#################################################### # Prof. Waltraud M. Kriven # requesting 7 days, at minimum=7 days # beamline 33BM, Installation, testing, and calibration of curved image plate detector for in-situ high temperature powder x-ray diffraction # instrument 33BM-C fourc #################################################### # top:/home/www/beamtime-requests/req00843.txt # UNICAT Member Beam Time Request #843 # created Sat Aug 20 18:23:57 CDT 2005 #################################################### apsrun: 2005-03 beamline: 33BM collaboration: Yes collaborator_Jenia: ON collaborator_Paul: ON collaborator_Pete: ON contact: kriven@uiuc.edu days: 7 description: We have developed a 2-dimensional (2-D) Curved Image Plate Detector (CIPD) in collaboration with scientists at the Deutsche Elektronen Synchotron Laboratorium (DESY) in Hamburg, Germany and at the APS/UNICAT beam line. The detector has been configured for use with the Huber 4-circle diffractometer at 33BM-C beamline. In addition, we have also developed a quadrupole lamp furnace (QLF)) and demonstrated the feasibility of conducting in-situ high temperature x-ray diffraction (HTXRD) experiments to dynamically follow solid state phase transformations and crystallographic thermal expansion behavior of materials up to 2000 C in air. The QLF is used to create a hot zone in free air, and when used in conjunction with synchrotron radiation, it affords the unique possibility to conduct HTXRD experiments and gain in-depth understanding of the structure-property relationships at high temperatures. So far, we have successfully conducted these studies using a point detector. The use of 2-D detectors in powder diffraction experiments, although having several advantages over 1-dimensional (1-D) or point detectors, has not been explored for studying high temperature, phase transformation studies. The primary advantage of using a 2-D detector, in comparison to a point detector, is the increased rate at which data can be acquired. The CIPD will reduce the time for a given experiment by at least a factor of 30, and therefore will make it possible to study the kinetic aspects of material behavior. We foresee that QLF together with the CIPD will be an invaluable resource for conducting in-situ, time resolved, HTXRD investigations at high temperatures, such as phase transformations, chemical decomposition reactions, texturing, and growth of single crystals, etc. Such studies are not feasible with point detectors. During our last experimental run at the 33BM-C beamline, earlier in June 2005, we had successfully commissioned the CIPD and integrated it for operation with the existing instruments and software. We had commenced studies on calibration and operation of the CIPD using standard materials (such as SRM 660a and SRM 674), both in transmission and reflection geometries. Specific studies conducted included (a) determination of instrumental resolution, (b) evaluation of detector performance over a wide energy range of x-ray radiation, (c) assessment of ability of the detector to identify minor phase constituents, and (d) investigation of possibility to conduct reflection studies in asymmetric diffraction mode. In addition, we had also successfully incorporated a temperature controller for remote operation of the QLF. Software is being developed for conducting HTXRD studies by coupling the operation of the CIPD together with the QLF. Preliminary HTXRD studies were attempted to test the QLF+CIPD setup and included (a) thermal expansion measurements on standard materials (MgO and Pt), (b) phase transformation studies on candidate materials (DyNbO4 and Ta2O5) as a function of temperature and time, and (c) growth of single crystal 3:2 mullite from seed-templated polycrystalline mullite as a function of temperature and time. Analysis of the above studies has identified some key issues that need to be resolved, particularly to optimize the data collection and data quality using the CIPD, both in transmission and reflection geometries. These include, but are not limited to the following: (a) effect of data collection methodology on peak shapes, (b) optimal experimental protocol to maximize signal/noise in the collected datasets (c) understanding of instrumental resolution limitations, (d) identification of the source of sporadic shifts/errors in the collected datasets (e) evaluation of experimental configuration for conducting experiments in reflection mode, etc. We also plan to implement more robust and smart software, which will be self-correcting and optimized for improving signal/noise ratio of the collected dataset. At the same time each and every aspect of the experiment will be documented in separately created log-files. The CIPD+QLF setup will also be re-evaluated using some of the previously tested material systems. In addition, high temperature chemical oxidation kinetics of materials (such as ZrB2, and TiB2) will also be attempted to assess the potential of this setup for conducting time-resolved studies. We request more beamtime in order to understand, develop and realize the full potential of the CIPD, which is a very unique and dynamic novel detector system, for conducting forefront HTXRD investigations. equipment_required: None experiment: Installation, testing, and calibration of curved image plate detector for in-situ high temperature powder x-ray diffraction foreign_nationals: Prof. Waltraud M. Kriven (citizen of Australia) Dr. Pankaj Sarin (citizen of India) Wonki Yoon (citizen of South Korea) hazards: The HTXRD experiment uses a small, water-cooled, four-lamp furnace capable of 2000 deg C. There are no apparent hazards other than those normally associated with using high energy synchrotron radiation. The samples of the following types will be studied (a) small sintered rods (300-400 microns in diameter and < 2.5 cm in length), or (b) thin sintered plates (4mm (L) X 4mm (H) X 250 microns (W)), or (c) pellets (3mm (W) X 5mm (L) X 1 mm (H)), or (d) small quantities of ceramic oxide powders (<0.1gm). While the rod samples and the thin plate samples are intended for studies in transmission mode, with the x-rays passing through the sample, the pellets and powders are for experiments conducted in reflection geometry. All the samples are non-toxic. Similar experiments have been conducted at UNICAT 33BM-C before. The design and operation of the CIPD has been discussed in detail with the UNICAT scientists, considering all the safety requirements. All necessary precautions will be taken for successful operation of this detector. instrument: 33BM-C fourc instrument_other: minimumdays: 7 name: Prof. Waltraud M. Kriven nonmembers: submit: Submit unacceptable_dates: 11/06/2005 – 11/27/2005; 12/12/2005 – 12/23/2005 z34ID_details: #REMOTE_HOST: mach-200.mse.uiuc.edu #REMOTE_ADDR: 128.174.228.200 #CONTENT_LENGTH: 6627 #HTTP_REFERER: http://www.uni.aps.anl.gov/admin/unireq.html #HTTP_USER_AGENT: Mozilla/4.0 (compatible; MSIE 6.0; Windows NT 5.1; .NET CLR 1.1.4322)