具有纳米结构的聚偏氟乙烯/1-乙烯基-3-丁基咪唑氯盐离子液体复合材料的结晶行为

doi:10.7503/cjcu20150822

高等学校化学学报 ›› 2016, Vol. 37 ›› Issue (4): 775.doi: 10.7503/cjcu20150822

具有纳米结构的聚偏氟乙烯/1-乙烯基-3-丁基咪唑氯盐离子液体复合材料的结晶行为

邢晨阳^1,^2,³, 王艳媛², 李勇进²(), 李景烨¹

1. 中国科学院上海应用物理研究所, 上海 201800
2. 杭州师范大学材料与化学化工学院, 杭州 310036
3. 中国科学院大学, 北京 100049

收稿日期:2015-10-26 出版日期:2016-04-10 发布日期:2016-03-16
基金资助:
国家自然科学基金(批准号: 51173036, 21374027)资助

Crystallization Behavior of Nanostructured Poly(vinylidene fluoride)/1-Vinyl-3-butylimidazolium Chloride Ionic Liquid Composites^†

XING Chenyang^1,^2,³, WANG Yanyuan², LI Yongjin^2,^*, LI Jingye¹()

1. Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China
2. College of Material, Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China
3. University of Chinese Academy of Sciences, Beijing 100049, China

Received:2015-10-26 Online:2016-04-10 Published:2016-03-16
Contact: LI Yongjin E-mail:20100106@hznu.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(Nos.51173036, 21374027)

摘要/Abstract

摘要：

用示差扫描量热(DSC)、偏光显微镜(POM)及X射线衍射(XRD)分析考察了具有纳米结构的聚偏氟乙烯(PVDF)/1-乙烯基-3-丁基咪唑氯盐离子液体([VBIM][Cl])复合材料(PVDF/[VBIM][Cl])中经[VBIM][Cl]接枝的PVDF(PVDF-g-[VBIM][Cl])纳米微区对PVDF结晶行为的影响. 研究结果表明, [VBIM][Cl]化学接枝在PVDF的分子链上, 在PVDF/[VBIM][Cl]复合材料中, PVDF-g-[VBIM][Cl]嵌段形成大量纳米微区, 分散在PVDF基体中. PVDF-g-[VBIM][Cl]纳米微区能够显著提高PVDF熔体结晶温度(T_c)并显著降低PVDF晶体的等温结晶时间. 与纯PVDF相比, 在纳米结构的PVDF/[VBIM][Cl]复合材料中, PVDF-g-[VBIM][Cl]纳米微区大大提高了PVDF晶体的成核速率, PVDF的球晶尺寸明显减小. 由于[VBIM][Cl]完全“受限”于PVDF-g-[VBIM][Cl]纳米微区中, 无法与PVDF分子链发生相互作用, 因此纳米结构的PVDF/[VBIM][Cl] 复合材料最终以非极性的α晶体为主. 由于PVDF-g-[VBIM][Cl]纳米微区与PVDF基体具有热力学不相容性, 因此其界面处的PVDF分子链处于部分有序的状态, 有助于PVDF晶体的成核, 加速了PVDF晶体的结晶速率.

关键词: 聚偏氟乙烯, 离子液体, 纳米结构, 结晶行为

Abstract:

The effect of poly(vinylidene fluoride)-graft-(1-vinyl-3-butylimidazolium chloride [VBIM][Cl])(i.e. PVDF-g-[VBIM][Cl]) nanodomains on the crystallization behavior in nanostructured PVDF/[VBIM][Cl] composite was investigated by means of differential scanning calorimeter(DSC), polarized optical microscope(POM) and wide-angle X-ray diffractometer(WAXD) measurements. ¹H nuclear magnetic resonance(¹H NMR) results confirm the successful grafting of [VBIM][Cl] onto the PVDF chains. Transmission electron microscopy(TEM) images show PVDF-g-[VBIM][Cl] nanodomains in the nanostructured PVDF/[VBIM][Cl](100/8, mass ratio) composite, which is distinct from the miscible PVDF/[VBIM][Cl] blend prepared by physically blending. The DSC results show higher crystallization temperature(T_c) and shorter crystallization time in the nanostructured PVDF/[VBIM][Cl] composite, compared with those of neat PVDF and PVDF/[VBIM][Cl] blend(100/8), respectively, indicating that nanodomains enhanced the crystallization rate of the PVDF crystals. Moreover, a larger nucleation density accompanied with smaller spherulites was observed in the nanostructured sample by POM photos. It is considered that strong thermodynamic incompatibility of nanodomains with PVDF matrix caused a large amount of partially ordered molecular chains at their interface, which favorites the nucleus formation and thus improves the entire crystallization rate of the PVDF crystals. Because of the confinement of [VBIM][Cl] within nanodomains, dominant non-polar α crystals were found in the nanostructured sample, which was the same with that of neat PVDF.

Key words: Poly(vinylidene fluoride), Ionic liquid, Nanostructure, Crystallization

中图分类号:

O631

TrendMD:

邢晨阳, 王艳媛, 李勇进, 李景烨. 具有纳米结构的聚偏氟乙烯/1-乙烯基-3-丁基咪唑氯盐离子液体复合材料的结晶行为. 高等学校化学学报, 2016, 37(4): 775.

XING Chenyang, WANG Yanyuan, LI Yongjin, LI Jingye. Crystallization Behavior of Nanostructured Poly(vinylidene fluoride)/1-Vinyl-3-butylimidazolium Chloride Ionic Liquid Composites^†. Chem. J. Chinese Universities, 2016, 37(4): 775.

图/表 5

Fig.1 1H NMR spectra of nanostructured PVDF/ [VBIM][Cl](100/8) composite^Inset: the possible chemical structure of PVDF-g-[VBIM][Cl].

Fig.2 TEM images of nanostructured PVDF/[VBIM][Cl](100/8) composite(A) ^ (B) Magnification of the rectangle of (A).

Fig.3 DSC curves of cooling run with a scanning rate of 10 ℃/min(A) and isothermal crystallization at 155 ℃(B) of neat PVDF(a), PVDF/[VBIM][Cl](100/8) blend(b) and nanostructured PVDF/[VBIM][Cl](100/8) composite(c)

Fig.4 POM photos of neat PVDF(A, B) and nanostructured PVDF/[VBIM][Cl](100/8) composite(C, D) at 155 ℃ ^Crystallization time/min: (A, C) 1; (B, D) 8.

Fig.5 Schematic structures of irradiated PVDF/[VBIM][Cl] sample(A), PVDF-g-[VBIM][Cl] nanodomains(B) and WAXD patterns of neat PVDF(a) and nanostructured PVDF/[VBIM][Cl](100/8) composite(b)(C)

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具有纳米结构的聚偏氟乙烯/1-乙烯基-3-丁基咪唑氯盐离子液体复合材料的结晶行为

Crystallization Behavior of Nanostructured Poly(vinylidene fluoride)/1-Vinyl-3-butylimidazolium Chloride Ionic Liquid Composites^†

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具有纳米结构的聚偏氟乙烯/1-乙烯基-3-丁基咪唑氯盐离子液体复合材料的结晶行为

Crystallization Behavior of Nanostructured Poly(vinylidene fluoride)/1-Vinyl-3-butylimidazolium Chloride Ionic Liquid Composites†

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Crystallization Behavior of Nanostructured Poly(vinylidene fluoride)/1-Vinyl-3-butylimidazolium Chloride Ionic Liquid Composites^†