A small/wide-angle X-ray scattering instrument for structural characterization of air-liquid interfaces, thin films and bulk specimens

被引:159
作者
Jeng, U-Ser [1 ]
Su, Chiu Hun [1 ]
Su, Chun-Jen [1 ]
Liao, Kuei-Fen [1 ]
Chuang, Wei-Tsung [1 ]
Lai, Ying-Huang [2 ]
Chang, Je-Wei [2 ]
Chen, Yi-Jiun [2 ]
Huang, Yu-Shan [1 ]
Lee, Ming-Tao [1 ]
Yu, Kuan-Li [1 ]
Lin, Jhih-Min [3 ]
Liu, Din-Goa [1 ]
Chang, Chia-Feng [1 ]
Liu, Chin-Yen [1 ]
Chang, Chien-Hung [1 ]
Liang, Keng S. [1 ]
机构
[1] Natl Synchrotron Radiat Res Ctr, Hsinchu 300, Taiwan
[2] Tunghai Univ, Dept Chem, Taichung 407, Taiwan
[3] Australian Natl Univ, Res Sch Chem, Canberra, ACT 0200, Australia
关键词
ANOMALOUS SMALL-ANGLE; ADVANCED PHOTON SOURCE; BEAMLINE; ABSORPTION; NSRRC; DIFFRACTION; CRYSTALLIZATION; SYNCHROTRON; DISPERSION; APPARATUS;
D O I
10.1107/S0021889809043271
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
At the National Synchrotron Radiation Research Center, a small/wide-angle X-ray scattering (SAXS/WAXS) instrument has been installed at the BL23A beamline with a superconducting wiggler insertion device. This beamline is equipped with double Si(111) crystal and double Mo/B(4)C multilayer monochromators, and an Si-based plane mirror that can selectively deflect the beam downwards for grazing-incidence SAXS (GISAXS) studies of air-liquid or liquid-liquid interfaces. The SAXS/WAXS instrument, situated in an experimental hutch, comprises collimation, sample and post-sample stages. Pinholes and slits have been incorporated into the beam collimation system spanning a distance of similar to 5 m. The sample stage can accommodate various sample geometries for air-liquid interfaces, thin films, and solution and solid samples. The post-sample section consists of a 1 m WAXS section with two linear gas detectors, a vacuum bellows (1-4 m), a two-beamstop system and the SAXS detector system, all situated on a motorized optical bench for motion in six degrees of freedom. In particular, the vacuum bellows of a large inner diameter (260 mm) provides continuous changes of the sample-to-detector distance under vacuum. Synchronized SAXS and WAXS measurements are realized via a data-acquisition protocol that can integrate the two linear gas detectors for WAXS and the area detector for SAXS (gas type or Mar165 CCD); the protocol also incorporates sample changing and temperature control for programmable data collection. The performance of the instrument is illustrated via several different measurements, including (1) simultaneous SAXS/WAXS and differential scanning calorimetry for polymer crystallization, (2) structural evolution with a large ordering spacing of similar to 250 nm in a supramolecular complex, (3) SAXS for polymer blends under in situ drawing, (4) SAXS and anomalous SAXS for unilamellar lipid vesicles and metalloprotein solutions, ( 5) anomalous GISAXS for oriented membranes of Br-labeled lipids embedded with peptides, and (6) GISAXS for silicate films formed in situ at the air-water interface.
引用
收藏
页码:110 / 121
页数:12
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