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# Prof. Waltraud M. Kriven <kriven@uiuc.edu>
# 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
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# top:/home/www/beamtime-requests/req00772.txt
# UNICAT Member Beam Time Request  #772
# created Fri Apr 15 14:32:21 CDT 2005
####################################################

apsrun:
	2005-02

beamline:
	33BM

collaboration:
	Yes

collaborator_Jenia:
	ON

collaborator_Paul:
	ON

collaborator_Pete:
	ON

contact:
	kriven@uiuc.edu

days:
	7

description:
	Over the past one and a half years we have been collaborating with Technische Universitat Darmstadt, Germany together with UNICAT scientists to develop a 2-dimensional (2-D) Curved Image Plate Detector (CIPD). The detector has been configured for use with the Huber 4-circle diffractometer at 33BM-C beamline and is ready for testing. We propose to install, calibrate, and test the CIPD for conducting in-situ high temperature x-ray diffraction (HTXRD).

We have developed instrumentation (quadrupole lamp furnace (QLF)) and demonstrated the feasibility of conducting HTXRD experiments to dynamically follow solid state phase transformations and crystallographic expansion behavior of materials up to high temperatures. The QLF is used to create a hot zone in free air, enabling studies up to 2000 C in air. When used in conjunction with synchrotron radiation to do HTXRD experiments, it affords the unique possibility of gaining 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 properties. 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.

We anticipate the proposed experimentation to develop in two phases. In the first phase we propose to install and calibrate CIPD for powder x-ray diffraction experiments using standard reference materials, both in transmission and reflection geometries. In the second phase, tests will be conducted which will involve HTXRD studies (using QLF) on a number of materials and will aim at testing the QLF+CIPD setup for HTXRD experiments. These preliminary experiments include (a) thermal expansion measurements on standard materials (MgO, CeO2, and Pt), (b) phase transformation studies on candidate materials (DyNbO4, Ta2O5, and calcium phosphates) as a function of temperature and time, (c) high temperature chemical oxidation kinetics of materials (such as ZrB2, and TiB2), and (d) growth of single crystal 3:2 mullite from seed-templated polycrystalline mullite as a function of temperature and time.

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. Michael Knapp (citizen of Germany)
Dr. Pankaj Sarin (citizen of India)

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 are small sintered rods (300-400 microns in diameter and < 2.5 cm in length) or pellets (3mm (W) X 5mm (L) X 1 mm (H)) or small quantities of ceramic oxide powders (<0.1gm). While the rod samples are studied in transmission mode, with the x-rays passing through the sample, the pellets and powders are used 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 installation and successful operation of this detector.

instrument:
	33BM-C fourc

instrument_other:
	

minimumdays:
	7

name:
	Prof. Waltraud M. Kriven

new_request:
	ON

nonmembers:
	Dr. Michael Knapp, Technische Universitat Darmstadt, Germany

unacceptable_dates:
	

z34ID_details:
	


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