CN113463395A - 一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法 - Google Patents
一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法 Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 150000001412 amines Chemical class 0.000 title claims abstract description 77
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 112
- 239000004917 carbon fiber Substances 0.000 claims abstract description 112
- 239000006185 dispersion Substances 0.000 claims abstract description 90
- 239000007788 liquid Substances 0.000 claims abstract description 78
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 40
- 239000012528 membrane Substances 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000002041 carbon nanotube Substances 0.000 claims description 19
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000004952 Polyamide Substances 0.000 claims description 10
- 229920002873 Polyethylenimine Polymers 0.000 claims description 10
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- 229920000736 dendritic polymer Polymers 0.000 claims description 10
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 10
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 10
- 229920000333 poly(propyleneimine) Polymers 0.000 claims description 10
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- 229920000877 Melamine resin Polymers 0.000 claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
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- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 3
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- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 26
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- MCHZKGNHFPNZDP-UHFFFAOYSA-N 2-aminoethane-1,1,1-triol;hydrochloride Chemical compound Cl.NCC(O)(O)O MCHZKGNHFPNZDP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000003822 epoxy resin Substances 0.000 description 1
- DLINORNFHVEIFE-UHFFFAOYSA-N hydrogen peroxide;zinc Chemical compound [Zn].OO DLINORNFHVEIFE-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法。该方法包括：对碳纤维进行去剂和硝酸氧化处理，然后配制一维纳米材料分散液和高分子胺类分散液，将碳纤维丝束均匀铺放在滤膜上，并在垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，采用真空抽滤法将一维纳米材料和高分子胺类分散液沉积在碳纤维丝束表面，后将碳纤维丝束翻转180°，同样采用真空抽滤法将一维纳米材料和高分子胺类分散液沉积在碳纤维丝束的另一面，得到种一维纳米材料/高分子胺类首尾交替排列改性的碳纤维。本发明的制备方法首次在碳纤维圆周表面构筑一维纳米材料和高分子胺类首尾交替排列的间隔结构，使复合材料界面粘结强度提高43.3％～110.5％。
Description
技术领域
本发明属于材料的表面与界面改性应用技术领域，具体涉及一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法。
