Solution Small-Angle Scattering in Soft Matter: Application and Prospective※

doi:10.6023/A21120624

Acta Chimica Sinica ›› 2022, Vol. 80 ›› Issue (5): 690-702.DOI: 10.6023/A21120624 Previous Articles

Special Issue: 中国科学院青年创新促进会合辑

Review

溶液小角散射技术在软物质研究中的应用与展望^※

宋攀奇, 张建桥, 李怡雯, 刘广峰, 李娜^*()

中国科学院上海高等研究院国家蛋白质科学研究(上海)设施张江国家实验室上海 201210

投稿日期:2021-12-31 发布日期:2022-05-31
通讯作者: 李娜

作者简介:

宋攀奇, 硕士, 助理工程师, 毕业于北京理工大学, 现于国家蛋白质科学研究(上海)设施工作, 负责同步辐射生物小角散射线站的运行、管理工作, 参与线站的用户服务和技术支持. 主要研究方向为基于同步辐射BioSAXS技术进行方法学开发研究.

张建桥, 硕士, 助理工程师, 毕业于西南科技大学, 现于国家蛋白质科学研究(上海)设施工作, 负责协助开展BL19U2生物小角X射线散射(BioSAXS)线站的运行、维护和管理工作.

李怡雯, 博士, 工程师, 同步辐射生物小角X射线散射线站用户负责人, 毕业于中国科学院上海应用物理研究所, 获核科学与技术专业博士学位, 主要从事脂质体药物结构研究、X射线小角散射实验方法学研究. 作为项目骨干参与国家重点研发项目1项、中科院基础设施维修改造项目1项, 主持国家自然科学基金青年项目1项.

刘广峰, 博士, 副研究员, 同步辐射生物小角X-射线散射线站运行负责人, 毕业于中国科学院高能物理研究所, 主要从事生物小角散射线站的运行维护工作. 作为项目骨干参加了中国科学院战略性先导科技专项(B类)生物小角X射线散射技术及国家自然科学基金大科学装置联合基金重点项目, 主持自然科学基金青年项目1项, 入选2020年中科院青年创新促进会会员.

李娜, 博士, 副研究员, 同步辐射生物小角X射线散射线站团队负责人. 现担任中国晶体学会小角散射委员会委员、中国生物物理学会分子生物物理委员会委员、中国科学院青年创新促进会会员. 2011年加入国家蛋白质科学研究(上海)设施. 主要研究方向为基于同步辐射溶液散射技术方法开发以及溶液散射技术在软物质领域中的应用研究. 曾作为第四完成人获得中国水产科学研究院科技进步二等奖. 已在国际知名期刊发表论文68篇. 已提交专利申请4项, 获批1项. 现已出版科普译著1部、科普专著1部; 同时参与撰写学术专著1部; 主持完成学术译著1部. 作为项目负责人主持科研项目11项; 作为技术骨干参与科研项目4项; 多次组织生物小角散射技术相关的国际培训课程及国际会议, 录制生物小角散射专业技术微课, 于2019年12月份上线中科院继续教育网络课程.

^※庆祝中国科学院青年创新促进会十年华诞.

基金资助:
国家自然科学基金(U1832144); 中科院青年创新促进会人才项目(2017319); 上海市自然科学基金(21ZR1471600)

Solution Small-Angle Scattering in Soft Matter: Application and Prospective^※

Panqi Song, Jianqiao Zhang, Yiwen Li, Guangfeng Liu, Na Li()

National Facility for Protein Science in Shanghai, Zhangjiang Laboratory, Shanghai Advanced Research Institute, Chinese Academy of Sciences, Shanghai 201210

Received:2021-12-31 Published:2022-05-31
Contact: Na Li
About author:
^※Dedicated to the 10th anniversary of the Youth Innovation Promotion Association, CAS.
Supported by:
National Natural Science Foundation of China(U1832144); Youth Innovation Promotion Association of Chinese Academy of Sciences(2017319); Natural Science Foundation of Shanghai(21ZR1471600)

