Hostname: page-component-78c5997874-dh8gc Total loading time: 0 Render date: 2024-11-13T09:27:44.186Z Has data issue: false hasContentIssue false
  • English
  • Français

A beryllium dome specimen holder for XRD analysis of air sensitive materials

Published online by Cambridge University Press:  29 February 2012

Mark A. Rodriguez ,
Timothy J. Boyle ,
Pin Yang  and
Damon L. Harris
Mark A. Rodriguez*
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Timothy J. Boyle
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Pin Yang
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
Damon L. Harris
Affiliation:
Brush Wellman Electrofusion Products, Fremont, California 94538-6346
*
a)Author to whom correspondence should be addressed. Electronic mail: [email protected]
Get access Rights & Permissions [Opens in a new window]

Abstract

A specially designed specimen holder employing a beryllium dome has been fabricated for collection of X-ray diffraction (XRD) data from highly reactive materials. The specimen holder has a robust O-ring type seal (<10−9Torr) and no observed intensity artifacts in the 1° to 150° 2θ range. The design also minimizes specimen displacement errors and allows for analysis of both powders and bulk specimens (i.e., pellets). The simple design makes for straightforward assembly of the holder within the confines of a glove box. XRD analysis of hygroscopic LaBr3 powders collected with this holder are suitable for Rietveld structure refinement, yielding unit cell lattice parameters of a=7.9703(6) Å and c=4.5122(6) Å; cell volume=248.44(6) Å3; Rp=7.70%.

Keywords

berylliumreactiveair-sensitiveBeDXRD
Type
X-Ray Diffraction
Information
Powder Diffraction , Volume 23 , Issue 2 , June 2008 , pp. 121 - 124
Copyright
Copyright © Cambridge University Press 2008

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Belin, R. C., Valenza, P. J., Reynaud, M. A., and Raison, P. E. (2004). “New hermetic sample holder for radioactive materials fitting to Siemens D5000 and Bruker D8 x-ray diffractometers: Application to the Rietveld analysis of plutonium dioxide,” J. Appl. Crystallogr. JACGAR 37, 1034–1037.Google Scholar
Boyle, T. J., Ottley, L. A. M., Sewell, R. M., Rodriguez, M. A., Alam, T. M., McIntyre, S. K., Yang, P., Baros, C. M., and Sanchez, M. R. (2008). “Facile synthesis of structurally characterized lanthanide/group 3 halide hydrates, halides, and solid-solution of mixed lanthanide halide materials,” Inorg. Chem. (submitted).Google Scholar
Buckner, C. and Varlashkin, P. (2000). “Cover to provide an inert atmosphere for XRD sample changers,” Powder Diffr. PODIE2 15, 101–103.CrossRefGoogle Scholar
Buhrke, V. E., Jenkins, R., and Smith, D. K. (Eds.) (1998). A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis (Wiley, New York), pp. 242–243.Google Scholar
Cullity, B. D. (1978). Elements of X-ray Diffraction, 2nd ed. (Addison-Wesley, Reading, Massachusetts), p. 13.Google Scholar
Ewen, D. A., Wirth, F. W., and Hallock, R. B. (1981). “Windows for x-ray diffraction experiments,” Rev. Sci. Instrum. RSINAK 10.1063/1.1136449 52, 71–74.Google Scholar
ICDD (2005). “Powder diffraction file,” International Centre for Diffraction Data, edited by McClune, Frank, 12 Campus Boulevard, Newtown Square, PA19073–3272.Google Scholar
Jenkins, R. and Snyder, R. L. (1996). Introduction to X-Ray Powder Diffractometry (Wiley, New York), pp. 249–250.CrossRefGoogle Scholar
Krämer, K., Schleid, T., Schulze, M., Urland, W., and Meyer, G. (1989). “Three bromides of lanthanum: LaBr2, La2Br5, and LaBr3,” Z. Anorg. Allg. Chem. ZAACAB 10.1002/zaac.19895750109 575, 61–70.Google Scholar
Larson, A. C. and Von Dreele, R. B. (2000). General Structure Analysis System (GSAS) (Report LAUR No. 86-748). Los Alamos National Laboratory, Los Alamos, New Mexico.Google Scholar
Rink, W. J., Mathias, H. G., and Schlenoff, J. B. (1994). “Hermetic sample housing for x-ray diffraction studies,” J. Appl. Crystallogr. JACGAR 10.1107/S0021889893013822 27, 666–668.CrossRefGoogle Scholar
Semenova, L. I., Junk, P. C., Skelton, B. W., and White, A. H. (1999). “Structural systematics of rare earth complexes. XVI (‘maximally’) hydrated rare earth(III) bromides,” Aust. J. Chem. AJCHAS 52, 531–538.Google Scholar
Strachan, D. M., Schaef, H. T., Schweiger, M. J., Simmons, K. L., Woodcock, L. J., and Krouse, M. K. (2003). “A versatile and inexpensive XRD specimen holder for highly radioactive or hazardous specimens,” Powder Diffr. PODIE2 10.1154/1.1523078 18, 23–28.CrossRefGoogle Scholar
Toby, B. H. (2001). “EXPGUI, a graphical user interface for GSAS,” J. Appl. Crystallogr. JACGAR 10.1107/S0021889801002242 34, 210–213.Google Scholar