背景技术
近些年，我国不断推崇节能减排政策，因此轻质高强的复合材料具有不可估量的发展潜力，是未来材料发展的重要方向。目前，碳纤维增强树脂基复合材料因其轻质、强度高、模量高、耐疲劳好、抗蠕变等优越性能，且其带来的节能减排长远效益是其他材料无法替代的，成为研究的热点，在空航天、交通运输、桥梁建筑、高压容器等领域有巨大的应用市场。碳纤维复合材料的力学性能与碳纤维和树脂基体的界面粘结强度紧密相关，但碳纤维表面的惰性、非极性、与树脂粘合度差等问题限制了其性能的发挥。
为增加碳纤维的表面能使其与基体树脂间更好的结合，国内外研究学者对于碳纤维表面修饰的研究非常多，但目前的方法存在效率低、反应条件苛刻、有机试剂污染、高成本等问题，与国家绿色节能减排的政策相矛盾。因此，寻找一种简便、绿色环保、高效、低成本的碳纤维表面改性方法以提高碳纤维树脂基复合材料的界面性能十分重要。
一维纳米材料，如碳纳米管、纳米纤维素、二氧化锌纳米线等具有优异的力学、热学和电学性能，被广泛用作增强体来修饰碳纤维以提高纤维与树脂的界面粘结强度，但纳米材料表面缺少活性官能团和易团聚的问题又限制了复合材料界面性能的提升。高分子胺类由于其分子结构中含有氨基官能团，可以与环氧树脂产生共价键连接以促进应力传递，弥补纳米材料表面确实活性官能团的弊端。因此，将一维纳米材料和高分子胺类相结合以提高复合材料界面粘结强度是一种可行的解决策略。
发明内容
本发明旨在提供一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，该方法可在碳纤维表面首尾交替排列一维纳米材料和高分子胺类，产生强弱搭配的化学和物理相互作用，使复合材料界面粘结强度提高。此外，该方法具有简便、绿色环保、高效和低成本的优点。
为实现上述目的，本发明采用的技术方案是：
1)将碳纤维丝束在丙酮溶液中冷凝回流，然后用去离子水清洗干净并真空干燥；
2)将步骤1)处理得到的碳纤维丝束在浓酸中处理后用去离子水清洗干净并在真空干燥；
3)将一维纳米材料分散在水或有机溶剂中，磁力搅拌使其分散均匀，得到质量分数为0.01％～5％的一维纳米材料分散液；
4)将高分子胺类分散在有机溶剂中，磁力搅拌使其分散均匀，得到质量分数为0.1％～5％的高分子胺类分散液；
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤一维纳米材料分散液，抽滤后移动模具使一维纳米材料和高分子胺首尾相接排列，然后再抽滤高分子胺类分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤一维纳米材料分散液，抽滤后移动模具使一维纳米材料和高分子胺首尾相接排列，然后再抽滤高分子胺类分散液，干燥后得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；
将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤高分子胺类分散液，抽滤后移动模具使高分子胺和一维纳米材料首尾相接排列，然后再抽滤一维纳米材料分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤高分子胺类分散液，抽滤后移动模具使高分子胺和一维纳米材料首尾相接排列，然后再抽滤一维纳米材料分散液，干燥后得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维。
所述步骤(1)的碳纤维为长碳纤维。
所述步骤1)的回流温度为80～100℃，回流时间为12～48h。
所述步骤2)的浓酸采用硝酸、硫酸或王水，浓酸处理温度为80～100℃，时间为3～8h。
所述步骤3)一维纳米材料长径比＞10，直径1～100nm的纳米纤维素、碳纳米管、氧化锌纳米线、二氧化钛纳米线或二氧化硅晶须。
所述步骤3)的磁力搅拌转速为200～1000rpm/min，时间为30～120min。
所述步骤4)的高分子胺类为聚醚胺、聚多巴胺、聚乙烯亚胺、聚丙烯亚胺、三聚氰胺、聚酰胺-胺型树枝状高分子、超支化聚酰胺或端氨基超支化聚合物。
所述步骤3)和4)的有机溶剂为丙酮、乙醇、四氢呋喃、二甲基甲酰胺、二氯甲烷、三羟甲基氨基甲烷盐酸盐缓冲液。
所述步骤4)的磁力搅拌转速为200～800rpm/min，时间为10～60min。
所述步骤5)的模具间隙与间隔距离均为50～500μm。
所述步骤5)真空抽滤按一维纳米材料分散液、高分子胺类分散液体积(ml):滤膜直径(cm)＝(0.1～8):1。
所述步骤1)、2)和5)的干燥温度为50～80℃，干燥时间为2～5h。
与现有技术相比，本发明具有以下有益的技术效果：(1)本发明首次成功地采用真空抽滤法在碳纤维圆周表面构筑一维纳米材料和高分子胺类首尾交替排列的间隔结构，利用一维纳米材料高长径比、大比表面积和优异的力学性能增加纤维与树脂的机械咬合作用，并起到阻碍裂纹扩展的作用；利用高分子胺类与树脂的共价键合作用，有利于应力在界面传递。此外，碳纤维表面首尾交替排列的一维纳米材料和高分子胺类可以产生强弱搭配的化学和物理相互作用，有利于复合材料界面强度和韧性的同时提高；(2)本发明的方法可根据需要进行材料和分布距离进行合理的调节和搭配，达到加工种类的多样性；(3)本发明的方法设备简单、反应条件温和、无毒、环保、低成本和高效；(4)本发明制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料相比未改性碳纤维增强环氧复合材料，使界面粘结强度提高43.3％～110.5％。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
