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Multi-use high/low-temperature and pressure compatible portable chamber for in situ grazing-incidence X-ray scattering studies

AuthorsFerrer, Pilar ; Rubio-Zuazo, J. ; Heyman, Catherine; Esteban-Betegón, Fátima ; Castro, Germán R.
KeywordsAtomic structure
Oxygen vacancies
Mixed-valence manganites
Environment set-up
Cooling–heating system
In situ X-ray scattering
Portable chamber
Issue Date1-May-2013
PublisherInternational Union of Crystallography
CitationJournal of Synchrotron Radiation 20: 474-481 (2013)
AbstractThe multipurpose portable ultra-high-vacuum-compatible chamber described in detail in this article has been designed to carry out grazing-incidence X-ray scattering techniques on the BM25-SpLine CRG beamline at the ESRF. The chamber has a cylindrical form, built on a 360° beryllium double-ended conflate flange (CF) nipple. The main advantage of this chamber design is the wide sample temperature range, which may be varied between 60 and 1000 K. Other advantages of using a cylinder are that the wall thickness is reduced to a minimum value, keeping maximal solid angle accessibility and keeping wall absorption of the incoming X-ray beam constant. The heat exchanger is a customized compact liquid-nitrogen (LN2) continuous-flow cryostat. LN2 is transferred from a storage Dewar through a vacuum-isolated transfer line to the heat exchanger. The sample is mounted on a molybdenum support on the heat exchanger, which is equipped with a BORALECTRIC heater element. The chamber versatility extends to the operating pressure, ranging from ultra-high vacuum (<10-10 mbar) to high pressure (up to 3 × 103 mbar). In addition, it is equipped with several CF ports to allocate auxiliary components such as capillary gas-inlet, viewports, leak valves, ion gun, turbo pump, etc., responding to a large variety of experiment requirements. A movable slits set-up has been foreseen to reduce the background and diffuse scattering produced at the beryllium wall. Diffraction data can be recorded either with a point detector or with a bi-dimensional CCD detector, or both detectors simultaneously. The system has been designed to carry out a multitude of experiments in a large variety of environments. The system feasibility is demonstrated by showing temperature-dependence grazing-incidence X-ray diffraction and conductivity measurements on a 20 nm-thick La0.7Ca0.3MnO3 thin film grown on a SrTiO3(001) substrate.
Publisher version (URL)https://doi.org/10.1107/S0909049513002598
Appears in Collections:(ICMM) Artículos
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