description 18
- 238000009987 spinning Methods 0.000 claims description 18
- 238000012986 modification Methods 0.000 claims description 16
- 230000004048 modification Effects 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 6
- 239000003504 photosensitizing agent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 11
- 230000007423 decrease Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明提供了一种碳纳米管/尼龙纤维改性环氧树脂复合材料，属于复合材料领域。The invention provides a carbon nanotube/nylon fiber modified epoxy resin composite material, which belongs to the field of composite materials.
背景内容background content
环氧树脂具有优异的电气绝缘性能、化学稳定性、良好的粘结性能和简单的加工成型工艺，被广泛用于电子、汽车以及航空航天等领域。随着现代电气、电子工业的发展，尤其是电子封装材料的变化发展，环氧树脂已占整个封装材料的90％以上，因此近年来，环氧树脂复合材料的研究与制备成为电子封装行业的热点。随着电子元器件的小型化、集成化发展使得热量剧增，对封装材料提出了更高的耐热要求，以保证电气、电子产品的寿命及可靠性。然而，环氧树脂存在固化后耐冲击损伤能力差，韧性差及耐热性能较低等缺陷，此外其导热能力也有待提高。因此单一环氧树脂已很难满足高要求，必须另辟蹊径发展新型复合材料，环氧树脂材料将向复合化方向发展。目前对环氧树脂的改性主要是将橡胶弹性体、热塑性树脂或液晶聚合物、刚性颗粒等分散相加入树脂基体，再进行物理共混。填料的填充量、形状、几何尺寸及堆积方式、填料/树脂两相间的界面相容性等都会影响环氧树脂的整体性质。尤其是填料在基体中很容易聚集成团，导致复合材料的力学性能及耐热性能均有所下降，这些问题急待解决。Epoxy resin has excellent electrical insulation performance, chemical stability, good bonding performance and simple processing and molding process, and is widely used in the fields of electronics, automobiles and aerospace. With the development of modern electrical and electronic industries, especially the change and development of electronic packaging materials, epoxy resin has accounted for more than 90% of the entire packaging materials. Therefore, in recent years, the research and preparation of epoxy resin composite materials has become the focus of the electronic packaging industry hotspot. With the development of miniaturization and integration of electronic components, the heat increases sharply, and higher heat resistance requirements are put forward for packaging materials to ensure the life and reliability of electrical and electronic products. However, epoxy resin has defects such as poor resistance to impact damage after curing, poor toughness and low heat resistance, and its thermal conductivity needs to be improved. Therefore, it is difficult for a single epoxy resin to meet the high requirements, and it is necessary to find another way to develop new composite materials, and epoxy resin materials will develop in the direction of composite. At present, the modification of epoxy resin is mainly to add dispersed phases such as rubber elastomer, thermoplastic resin or liquid crystal polymer, and rigid particles into the resin matrix, and then perform physical blending. The filling amount, shape, geometric size and stacking mode of the filler, the interfacial compatibility between the filler/resin and the like will all affect the overall properties of the epoxy resin. In particular, fillers are easy to aggregate into clusters in the matrix, resulting in a decline in the mechanical properties and heat resistance of the composite material. These problems need to be solved urgently.
发明内容 Contents of the invention
本发明提供了一种碳纳米管/尼龙纤维改性环氧树脂复合材料，解决了背景技术中的缺点，该复合材料柔韧性强，耐热性能和导热性均良好，同时还不会对环氧树脂的本身性能造成影响。The invention provides a carbon nanotube/nylon fiber modified epoxy resin composite material, which solves the shortcomings in the background technology. The composite material has strong flexibility, good heat resistance and thermal conductivity, and will not damage the environment at the same time The performance of the oxygen resin itself is affected.
