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A small/wide‐angle X‐ray scattering instrument for structural characterization of air–liquid interfaces, thin films and bulk specimens
Author(s) -
Jeng USer,
Su Chiu Hun,
Su ChunJen,
Liao KueiFen,
Chuang WeiTsung,
Lai YingHuang,
Chang JeWei,
Chen YiJiun,
Huang YuShan,
Lee MingTao,
Yu KuanLi,
Lin JhihMin,
Liu DinGoa,
Chang ChiaFeng,
Liu ChinYen,
Chang ChienHung,
Liang Keng S.
Publication year - 2010
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889809043271
Subject(s) - beamline , small angle x ray scattering , collimated light , optics , materials science , wiggler , scattering , detector , bellows , grazing incidence small angle scattering , storage ring , beam (structure) , physics , laser , nuclear physics , inelastic scattering , cathode ray , metallurgy , x ray raman scattering , electron
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 ∼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 ∼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.