Solution small-angle scattering (SAS) is a powerful tool for elucidating the structural properties of soft matter systems. SAS includes X-ray scattering (SAXS) and Neutron scattering (SANS) techniques which allow determination of the material’s properties at a scale ranging from few Angstroms to hundreds of nanometers. Wide time scales ranging from real time (milliseconds) to several minutes can be also covered by these techniques. In recent years, solution SAS techniques have had versatile applications in several research fields, especially in structural biology and in probing self-assembling nanomaterials. Probing the structure of materials at micro- and nano-scales provide an insight on the macroscopic properties of the material. The high throughput and fast time resolution offered by SAXS in combination with the neutron penetrating ability in SANS can offer a great potential to cover different soft-matter systems and processes (i.e. probing the kinetic of self-assembly). Here we review the solution SAS (both synchrotrons and Neutron Sources) capabilities which have been established in mainland China, and cover scattering theoretical developments. Recent advances in solutions SAS used in soft matter will also be discussed. Given the potential offered by the next generation X-ray and Neutron sources, further developments in this field are expected, with a proliferation of solution SAS applications.

Key words: solution SAXS, solution SANS, soft matter, high-throughput, structural dynamics

Cite this article

Panqi Song, Jianqiao Zhang, Yiwen Li, Guangfeng Liu, Na Li. Solution Small-Angle Scattering in Soft Matter: Application and Prospective^※[J]. Acta Chimica Sinica, 2022, 80(5): 690-702.

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Fig. & Tab. 10

Beamline	Synchrotron	Source type	Energy range/keV	Flux/(phs•s^–1)	Beam size (mm×mm)	Detectable spatial size (Max)/nm
1W2A	BSRF	Wiggler	8	≈10¹¹	1.4×0.2	200
Pinkbeam SAXS	HEPS	Undulator	8~12	≈10¹³~10¹⁵	0.5×0.5/0.05×0.05	5000
BL16B1	SSRF	Bending magnet	5~20	≈10¹¹	0.16×0.24	240
BL19U2	SSRF	Undulator	7~15	≈10¹²	0.33×0.05/0.01×0.01	300
BL10U1	SSRF	Undulator	8~15	≈10¹³	0.4×0.45/0.008×0.006	2100

Table 1. List of synchrotron facility based SAXS beamline in mainland China (both in operation and under construction)

Spectrometer	Neutron source	λ range/nm	Flux/(cm^–2•s^–1)	Beam size (mm×mm)
Suanni	CMRR	0.25~2, 0.35~2	1.18×10⁷	Aperture Φ 4~10
CNGD	CARR	0.4~2	10⁴~10⁷	Aperture Φ 5~25
SANS	CSNS	0.12~0.95, 0.12~1.1	1.08×10⁸/6.46×10⁶	20×30
VSANS	CSNS	0.24~1.14	2.2×10⁵	20×30

Table 2. List of neutron source based SANS beamline in mainland China (both in operation and under construction)

Figure 1. View of sample environments at BL19U2 (Color online). (a) In-vacuum automated sample changer. (b) Inline sample purification system, showing in-vacuum cell unit, high-performance liquid chromatography (HPLC), multi-angle light scattering, and refractive index detection devices (MALS and RI)[18]