实现本发明上述目的所采用的技术方案为：The technical scheme adopted to realize the above-mentioned purpose of the present invention is:
一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为1％～5％的碳纳米管/尼龙复合纤维膜以及质量分数为95％～99％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，碳纳米管/尼龙复合纤维膜均匀的分布于环氧树脂的内部，碳纳米管/尼龙复合纤维膜中碳纳米管的含量为0.5％～1.5％，尼龙包覆于碳纳米管上。A carbon nanotube/nylon fiber modified epoxy resin composite material, the composite material includes a carbon nanotube/nylon composite fiber film with a mass fraction of 1% to 5% and an epoxy resin with a mass fraction of 95% to 99% The carbon nanotube/nylon composite fiber film is the skeleton, the epoxy resin is the pouring material, the carbon nanotube/nylon composite fiber film is uniformly distributed in the epoxy resin, and the carbon nanotube/nylon composite fiber film The content of the carbon nanotube is 0.5%-1.5%, and the nylon is coated on the carbon nanotube.
所述的碳纳米管为多壁碳纳米管。所述的尼龙为尼龙6。所述的复合材料的断裂伸长率为15～25％，热分解温度为328～337℃。The carbon nanotubes are multi-walled carbon nanotubes. Described nylon is nylon 6. The elongation at break of the composite material is 15-25%, and the thermal decomposition temperature is 328-337°C.
本发明提供的碳纳米管/尼龙纤维改性环氧树脂复合材料中以碳纳米管和尼龙复合纤维膜作为骨架，以环氧树脂做为浇注材料。由于碳纳米管和尼龙复合纤维膜由电纺纤维组成，其纤维直径较小，一般在100nm至1um之间，且其直径分布均匀、比表面积大、孔隙率高，因此骨架能够均匀的分布在环氧树脂内部。同时又由于该复合材料的骨架为碳纳米管和尼龙纤维构成的三维网络结构，包覆在碳纳米管上的尼龙一方面起绝缘层作用屏蔽碳纳米管的导电能力；另一方面起界面层作用增加碳纳米管和环氧树脂之间的模量匹配程度，从而提高了该材料的柔韧性、耐热性和导热性，同时又不会对环氧树脂的原有电绝缘性、化学稳定性、力学性能以及粘结性能造成影响，其加工成型工艺简单，因而能够广泛的应用于电子、汽车以及航空航天等领域。In the carbon nanotube/nylon fiber modified epoxy resin composite material provided by the present invention, carbon nanotube and nylon composite fiber film are used as a skeleton, and epoxy resin is used as a pouring material. Since the carbon nanotube and nylon composite fiber membrane is composed of electrospun fibers, the fiber diameter is small, generally between 100nm and 1um, and its diameter distribution is uniform, the specific surface area is large, and the porosity is high, so the skeleton can be evenly distributed in the Epoxy interior. At the same time, because the skeleton of the composite material is a three-dimensional network structure composed of carbon nanotubes and nylon fibers, the nylon coated on the carbon nanotubes acts as an insulating layer to shield the conductivity of the carbon nanotubes; on the other hand, it acts as an interface layer. The effect increases the modulus matching between carbon nanotubes and epoxy resin, thereby improving the flexibility, heat resistance and thermal conductivity of the material, while not affecting the original electrical insulation and chemical stability of epoxy resin Sex, mechanical properties and bonding properties are affected, and its processing and molding process is simple, so it can be widely used in electronics, automobiles, aerospace and other fields.
具体实施方式 Detailed ways
下面结合具体实施例对本发明做详细具体的说明。The present invention will be described in detail below in conjunction with specific embodiments.
实施例1：一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为1％的碳纳米管/尼龙复合纤维膜以及质量分数为99％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，骨架均匀的分布于浇注材料的内部。碳纳米管/尼龙复合纤维膜中碳纳米管的含量为0.5％，尼龙包覆于碳纳米管上。本实施例中碳纳米管采用多壁碳纳米管，尼龙采用尼龙6。Embodiment 1: a kind of carbon nanotube/nylon fiber modified epoxy resin composite material, this composite material comprises the carbon nanotube/nylon composite fiber membrane that mass fraction is 1% and the epoxy resin that mass fraction is 99%; Wherein The carbon nanotube/nylon composite fiber film is the skeleton, the epoxy resin is the pouring material, and the skeleton is uniformly distributed inside the pouring material. The carbon nanotube content in the carbon nanotube/nylon composite fiber film is 0.5%, and the nylon is coated on the carbon nanotube. In this embodiment, the carbon nanotubes are multi-walled carbon nanotubes, and the nylon is nylon 6.