实施例1：
1)将长碳纤维丝束在80℃的丙酮溶液中冷凝回流24h，后用去离子水清洗纤维并在真空干燥箱中60℃干燥3h。
2)将步骤1)处理得到的碳纤维丝束在硝酸中80℃处理4h，后用去离子水清洗纤维并在真空干燥箱中60℃干燥3h。
3)将长约5μm和直径3～5nm的碳纳米管分散在水溶液中，300rpm/min磁力搅拌30min使其分散均匀，得到质量分数为0.05％的碳纳米管分散液。
4)将聚醚胺分散在二甲基甲酰胺中，200rpm/min磁力搅拌10min使其分散均匀，得到质量分数为1％的聚醚胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置50μm等间隙等间隔的模具，真空抽滤碳纳米管分散液，抽滤后移动模具50μm使碳纳米管和聚醚胺首尾相接排列，然后再抽滤聚醚胺分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置50μm等间隙等间隔的模具，真空抽滤碳纳米管分散液，抽滤后移动模具使碳纳米管和聚醚胺首尾相接排列，然后再抽滤聚醚胺分散液；60℃干燥3h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中碳纳米管分散液、聚醚胺分散液体积(ml):滤膜直径(cm)＝0.5:1。
所制备的一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了70.1％。
实施例2：
1)将长碳纤维丝束在90℃的丙酮溶液中冷凝回流24h，后用去离子水清洗纤维并在真空干燥箱中50℃干燥5h。
2)将步骤1)处理得到的碳纤维丝束在硝酸中90℃处理6h，后用去离子水清洗纤维并在真空干燥箱中50℃干燥5h。
3)将长约5μm和直径3～5nm的碳纳米管分散在乙醇溶液中，500rpm/min磁力搅拌60min使其分散均匀，得到质量分数为2％的碳纳米管分散液。
4)将聚乙烯亚胺分散在二甲基甲酰胺中，300rpm/min磁力搅拌30min使其分散均匀，得到质量分数为2％的聚乙烯亚胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置50μm等间隙等间隔的模具，真空抽滤碳纳米管分散液，抽滤后移动模具50μm使碳纳米管和聚乙烯亚胺首尾相接排列，然后再抽滤聚乙烯亚胺分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置50μm等间隙等间隔的模具，真空抽滤碳纳米管分散液，抽滤后移动模具使碳纳米管和聚乙烯亚胺首尾相接排列，然后再抽滤聚乙烯亚胺分散液；50℃干燥5h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中碳纳米管分散液、聚乙烯亚胺分散液体积(ml):滤膜直径(cm)＝2:1。
制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了92.7％。
实施例3：
1)将长碳纤维丝束在80℃的丙酮溶液中冷凝回流48h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥4h。
2)将步骤1)处理得到的碳纤维丝束在硫酸中100℃处理3h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥4h。
3)将长约1μm和直径35nm的纳米纤维素分散在水溶液中，200rpm/min磁力搅拌30min使其分散均匀，得到质量分数为0.01％的纳米纤维素分散液。
4)将聚多巴胺分散在三羟甲基氨基甲烷盐酸盐缓冲液中，300rpm/min磁力搅拌30min使其分散均匀，得到质量分数为0.1％的聚多巴胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置100μm等间隙等间隔的模具，真空抽滤纳米纤维素分散液，抽滤后移动模具100μm使纳米纤维素和聚多巴胺首尾相接排列，然后再抽滤聚多巴胺分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置100μm等间隙等间隔的模具，真空抽滤纳米纤维素分散液，抽滤后移动模具100μm使纳米纤维素和聚多巴胺首尾相接排列，然后再抽滤聚多巴胺分散液；70℃干燥4h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中纳米纤维素分散液、聚多巴胺分散液体积(ml):滤膜直径(cm)＝8:1。
制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了67.8％。
实施例4：
1)将长碳纤维丝束在90℃的丙酮溶液中冷凝回流48h，后用去离子水清洗纤维并在真空干燥箱中80℃干燥3h。
2)将步骤1)处理得到的碳纤维丝束在王水中80℃处理8h，后用去离子水清洗纤维并在真空干燥箱中80℃干燥3h。
3)将长约2～20μm和直径50～120nm的氧化锌纳米线分散在四氢呋喃中，1000rpm/min磁力搅拌120min使其分散均匀，得到质量分数为5％的氧化锌纳米线分散液。
