University of the Basque Country UPV/EHU Science and technology faculty Edificio CD3 Bº Sarriena, s/n 48940 Leioa (Bizkaia)
The X-ray Service may used by researchers from University Colleges, Technology Centres and Companies, etc. Routine and special experiments can be carried out, in addition to analyses of results. The Service Personnel can in any event advise you about the most suitable experiments and conditions for each problem. Access to the unit of X-rays: Molecules and Materials involves meeting the requirements set forth in the Protocol for access to SGIker and the services it provides.
The General X-ray Service of the University of the Basque Country/EHU attempts to provide support for basic and applied research in, among others, the different areas of knowledge of Geological Science, Chemistry, Materials Science, Aeronautics, Pharmacy, Biochemistry, Archaeology, Palaeontology, Anthropology and Environmental Science, in addition to helping to provide a service in the fields of Construction, Mining Prospecting and Civil Engineering. Researchers may also access the service from the Basque Network of Science and Technology, and it is available to other researchers outside the UPV/EHU, and other public and private institutions - both national and international. Integrated in the General Service of X-ray Analysis, the Unit Molecules and Materials, provides the structural study of organic and inorganic materials in the form of single crystals or polycrystalline sample, under a wide range of conditions. The performance of this unit covers all aspects of the study of crystal structure from diffraction data: the selection and installation of the sample, previous studies of symmetry, diffraction data collection, the resolution or structural identification and the analysis of results. The available equipment also enables structural studies starting from diffraction data of polycrystalline materials. This technique allows us to identify the crystalline phases present in the sample without destroying it, allowing you to recover the material without deterioration. It is possible to characterize, in a wide variety of materials, his crystalline structure, or the presence of texturin or residual stresses, material fatigue, etc., These studies were performed by analyzing the profile of diffractogram using, in the cases that require it, the Rietveld method. The X-Ray Service: Molecules and Materials Unit supports basic and applied research through scientific and technical advice and the use of a high-performance infrastructure in materials analysis by X-ray diffraction, with applications in many areas knowledge.
Monocrystal sample: - Visual selection and preparation (assembly) of the crystal. The samples are accepted as previously filtered crystals or in solution, with the latter being the preferable option in many cases. - Prior quality measures and preliminary data-taking, the moment when the monocrystal to be measured is selected, the unit cell parameters are determined, along with its symmetry (preliminary). When necessary, the ICSD and CSD crystallographic data bases are consulted with this information to determine whether the crystalline phase in question has already been determined and published in international data bases. If that is not the case, the preliminary data taking allows the most appropriate diffractometer to be selected and the measurement conditions be optimized: temperature, angular range, time,… - Diffraction data collection. The data taking is performed at 100K by default, except in those cases when the user requests the contrary, or the preliminary data indicate the formation of an intersecting twin, non-desired phase transition, crystal degradation or any other non-desired effect when the temperature is reduced. In any case, the data taking can be performed at a wide range of temperatures (10-600K) and can be performed at different temperatures for phase transition studies. - Data processing. The process can end here if the user has sufficient knowledge to solve and refine the structure. - Structural resolution, tuning and results presentation (report). The results obtained are sent to the users in the form of reports, graphs and/or tables, always facilitating the source data collected by the diffractometer, along with information relating to the equipment user,measurement conditions, etc. A comprehensive CIF file, ready to be entered in the database and/or for publication, is delivered. Polycrystalline Sample: - Diffractogram measuring and processing: the specific diffractometer software is used to prepare the measurement programs as per the needs raised by the users. - Phase identification: the phases are identified using specific software, combined with the ICDD PDF2-4 database, for the users that so require this service. - Data processing for crystallinity analysis, crystalline domain size and efforts. The data processing is performed both at the level of individual diffraction maxims and by means of full diffraction diagram processing. - Quantitative analysis: by means of the theoretical simulation of the diffraction diagrams using full profile tuning with structural model both of pure phases and for compound mixtures. This methodology requires a complex and intense data processing task, along with the registration of X-ray diffraction diagrams in high-resolution polycrystalline sample. - Data presentation: the results obtained are sent to the users in the form of reports, graphs and/or tables, always facilitating the source data collected by the diffractometer. The users are also given information on the equipment users, measurement conditions, methodology followed to prepare samples, etc. - Training by means of specific courses. Educational support for various degrees and Master’s degrees.
Huber, model 670. Equipped with Image Foil detection system. Can operate using Debye or transmission geometry.
Equipped with two Theta-2Theta goniometers that operate independently, share a single source of x-rays and are equipped with secondary monochromator. One goniometer is used for high temperature measurements (Anton Paar HTK16 camera). The second goniometer operates with an automatic 15-position charger.
Enables work to be carried out using flat samples (transmission) or with hairs. Equipped with a detector that is sensitive to the 6º aperture position. Its measured interval starts at 0.6º2Theta.
Operates with Theta-2Theta geometry. Equipped with a Vårio (CuKa 1) primary monochromator and an SolX solid detector with energy discrimination optimized for such radiation. Can work with automatic charger of flat samples, transmission geometry or samples in hair.
Operates with Theta-Theta geometry. Used for non-environmental measurements at high temperature (HTK2000 camera) or low temperature (MRI Wide Range camera). Equiiped with a Vantec ultra-fast detector with maximum 6º aperture.
Four-circle Kappa diffractometer equipped with a CCD Shappire 2 detector and an Enhance device that increases the x-ray intensity given off by the tube. Equipped with a Helojet low temperature system (from 15K) and high temperature RKD Hotjet system (up to 259ºC).
Two-circle diffractometer equipped with imaging plate detector of 340 mm in diameter and great signal/noise ratio. The possibility of rotating the complete goniometer enables very high Bragg angles to be accessed (up to 137º in 2Theta). Its geometry enables devices to be adapted in order to vary the environmental conditions of the measurements.
Precesión (Huber) and Weissenberg (Stoe). Equipped with low temperature accessory up to 80K.
Sequential wavelength dispersive spectrometer. Equipped with automated 30-positiion sample changer. Also equipped with 8 analyzer crystals and flow and sparkle detectors, being possible to analyse from fluorine.
Permits specific analysis of minerals and materials in polished section. Configured with four TAP, LIF, PET and PC1 crystal analyzers for analysis of both light and heavy and larger elements and traces.
- HERZOG HSM100 Widia disc oscillating mill.
- HERZOG HTP 40 mechanical press.
- PERL'X3 bead machine.
- Emitex metallyzer (carbon).
- Struers Planopol-V and DP10 polishers.
- Kubota KS-800 and 8410 centrifuges
- Olympus SZX 16 magnifying glass.
- Olympus KL1500 LCD cold light source.
- Oxford Cryostream low temperature system.
Operates using Theta-2Theta geometry and is equipped with secondary monochromator, variable opening diffraction aperture and 35 sample charger.