本实施例中提供的碳纳米管/尼龙纤维改性环氧树脂复合材料，其断裂伸长率为15.0％，拉伸强度为16.8MPa，热分解温度为328.7℃。而不含骨架的环氧树脂断裂伸长率为8.4％，拉伸强度为18.2MPa，热分解温度为322.6℃。相比而言，耐热性能得到提高，拉伸强度略有降低，但断裂伸长率增加79％。The carbon nanotube/nylon fiber modified epoxy resin composite material provided in this example has an elongation at break of 15.0%, a tensile strength of 16.8 MPa, and a thermal decomposition temperature of 328.7°C. The elongation at break of the epoxy resin without skeleton is 8.4%, the tensile strength is 18.2MPa, and the thermal decomposition temperature is 322.6°C. In contrast, heat resistance was improved with a slight decrease in tensile strength but a 79% increase in elongation at break.
本实施例中的碳纳米管/尼龙纤维改性环氧树脂复合材料采用以下方法制备：The carbon nanotube/nylon fiber modified epoxy resin composite material in this example is prepared by the following method:
(1)、采用甲酸溶液溶解尼龙6，制得尼龙6甲酸溶液；(1), adopt formic acid solution to dissolve nylon 6, make nylon 6 formic acid solution;
(2)、在制得的尼龙6甲酸溶液中按照一定的比例添加多臂碳纳米管，充分搅拌后，超声分散0.5小时，制得纺丝液；(2), in the prepared nylon 6 formic acid solution, add multi-armed carbon nanotubes according to a certain ratio, after fully stirring, ultrasonically disperse for 0.5 hours, and obtain spinning solution;
(3)、将纺丝液进行纺丝处理，制得多壁碳纳米管和尼龙6的混合纤维膜即骨架，将骨架裁剪成合适的尺寸，平铺放入定制的特殊模具中；(3) Spinning the spinning solution to make a mixed fiber membrane of multi-walled carbon nanotubes and nylon 6, that is, a skeleton, cutting the skeleton into a suitable size, and laying it in a custom-made special mold;
(4)、在环氧丙烯酸树脂中添加光敏剂，制得浇注材料；(4), add photosensitizer in epoxy acrylic resin, make pouring material;
(5)、在60℃的条件下，按照一定的比例将浇注材料均匀浇注在平铺的骨架上；(5) Under the condition of 60°C, pour the pouring material evenly on the tiled skeleton according to a certain proportion;
(6)、采用紫外灯照射40s固化后得到碳纳米管/尼龙纤维改性环氧树脂复合材料。(6) The carbon nanotube/nylon fiber modified epoxy resin composite material was obtained after being cured by ultraviolet lamp irradiation for 40 s.
实施例2：一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为3％的碳纳米管/尼龙复合纤维膜以及质量分数为97％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，骨架均匀的分布于浇注材料的内部。碳纳米管/尼龙复合纤维膜中碳纳米管的含量为1％，尼龙包覆于碳纳米管上。本实施例中碳纳米管采用多壁碳纳米管，尼龙采用尼龙6。Embodiment 2: a kind of carbon nanotube/nylon fiber modified epoxy resin composite material, this composite material comprises the carbon nanotube/nylon composite fiber membrane that mass fraction is 3% and the epoxy resin that mass fraction is 97%; Wherein The carbon nanotube/nylon composite fiber film is the skeleton, the epoxy resin is the pouring material, and the skeleton is uniformly distributed inside the pouring material. The carbon nanotube content in the carbon nanotube/nylon composite fiber film is 1%, and the nylon is coated on the carbon nanotube. In this embodiment, the carbon nanotubes are multi-walled carbon nanotubes, and the nylon is nylon 6.