4)将聚酰胺-胺型树枝状高分子分散在四氢呋喃中，500rpm/min磁力搅拌60min使其分散均匀，得到质量分数为5％的聚酰胺-胺型树枝状高分子分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置80μm等间隙等间隔的模具，真空抽滤聚酰胺-胺型树枝状高分子分散液，抽滤后移动模具80μm使聚酰胺-胺型树枝状高分子和氧化锌纳米线首尾相接排列，然后再抽滤氧化锌纳米线分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置80μm等间隙等间隔的模具，真空抽滤聚酰胺-胺型树枝状高分子分散液，抽滤后移动模具80μm使聚酰胺-胺型树枝状高分子和氧化锌纳米线首尾相接排列，然后再抽滤氧化锌纳米线分散液；80℃干燥3h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中聚酰胺-胺型树枝状高分子分散液、氧化锌纳米线分散液体积(ml):滤膜直径(cm)＝0.1:1。
制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了110.5％。
实施例5：
1)将长碳纤维丝束在100℃的丙酮溶液中冷凝回流24h，后用去离子水清洗纤维并在真空干燥箱中80℃干燥5h。
2)将步骤1)处理得到的碳纤维丝束在硫酸中100℃处理3h，后用去离子水清洗纤维并在真空干燥箱中80℃干燥5h。
3)将长约2～20μm和直径50～120nm的氧化锌纳米线分散在四氢呋喃中，800rpm/min磁力搅拌100min使其分散均匀，得到质量分数为2.5％的氧化锌纳米线分散液。
4)将聚丙烯亚胺分散在四氢呋喃中，400rpm/min磁力搅拌40min使其分散均匀，得到质量分数为3％的聚丙烯亚胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置500μm等间隙等间隔的模具，真空抽滤聚丙烯亚胺分散液，抽滤后移动模具500μm使聚丙烯亚胺和氧化锌纳米线首尾相接排列，然后再抽滤氧化锌纳米线分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置500μm等间隙等间隔的模具，真空抽滤聚丙烯亚胺分散液，抽滤后移动模具500μm使聚丙烯亚胺和氧化锌纳米线首尾相接排列，然后再抽滤氧化锌纳米线分散液；80℃干燥5h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中聚丙烯亚胺分散液、氧化锌纳米线分散液体积(ml):滤膜直径(cm)＝3:1。
实施例6：
1)将长碳纤维丝束在85℃的丙酮溶液中冷凝回流48h，后用去离子水清洗纤维并在真空干燥箱中60℃干燥2h。
2)将步骤1)处理得到的碳纤维丝束在硫酸中85℃处理4h，后用去离子水清洗纤维并在真空干燥箱中60℃干燥2h。
3)将长约20～30μm和直径100nm的二氧化钛纳米线分散在丙酮中，600rpm/min磁力搅拌60min使其分散均匀，得到质量分数为1.5％的二氧化钛纳米线分散液。
4)将超支化聚酰胺分散在丙酮中，600rpm/min磁力搅拌20min使其分散均匀，得到质量分数为1.5％的超支化聚酰胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置120μm等间隙等间隔的模具，真空抽滤二氧化钛纳米线分散液，抽滤后移动模具120μm使二氧化钛纳米线和超支化聚酰胺首尾相接排列，然后再抽滤超支化聚酰胺分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置120μm等间隙等间隔的模具，真空抽滤二氧化钛纳米线分散液，抽滤后移动模具120μm使二氧化钛纳米线和超支化聚酰胺首尾相接排列，然后再抽滤超支化聚酰胺分散液；60℃干燥2h得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中二氧化钛纳米线分散液、超支化聚酰胺分散液体积(ml):滤膜直径(cm)＝4:1。
制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了43.3％。
实施例7：
1)将长碳纤维丝束在95℃的丙酮溶液中冷凝回流12h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥3h。
2)将步骤1)处理得到的碳纤维丝束在硫酸中95℃处理5h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥3h。
3)将长约1μm和直径60nm的二氧化硅晶须分散在丙酮中，800rpm/min磁力搅拌80min使其分散均匀，得到质量分数为0.01％的二氧化硅晶须分散液。
4)将端氨基超支化聚合物分散在二甲基甲酰胺中，400rpm/min磁力搅拌20min使其分散均匀，得到质量分数为0.1％的端氨基超支化聚合物分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置300μm等间隙等间隔的模具，真空抽滤二氧化硅晶须分散液，抽滤后移动模具300μm使二氧化硅晶须和端氨基超支化聚合物首尾相接排列，然后再抽滤端氨基超支化聚合物分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置300μm等间隙等间隔的模具，真空抽滤二氧化硅晶须分散液，抽滤后移动模具300μm使二氧化硅晶须和端氨基超支化聚合物首尾相接排列，然后再抽滤端氨基超支化聚合物分散液；70℃干燥3h一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中二氧化硅晶须分散液、端氨基超支化聚合物分散液体积(ml):滤膜直径(cm)＝6:1。
制备的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维增强环氧复合材料的界面粘结强度相比未改性碳纤维增强环氧复合材料提高了88.4％。
