原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响

doi:10.7503/cjcu20170184

高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (11): 2128.doi: 10.7503/cjcu20170184

• 高分子化学 • 上一篇

原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响

王卫¹(), 徐佳丽¹, 林元菲², 李薛宇², 孟令蒲²(), 李良彬²

1. 石河子大学化学化工学院, 新疆兵团化工绿色过程重点实验室, 石河子 832003
2. 中国科学技术大学国家同步辐射实验室, 合肥 230029

收稿日期:2017-03-27 出版日期:2017-11-10 发布日期:2017-09-15
作者简介:联系人简介: 王卫, 男, 博士, 副教授, 主要从事催化化学及环境学研究. E-mail: wangweiww0409@sina.com。孟令蒲, 男, 博士, 主要从事高性能薄膜拉伸加工物理研究. E-mail: mlp2014@ustc.edu.cn
基金资助:
国家自然科学基金(批准号: 21267020)和中国博士后科学基金(批准号: 2017M612087)资助

Effect of Hot Stretching on the Structure of Polypropylene Microporous Membranes with in situ Small Angle X-Ray Scattering^†

WANG Wei^1,^*(), XU Jiali¹, LIN Yuanfei², LI Xueyu², MENG Lingpu^2,^*(), LI Liangbin²

1. School of Chemistry and Chemical Engineering, Key Laboratory for Green Processing of Chemical Engineering of Xinjiang Bingtuan, Shihezi University, Shihezi 832003, China
2. National Synchrotron Radiation Laboratory,University of Science and Technology of China, Hefei 230029, China

Received:2017-03-27 Online:2017-11-10 Published:2017-09-15
Contact: WANG Wei,MENG Lingpu E-mail:wangweiww0409@sina.com;mlp2014@ustc.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(No.21267020) and the China Postdoctoral Science Foundation(No.2017M612087)

摘要/Abstract

摘要：

采用原位小角X射线散射和扫描电子显微镜研究了热拉过程中, 拉伸比和拉伸温度对熔融拉伸法制备的聚丙烯微孔膜晶体和孔洞结构的影响. 研究结果表明, 冷拉、热定型过程中片晶簇被分离开, 其内部结构在热拉过程中不发生分离等变形; 随着热拉拉伸比的增加, 片晶簇间架桥长度不断增大; 与冷拉、热定型样品相比, 热拉后的微孔膜架桥沿垂直于拉伸方向具有较好的周期性. 不同的拉伸温度结果表明, 架桥长度随拉伸温度升高而增加; 温度过高时架桥会发生熔融.

关键词: 聚丙烯微孔膜, 原位小角X射线散射, 冷拉-热定型-热拉, 微孔, 片晶簇

Abstract:

With in situ small angle X-ray scattering and scanning electron microscopy measurements, effects of hot stretching temperatures and draw ratios on the lamellae and pore structure of the polypropylene microporous membrane were studied. The results show that the lamellar clusters are separated during the cold stretching and heat setting process, while the internal structures do not undergo separation during the hot stretching process. With the increase of the hot stretching ratio, the bridge length of microporous membrane after hot stretching process increases substantially. Also, it has better periodicity along the equatorial direction compared with the cold-stretching and heat-setting samples. The results of different stretching temperatures show that the length of the bridge increases with the increase of the stretching temperature. When the temperature is too high, the bridge will partially melt. This work can provide guidance for the structural control during preparation of polypropylene microporous membranes.

Key words: Polypropylene microporous membrane, In situ small angle X-ray scattering, Cold stretching-heat setting-hot stretching, Micropore, Lamellar cluster

中图分类号:

O631

TrendMD:

王卫, 徐佳丽, 林元菲, 李薛宇, 孟令蒲, 李良彬. 原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响. 高等学校化学学报, 2017, 38(11): 2128.

WANG Wei, XU Jiali, LIN Yuanfei, LI Xueyu, MENG Lingpu, LI Liangbin. Effect of Hot Stretching on the Structure of Polypropylene Microporous Membranes with in situ Small Angle X-Ray Scattering^†. Chem. J. Chinese Universities, 2017, 38(11): 2128.

图/表 11

Fig.1 Pictures of the tensile apparatus for microporous membrane preparation(A) and polypropylene microporous membrane after stretching(B)

Fig.2 2D SAXS patterns of samples stretched to 30% at room temperature and then hot stretched with different strains(A1—A4), heat-set(B1—B4) and cooled down(C1—C4)(A1—C1) L0.3R1.0; (A2—C2) L0.3R1.5; (A3—C3) L0.3R2.0; (A4—C4) L0.3R2.5.

Fig.3 SEM images of L0.3 and other membranes with different hot stretching ratios(A) L0.3R1.0; (B) L0.3R1.5; (C) L0.3R2.0; (D) L0.3R2.5; (E) L0.3.

Fig.4 Average length of bridges(a), lamellar stack thickness(b), mean lamellar thickness(c) and long period(d)

Fig.5 Curves of one-dimensional electron density correlation functionInset: long period(L) and amorphous thickness(da).

Fig.6 SAXS integral curves along equatorial direction of L0.3 and microporous films made of different draw ratios at higher temperature

Fig.7 SAXS patterns of different stretching temperature during hot stretching(A1—A3), heat setting(B1—B3) and cooling down(C1—C3) (A1)—(C1) W127; (A2)—(C2) W135; (A3)—(C3) W153.

Table 1 Some parameters of different hot stretching temperatures

State	W₁₂₇		W₁₃₅		W₁₅₃
State	L/nm	d_c/nm	L/nm	d_c/nm	L/nm	d_c/nm
Heat stretching	22.9	12.7	22.9	12.7	23.7	13.4
Heat setting	23.7	13.3	24.1	13.7	23.3	12.6
Cool down	22.9	12.7	24.1	13.7	22.9	12.7

Fig.8 SEM images of microporous films made at different hot stretching temperatures(A) W127; (B) W135; (C) W153.

Fig.9 Bridge length and lamellar stack thickness

Fig.10 SAXS integral curves of equatorial direction of samples made at different hot stretching temperatures

参考文献 18

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原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响

Effect of Hot Stretching on the Structure of Polypropylene Microporous Membranes with in situ Small Angle X-Ray Scattering^†

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原位小角X射线散射研究热拉工艺对熔融拉伸法制备的聚丙烯微孔膜结构的影响

Effect of Hot Stretching on the Structure of Polypropylene Microporous Membranes with in situ Small Angle X-Ray Scattering†

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Effect of Hot Stretching on the Structure of Polypropylene Microporous Membranes with in situ Small Angle X-Ray Scattering^†