本实施例中的碳纳米管/尼龙纤维改性环氧树脂复合材料的制备方法与实施例1相同。The preparation method of the carbon nanotube/nylon fiber modified epoxy resin composite material in this example is the same as that in Example 1.
本实施例中提供的碳纳米管/尼龙纤维改性环氧树脂复合材料，其断裂伸长率为24.2％，拉伸强度为17.9MPa，热分解温度为330.6℃。而不含骨架的环氧树脂断裂伸长率为8.4％，拉伸强度为18.2MPa，热分解温度为322.6℃。相比而言，耐热性能得到提高，拉伸强度略有降低，但断裂伸长率增加188％。The carbon nanotube/nylon fiber modified epoxy resin composite material provided in this example has an elongation at break of 24.2%, a tensile strength of 17.9 MPa, and a thermal decomposition temperature of 330.6°C. The elongation at break of the epoxy resin without skeleton is 8.4%, the tensile strength is 18.2MPa, and the thermal decomposition temperature is 322.6°C. In contrast, heat resistance was improved, tensile strength was slightly reduced, but elongation at break increased by 188%.
实施例3：Example 3:
一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为5％的碳纳米管/尼龙复合纤维膜以及质量分数为95％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，骨架均匀的分布于浇注材料的内部。碳纳米管/尼龙复合纤维膜中碳纳米管的含量为1.5％，尼龙包覆于碳纳米管上。本实施例中碳纳米管采用多壁碳纳米管，尼龙采用尼龙6。A carbon nanotube/nylon fiber modified epoxy resin composite material, the composite material comprises a carbon nanotube/nylon composite fiber film with a mass fraction of 5% and an epoxy resin with a mass fraction of 95%; wherein the carbon nanotube/nylon composite fiber film The nylon composite fiber membrane is the skeleton, the epoxy resin is the pouring material, and the skeleton is evenly distributed inside the pouring material. The carbon nanotube content in the carbon nanotube/nylon composite fiber film is 1.5%, and the nylon is coated on the carbon nanotube. In this embodiment, the carbon nanotubes are multi-walled carbon nanotubes, and the nylon is nylon 6.
本实施例中的碳纳米管/尼龙纤维改性环氧树脂复合材料的制备方法与实施例1相同。The preparation method of the carbon nanotube/nylon fiber modified epoxy resin composite material in this example is the same as that in Example 1.
本实施例中提供的碳纳米管/尼龙纤维改性环氧树脂复合材料，其断裂伸长率为19.0％，拉伸强度为16.2MPa，热分解温度为329.6℃。而不含骨架的环氧树脂断裂伸长率为8.4％，拉伸强度为18.2MPa，热分解温度为322.6℃。相比而言，耐热性能得到提高，拉伸强度略有降低，但断裂伸长率增加126％。The carbon nanotube/nylon fiber modified epoxy resin composite material provided in this example has an elongation at break of 19.0%, a tensile strength of 16.2 MPa, and a thermal decomposition temperature of 329.6°C. The elongation at break of the epoxy resin without skeleton is 8.4%, the tensile strength is 18.2MPa, and the thermal decomposition temperature is 322.6°C. In contrast, heat resistance was improved, tensile strength was slightly reduced, but elongation at break increased by 126%.
实施例4：Example 4:
一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为3％的碳纳米管/尼龙复合纤维膜以及质量分数为97％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，骨架均匀的分布于浇注材料的内部。碳纳米管/尼龙复合纤维膜中碳纳米管的含量为1.5％，尼龙包覆于碳纳米管上。本实施例中碳纳米管采用多壁碳纳米管，尼龙采用尼龙6。A carbon nanotube/nylon fiber modified epoxy resin composite material, the composite material comprising a carbon nanotube/nylon composite fiber film with a mass fraction of 3% and an epoxy resin with a mass fraction of 97%; wherein the carbon nanotube/nylon composite fiber film The nylon composite fiber membrane is the skeleton, the epoxy resin is the pouring material, and the skeleton is evenly distributed inside the pouring material. The carbon nanotube content in the carbon nanotube/nylon composite fiber film is 1.5%, and the nylon is coated on the carbon nanotube. In this embodiment, the carbon nanotubes are multi-walled carbon nanotubes, and the nylon is nylon 6.