实施例8：
1)将长碳纤维丝束在105℃的丙酮溶液中冷凝回流12h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥5h。
2)将步骤1)处理得到的碳纤维丝束在硫酸中105℃处理6h，后用去离子水清洗纤维并在真空干燥箱中70℃干燥5h。
3)将长约1μm和直径60nm的二氧化硅晶须分散在丙酮中，700rpm/min磁力搅拌60min使其分散均匀，得到质量分数为0.5％的二氧化硅晶须分散液。
4)将三聚氰胺分散在二甲基甲酰胺中，300rpm/min磁力搅拌10min使其分散均匀，得到质量分数为0.5％的三聚氰胺分散液。
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置100μm等间隙等间隔的模具，真空抽滤三聚氰胺分散液，抽滤后移动模具100μm使三聚氰胺和二氧化硅晶须首尾相接排列，然后再抽滤二氧化硅晶须分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置100μm等间隙等间隔的模具，真空抽滤三聚氰胺分散液，抽滤后移动模具100μm使三聚氰胺和二氧化硅晶须首尾相接排列，然后再抽滤二氧化硅晶须分散液；70℃干燥5h得一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；其中二三聚氰胺分散液、二氧化硅晶须分散液体积(ml):滤膜直径(cm)＝5:1。
Claims (10)
1.一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于该方法按如下步骤进行：
1)将碳纤维丝束在丙酮溶液中冷凝回流，然后用去离子水清洗干净并真空干燥；
2)将步骤1)处理得到的碳纤维丝束在浓酸中处理后用去离子水清洗干净并在真空干燥；
3)将一维纳米材料分散在水或有机溶剂中，磁力搅拌使其分散均匀，得到质量分数为0.01％～5％的一维纳米材料分散液；
4)将高分子胺类分散在有机溶剂中，磁力搅拌使其分散均匀，得到质量分数为0.1％～5％的高分子胺类分散液；
5)将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤一维纳米材料分散液，抽滤后移动模具使一维纳米材料和高分子胺首尾相接排列，然后再抽滤高分子胺类分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤一维纳米材料分散液，抽滤后移动模具使一维纳米材料和高分子胺首尾相接排列，然后再抽滤高分子胺类分散液，干燥后得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维；
将步骤2)处理得到的碳纤维丝束均匀铺放在滤膜上，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤高分子胺类分散液，抽滤后移动模具使高分子胺和一维纳米材料首尾相接排列，然后再抽滤一维纳米材料分散液；将抽滤过的碳纤维丝束翻转180°，沿垂直于碳纤维轴向的方向放置具有等间隙等间隔的模具，真空抽滤高分子胺类分散液，抽滤后移动模具使高分子胺和一维纳米材料首尾相接排列，然后再抽滤一维纳米材料分散液，干燥后得到一维纳米材料/高分子胺类首尾交替排列改性的碳纤维。
2.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于，所述步骤(1)的碳纤维为长碳纤维。
3.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤1)的回流温度为80～100℃，回流时间为12～48h。
4.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤2)的浓酸采用硝酸、硫酸或王水，浓酸处理温度为80～100℃，时间为3～8h。
5.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤3)一维纳米材料长径比＞10，直径1～100nm的纳米纤维素、碳纳米管、氧化锌纳米线、二氧化钛纳米线或二氧化硅晶须。
6.根据权利要求1所述的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤3)的磁力搅拌转速为200～1000rpm/min，时间为30～120min；
所述步骤4)的磁力搅拌转速为200～800rpm/min，时间为10～60min。
7.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤4)的高分子胺类为聚醚胺、聚多巴胺、聚乙烯亚胺、聚丙烯亚胺、三聚氰胺、聚酰胺-胺型树枝状高分子、超支化聚酰胺或端氨基超支化聚合物。
8.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤3)和4)的有机溶剂为丙酮、乙醇、四氢呋喃、二甲基甲酰胺、二氯甲烷、三羟甲基氨基甲烷盐酸盐缓冲液。
9.根据权利要求1所述的一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤5)的模具间隙与间隔距离均为50～500μm。
10.根据权利要求1所述的一种一维纳米材料/高分子胺类首尾交替排列改性碳纤维的制备方法，其特征在于：所述步骤5)真空抽滤按一维纳米材料分散液、高分子胺类分散液体积(ml):滤膜直径(cm)＝(0.1～8):1。
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