Figure 2. Dissociation behavior of supramolecular polymers. (A) SAXS profiles of the as-prepared solution (green curve) and the 7-day-old solution (orange curve) of 1 (c=5×10-5 mol/L) prepared by cooling from 373 to 293 K at a cooling rate of 1.0 K•min-1. The black curve is the profile obtained from subtracting the two data sets. The black dashed curve is a simulation SAXS profile of the as-prepared sample data using a hollow cylinder model. (B) Temperature-dependent ultraviolet-visible (UV-Vis) spectra of an MCH solution of 1 (c=5×10-6 mol/L) upon cooling (1.0 K•min-1). The arrows indicate the changes in absorption spectra upon cooling. (C) Cooling and heating curves of 1 (c=5×10-6 mol/L) in MCH obtained by plotting the molar fractions of the aggregated molecules (αagg, calculated from the absorption change at λ=470 nm) as a function of the temperature during cooling (1.0 K•min-1; black dots) and subsequent heating after aging for 0 min (purple dots), 12 h (blue dots), 1 d (cyan dots), 1.5 d (green dots), 2 d (yellow dots), 3 d (orange dots), 5 d (pink dots), and 7 d (red dots) at 293 K. (D) Heating curves of the 7-day-oldMCH solution of 1, prepared using a cooling rate of 1.0 K•min-1 at different concentrations (purple dots, c=5×10-6 mol/L; cyan dots, c=6×10-6 mol/L; green dots, c=7×10-6 mol/L; yellow dots, c=8×10-6 mol/L; pink dots, c=1×10-5 mol/L). The black solid curves were obtained from fitting the experimental data to the cooperative model. Inset: van’t Hoff plot obtained from plotting the natural logarithm of CT–1 as a function of Te–1. The red line shows the corresponding linear fit. (E) The proposed mechanism of the thermal dissociation of the as-prepared supramolecular polymer in temperature regimes I and II. (F) AFM images of the as-prepared supramolecular polymer of 1, spin-coated onto HOPG substrate after heating to 343 K for 3 min. Scale bar, 100 nm[35]

Figure 3. Structural characterization of PtII amphiphiles in the bulk. (A, B) One-dimensional SAXS (Left) and WAXS (Right) patterns of bulk samples of 1 (A) and 4 (B) at 298 K (Miller indices in parentheses). (C) Top (Left) and side (Right) view schematic representations of the molecular arrangement of 1 in a 3D hexagonal lattice. Pt centers adopt a rhombitrihexagonal AT-like order, wherein red, orange, and green polygons represent the phase-separated domains consisting of the [Pt(tpy)-OPE-3] segments, TEG chains, and C18 chains, respectively. (D) Top-view schematic representation of the molecular arrangement of 4 in a 1D lamellar lattice with phase separation of hydrophilic (blue) and hydrophobic (gray) domains.[36]

Figure 4. (A) XRD patterns of the ST monomer powders and the resulting poly (ST) film. (B) Synchrotron radiation SAXS pattern of the poly (ST) film. Inset image shows the distinctive scattering ring of the sample. (C) One-dimensional GIWAXS plot of the poly (ST) film. Scattering intensity is plotted versus q. (D) Two-dimensional GIWAXS pattern of the poly (ST) film[39]

Figure 5. (a) Symbols represent the experimental data, and solid lines represent the fitting curves. (b) The log-log plot of scattering intensity versus scattering vector at 659 and 1244 ms (0.5 mol/L sodium silicate, 0.5 mol/L sulfuric acid, total flow rate 12.3 mL/min, 343 K)[41]

Figure 6. Conserved dimerization mode of hGBPs. (A) The calculated scattering curve using the crystal structure of hGBP51-486 in complex with GDP AlF3 is in agreement with the SAXS data. (B) The crystal structure fits the SAXS envelope. (C) hGBP1FL, hGBP2FL, and hGBP5FL have similar scattering curves. (D) The SAXS data support a closed conformation of hGBP5FL in solution[55]

Figure 7. Structural analysis of complete sfRNAs via SAXS (Color online). (a) Ab initio shape envelopes of complete sfRNAs. (b) Fitted chi-square plotted against ensemble size for complete sfRNAs[57]

Figure 8. SAXS pattern and its fit curve (A), SAXS pattern and its profile of power-law scattering PL plus scattering background B (B), decomposition of SAXS patterns into sub-patterns of net lamellar peak and PL+B (C), and linear correlation function profiles (D) for potato starch (PS)[68]

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溶液小角散射技术在软物质研究中的应用与展望^※

Solution Small-Angle Scattering in Soft Matter: Application and Prospective^※

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溶液小角散射技术在软物质研究中的应用与展望※

Solution Small-Angle Scattering in Soft Matter: Application and Prospective※

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Abstract

Cite this article

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Fig. & Tab. 10

References 75

Related Articles 4

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溶液小角散射技术在软物质研究中的应用与展望^※

Solution Small-Angle Scattering in Soft Matter: Application and Prospective^※