本实施例中的碳纳米管/尼龙纤维改性环氧树脂复合材料的制备方法与实施例1相同。The preparation method of the carbon nanotube/nylon fiber modified epoxy resin composite material in this example is the same as that in Example 1.
本实施例中提供的碳纳米管/尼龙纤维改性环氧树脂复合材料，其断裂伸长率为25.0％，拉伸强度为17.6MPa，热分解温度为336.8℃。而不含骨架的环氧树脂断裂伸长率为8.4％，拉伸强度为18.2MPa，热分解温度为322.6℃。相比而言，耐热性能得到提高，拉伸强度略有降低，但断裂伸长率增加198％。The carbon nanotube/nylon fiber modified epoxy resin composite material provided in this example has an elongation at break of 25.0%, a tensile strength of 17.6 MPa, and a thermal decomposition temperature of 336.8°C. The elongation at break of the epoxy resin without skeleton is 8.4%, the tensile strength is 18.2MPa, and the thermal decomposition temperature is 322.6°C. In contrast, heat resistance was improved with a slight decrease in tensile strength but a 198% increase in elongation at break.
实施例5：Example 5:
一种碳纳米管/尼龙纤维改性环氧树脂复合材料，该复合材料包括质量分数为1％的碳纳米管/尼龙复合纤维膜以及质量分数为99％的环氧树脂；其中碳纳米管/尼龙复合纤维膜为骨架，环氧树脂为浇注材料，骨架均匀的分布于浇注材料的内部。碳纳米管/尼龙复合纤维膜中碳纳米管的含量为1％，尼龙包覆于碳纳米管上。本实施例中碳纳米管采用多壁碳纳米管，尼龙采用尼龙6。A carbon nanotube/nylon fiber modified epoxy resin composite material, the composite material includes a carbon nanotube/nylon composite fiber film with a mass fraction of 1% and an epoxy resin with a mass fraction of 99%; wherein the carbon nanotube/nylon composite fiber film is 99% by weight; The nylon composite fiber membrane is the skeleton, the epoxy resin is the pouring material, and the skeleton is evenly distributed inside the pouring material. The carbon nanotube content in the carbon nanotube/nylon composite fiber film is 1%, and the nylon is coated on the carbon nanotube. In this embodiment, the carbon nanotubes are multi-walled carbon nanotubes, and the nylon is nylon 6.
本实施例中的碳纳米管/尼龙纤维改性环氧树脂复合材料的制备方法与实施例1相同。The preparation method of the carbon nanotube/nylon fiber modified epoxy resin composite material in this example is the same as that in Example 1.
本实施例中提供的碳纳米管/尼龙纤维改性环氧树脂复合材料，其断裂伸长率为20.2％，拉伸强度为16.7MPa，热分解温度为332.0℃。而不含骨架的环氧树脂断裂伸长率为8.4％，拉伸强度为18.2MPa，热分解温度为322.6℃。相比而言，耐热性能得到提高，拉伸强度略有降低，但断裂伸长率增加140％。The carbon nanotube/nylon fiber modified epoxy resin composite material provided in this example has an elongation at break of 20.2%, a tensile strength of 16.7 MPa, and a thermal decomposition temperature of 332.0°C. The elongation at break of the epoxy resin without skeleton is 8.4%, the tensile strength is 18.2MPa, and the thermal decomposition temperature is 322.6°C. In contrast, heat resistance was improved with a slight decrease in tensile strength but a 140% increase in elongation at break.
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