Single-Crystal X-ray Diffraction
CICECO has currently one single-crystal X-ray Diffractometer from Bruker, model D8 Quest, 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.
A second single-crystal instrument, RIGAKU XtaLAB Synergy-i, equipped with an X-ray microsource allow the screening and full structure elucidation of even smaller single crystals, thus opening the technique to a whole new set of functional materials and possible external services.
Powders and films
CICECO has X-ray powder and film (currently unavailable) 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 77 K and 620 K in powders and solids 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 analyzed, namely crystallographic texture, residual stresses, micro-deformation and average crystallite size;
Oriented films are studied using high resolution diffraction (reciprocal space maps, "rocking curves", reflectometry, "in plane" measurements).
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 -PDF4+
UA/CICECO/DQ and DEMAC – Panalytical Empyrean 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
Identification of crystalline phases by comparison with the ICDD -PDF4+ database, followed by Rietveld refinement for compounds with .cif files published
UA/CICECO/DQ e DEMAC - Panalytical Empyrean e X’Pert Pro
Diffraction of powders in transmission (between Kapton, Mylar or acetate sheets or in a capillary) and in reflection (Bragg-Brentano geometry)
Acquisition of diffractograms for further analytical treatment, at room temperature
UA/CICECO/DQ - Panalytical Empyrean
Powder diffraction – in situ (from -193ºC to 350ºC in vacuum and air)
Acquisition of diffractograms for further analytical treatment
UA/CICECO/DQ Panalytical Empyrean
Powder diffraction – in situ (from 25ºC to 1300ºC 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 -PDF4+ database on UA/CICECO/LCA and DEMAC thin films
UA/CICECO/LCA and DEMAC – Philips X’pert MRD and Panalytical X’Pert Pro3
Film diffraction in in-plane mode, ambient temperature
Determination of cell parameters, crystallite size and unit cell deformations of oriented films
UA/CICECO/LCA - Philips X’pert MRD
Crystallographic textures
Analysis of pole figures of film and solid materials at room temperature
UA/CICECO/LCA - X’per MRD
Determination of film thicknesses (1nm to about 400nm)
Room temperature x-ray reflectometry
UA/CICECO/LCA - Philips X’pert MRD
Analysis of lattice parameters, deformations, relaxation, epitaxy of films
Analysis of symmetrical and asymmetrical maps of the reciprocal space obtained at room temperature
UA/CICECO/LCA - Philips X’pert MRD
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 have been received via LCA, in accordance with the request model and the rules described on the website and the respective forms
Filipe A. Almeida Paz
Scientific Coordinator
Filipe A. Almeida Paz is a senior researcher of the University of Aveiro working on X-ray crystallography and the development of new crystalline hybrid materials (Metal-Organic Frameworks and Coordination Polymers). Filipe is one of the founding members of the Chemical Crystallography group at the Portuguese Chemical Society, is one the national representatives at the International Union of Crystallography and holds the position of co-Editor of Acta Crystallographica – Section C.
Paula Brandão
Single-Crystal X-ray Diffraction Laboratory Researcher
Rosário Soares
Powders and Films Laboratory Technician
Paula belongs to technical staff of the single crystal X-ray diffraction laboratory, responsible for its maintenance, as well as the training of the new users, contributing to the knowledge of the students not only to handle the single crystal X-ray machine but also in solving structures using different methodologies.
Marco Oliveira
Powders and Films at room and hight temperature Laboratory Technician
Phone
+351 234 370 200 (Single-Crystal X-ray Diffraction)
+351 234 401 533 (Powders and films @ LCA)
+351 234 378 184 (Powders and films @ DEMaC)
Email
pbrandao@ua.pt (Single-Crystal X-ray Diffraction)
rosarios@ua.pt (Powders and films @ LCA)
mpo@ua.pt (Powders and films @ DEMaC)
Rooms
15.1.8 (Single-Crystal X-ray Diffraction
14.1.2 (Powders and films @ LCA)
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 copper tube (bragg brentano theta theta, grazing angle xrd, “in situ” measurements up to 1300oC)
Philips X’pert MRD