4.2 Article

Flexible sample cell for real-time GISAXS, GIWAXS and XRR: design and construction

Journal

JOURNAL OF SYNCHROTRON RADIATION
Volume 25, Issue -, Pages 1664-1672

Publisher

INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S1600577518013218

Keywords

in situ; GIWAXS; GISAXS; XRR; thin film

Funding

  1. Deutsche Forschungsgemeinschaft (DFG) through the 'Cluster of Excellence Engineering of Advanced Materials (EAM)'
  2. research training group GRK 1896 'In situ Microscopy with Electrons, X-rays and Scanning Probes'
  3. research unit FOR 1878 'Functional Molecular Structures on Complex Oxide Surfaces'
  4. German Federal Ministry of Education and Research (BMBF) [05K16WEB, 05K16WE1]
  5. DFG [INST 90/825-1 FUGG, INST 90/751-1 FUGG, INST 90/827-1 FUGG]
  6. Bavarian State Government [FKZ 20.2-3410.5-4-5]
  7. DFG

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Since the properties of functional materials are highly dependent on their specific structure, and since the structural changes, for example during crystallization, induced by coating and annealing processes are significant, the study of structure and its formation is of interest for fundamental and applied science. However, structure analysis is often limited to ex situ determination of final states due to the lack of specialized sample cells that enable real-time investigations. The lack of such cells is mainly due to their fairly complex design and geometrical restrictions defined by the beamline setups. To overcome this obstacle, an advanced sample cell has been designed and constructed; it combines automated doctor blading, solvent vapor annealing and sample hydration with real-time grazing-incidence wide- and small-angle scattering (GIWAXS/GISAXS) and X-ray reflectivity (XRR). The sample cell has limited spatial requirements and is therefore widely usable at beamlines and laboratory-scale instruments. The cell is fully automatized and remains portable, including the necessary electronics. In addition, the cell can be used by interested scientists in cooperation with the Institute for Crystallography and Structural Physics and is expandable with regard to optical secondary probes. Exemplary research studies are presented, in the form of coating of P3HT:PC61PM thin films, solvent vapor annealing of DRCN5T:PC71BM thin films, and hydration of supported phospholipid multilayers, to demonstrate the capabilities of the in situ cell.

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