Single-Crystal X-ray Diffraction
CICECO has X-ray powder and film diffractometers with which it is possible to carry out the analysis of crystalline materials for research groups inside and outside the UA and industry:
Crystalline phases and phase transitions that occur between -190º C and 1300ºC in powders can be identified;
Crystalline phases can be identified in polycrystalline films using grazing angle and film thicknesses are determined by reflectometry;
Microstructural aspects of materials can be analysed, residual stresses, micro-deformation and average crystallite size;
The powder and film x-ray laboratories collaborate with UA research groups to provide results for indexing, determination of crystal structures and refinement of structure parameters.
In addition to analytical services, the X-ray diffraction laboratory collaborates in teaching disciplines for the undergraduate, masters and doctoral programs at the U.A. providing contact and practical knowledge of the XRD technique to the students who attend them
Webpage LCA Webpage DEMaCAbout X-Ray Diffraction Facility
Services
Short description
Equipments
Diffraction of polycrystalline materials – phase identification at room temperature
Identification of crystalline phases by comparison with the ICDD – PDF45+
UA/CICECO/DQ and DEMAC – Panalytical Empyrean, Rigaku Smartlab and X’Pert Pro (automatic sample feeder)
Diffraction of polycrystalline materials – phase quantification, determination of lattice parameters, crystallite size and lattice deformations at room temperature and in situ
Identification of crystalline phases by comparison with the ICDD – PDF4+ database, followed by Rietveld refinement for compounds with .cif files published
UA/CICECO/DQ and DEMAC – Panalytical Empyrean, Rigaku Smartlab and X’Pert Pro
Diffraction of powders in transmission (between Kapton, Mylar or acetate sheets or in a capillary)
Acquisition of diffractograms for further analytical treatment, at room temperature
UA/CICECO/DQ – Panalytical Empyrean and Rigaku Smartlab
Powder diffraction – in situ (from ?193°C to 350°C in vacuum and air)
Acquisition of diffractograms for further analytical treatment
UA/CICECO/DQ – Panalytical Empyrean
Powder diffraction – in situ (from 25°C to 1300°C in vacuum, air, and inert gas)
Acquisition of diffractograms for further analytical treatment
UA/CICECO/DEMAC – Panalytical X’Pert Pro3
Grazing angle film diffraction, room temperature
Identification of crystalline phases by comparison with the ICDD – PDF5+ database on UA/CICECO/DEMAC X’Pert Pro3 and Rigaku SmartLab
UA/CICECO/DEMAC – Panalytical X’Pert Pro3
Determination of film thicknesses (1 nm to about 200 nm)
Room temperature X-ray reflectometry
UA/CICECO/DEMAC – Rigaku Smartlab
CICECO researchers (including students and professor) have direct access to the instrument through the available technical supporting staff. Please use the contacts below.
External services are received via CDTM
Rosário Soares
Facility Coordinator
Paula Brandão
Single-Crystal X-ray Diffraction Laboratory Researcher
Rosário Soares
Powders and Films Laboratory Technician
Marco Oliveira
Powders and Films at room and high temperature Laboratory Technician
Phone
+351 234 370 200 (Single-Crystal X-ray Diffraction)
+351 234 378 184 (Powders and films @ DEMaC)
Email
pbrandao@ua.pt (Single-Crystal X-ray Diffraction)
rosarios@ua.pt (Powders and films @ DQ)
mpo@ua.pt (Powders and films @ DEMaC)
Rooms
15.1.8 (Single-Crystal X-ray Diffraction)
14.1.2 (Powders and films @ DQ)
9.1.22 (Powders and films @ DEMaC)
Instruments
Bruker D8 Quest
Diffractometer equipped with a molybdenum X-ray source, a TRIUMPH monochromator and a PHOTON III detector. The system is coupled to an Oxford Instruments Cryostream capable for data collection between ca. -173 ºC and 120 ºC. The instrument allows a quick screening of single-crystals and the selection of the most suitable for a full data collection to permit structural elucidation.
RIGAKU XtaLAB Synergy-i
A single crystal X-ray diffractometer with a microfocus sealed tube X-ray source for crystal detailed structure determination.
A single crystal X-ray diffractometer equipped with a Mo Kα (λ = 0.71073 Å) PhotonJet-i micro source and a HyPix3000 detector for crystal structure determination. The instrument is controlled by the CrysAlisPro software (Y. Oxford Diffraction Ltd, England, 2022, CrysAlis PRO, Rigaku V1.171.142.173a) and it is equipped with an Oxford Cryosystems Series 800 cryostream. Diffraction images are processed using CrysAlisPro software. Data can be corrected for absorption using the multi-scan absorption correction with spherical harmonics implemented in the SCALE3 ABSPACK scaling algorithm.
Panalytical X’Pert Pro3
X-ray diffraction with a Cu tube (Bragg brentano theta-theta, grazing angle diffraction, Pixel 1D detector and Anton-Paar chambers for in situ measurements up to 1300ºC
Rigaku Smartlab
X-ray diffraction with a Cu tube (bragg brentano theta theta, grazing angle xrd and reflectometry
Panalytical Empyrean
X-ray diffraction with a copper tube (Kα radiation) in Bragg Brentano geometry and transmission mode on capillary, in situ measurements from -190ºC to 350ºC, under air and vacuum