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嵌段共聚物PS-
b -PAA自组装过程的原位小角X射线散射In-situ SAXS study on self-assembly of copolymer PS-
b -PAA- 核技术 2018年41卷第8期 文章编号：080102
- 作者机构：
1.中国科学院上海应用物理研究所 上海光源 张江园区 上海 201204
2.中国科学院大学 北京 100049
3.华东理工大学 上海 200237
4.中国科学院上海高等研究院 国家蛋白质中心 上海 201210
- 作者简介：
[ "金鑫, 男, 1991年出生, 2012年毕业于中国科技大学, 现为博士研究生, 研究领域为小角X射线散射", "JIN Xin, male, born in 1991, graduated from University of Science and Technology of China in 2012, doctoral student, focusing on small angle X-ray scattering" ]
杨春明, E-mail:yangchunming@sinap.ac.cn YANG Chunming, E-mail:yangchunming@sinap.ac.cn
王劼, E-mail:wangjie@sinap.ac.cn WANG Jie, E-mail:wangjie@sinap.ac.cn
- 基金信息：上海市科学技术委员(17JC1400802);国家重点研发计划(2017YFA0403000);国家自然科学基金(11405259)
DOI：10.11889/j.0253-3219.2018.hjs.41.080102
中图分类号： O562.4收稿日期：2018-02-13，
修回日期：2018-04-01，
纸质出版日期：2018-08
- 稿件说明：
移动端阅览
金鑫, 王建军, 李怡雯, 等. 嵌段共聚物PS-
b -PAA自组装过程的原位小角X射线散射[J]. 核技术, 2018,41(8):080102Xin JIN, Jianjun WANG, Yiwen LI, et al. In-situ SAXS study on self-assembly of copolymer PS-
b -PAA[J]. Nuclear techniques, 2018, 41(8): 080102金鑫, 王建军, 李怡雯, 等. 嵌段共聚物PS-
b -PAA自组装过程的原位小角X射线散射[J]. 核技术, 2018,41(8):080102 DOI： 10.11889/j.0253-3219.2018.hjs.41.080102.Xin JIN, Jianjun WANG, Yiwen LI, et al. In-situ SAXS study on self-assembly of copolymer PS-
b -PAA[J]. Nuclear techniques, 2018, 41(8): 080102 DOI： 10.11889/j.0253-3219.2018.hjs.41.080102.
摘要
以嵌段共聚物聚苯乙烯聚丙烯酸（PS
3000
-
b
-PAA
5000
）（分子数分别为PS：PAA=3000：5000）为研究对象，应用变温小角X射线散射（Small-angle X-ray Scattering，SAXS）技术对其自组装过程进行了原位研究。SAXS峰位被发现随着温度的升高从
q
≈0.73 nm
-1
移动至低
q
区的
q
≈0.39 nm
-1
附近，同时SAXS峰的半峰宽、积分面积和强度的最大值也发生相应的转变。结果分析表明：该嵌段共聚物在128 ℃附近发生相变，相变温度跨度约为5 ℃。应用对距离分布函数（Pair Distance Distribution Function，PDDF），对SAXS数据进行拟合分析后发现：相变前为表面带有起伏的棒状体，随着温度升高棒状体出现孔洞，且棒状体变短，随后逐渐由棒状转变为带孔的球状体，并逐渐最终长大为直径30 nm左右的类球体。
Abstract
Background
2
Block copolymers can spontaneously self-assemble into various micro-scale morphologies under the various external fields
which have an extensive potential on the application of the electronics
information
chemistry and biology
etc. However
the self-assembly process is still a "black box"
the understanding is still limited to the evolution of morphology during the varying external conditions.
Purpose
2
This study aims to investigate the self-assembly behavior of Poly(styrene)-block-poly (acrylic acid) (PS-
b
-PAA) in the temperature field by using in-situ synchrotron radiation small-angle X-ray scattering (SAXS).
Methods
2
SAXS experiments were performed on the BL16B1 beamline of Shanghai Synchrotron Radiation Facility (SSRF). Energy was selected as 10 keV and the wave length is 0.124 nm. 2D SAXS patterns were recorded by Mar165 CCD with pixel size of 79 μm×79 μm. A sample-to-detector distance of 1946 mm was chosen. The temperatures of the specimens were monitored by using a Linkam thermal stage THMS600 (Linkam scientific instruments). One-dimensional integrated intensity curves were obtained from 2D SAXS patterns by self-developed software. PS-
b
-PAAs (PS:PAA=3000:5000) were used directly as purchased from Sigma-Aldrich Inc.
Results
2
The in-situ SAXS experiment shows that the center of scattering peak was shifted with increasing temperature from
q
≈0.73 nm
-1
to
q
≈0.39 nm
-1
which was also accompanied by the varying of full width of half maximum
integral area
and maximum value of SAXS peak. A phase transition temperature was estimated as
T
c
=128℃ and the temperature width of transition is 5℃. Pair distance distribution function was used for the analysis of SAXS data.
Conclusion
2
With increasing temperature
the length of particle decreased gradually and body perforated
A rod-like shape with an undulating surface exists before the phase transition. At the temperature higher than
T
c
the particle was degraded from the rod-like shape changes to a near-spherical shape still contains hole residue. The particles grow and gradually condense into a larger sphere with a diameter of~30 nm at the later stage.
关键词
Keywords
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