Accurate determination and correction of the lattice parameter of LaB6 (standard reference material 660) relative to that of Si (640b)

被引:17
作者
Chantler, C. T. [1 ]
Rae, N. A. [1 ]
Tran, C. Q. [1 ]
机构
[1] Univ Melbourne, Sch Phys, Parkville, Vic 3010, Australia
关键词
D O I
10.1107/S0021889806054094
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
X-ray powder diffraction and synchrotron radiation have been used to determine the lattice parameter of the NIST standard reference material (SRM 660) LaB6 as 4.156468 angstrom with an accuracy of 12 parts per million (p.p.m.), calibrated relative to the lattice parameter of the Si powder standard [a(0) = 5.430940 (11) angstrom, Si 640b]. A discrepancy of 0.00048 (5) angstrom, or nine standard deviations from the NIST reference, is observed between the currently accepted lattice spacing of LaB6 and the measured value. Twelve different measurements of the lattice parameter were made at beam energies between 10 and 20 keV. The observed discrepancy in the lattice parameter is consistent for the different energies used. The absolute values of the mean difference between the measured and calculated 2 theta centroids, \(delta 2 theta) over bar\, are highly consistent, between 0.0002 and 0.0004 degrees for energies from 5 to 14 keV, and between 0.0005 and 0.0008 degrees for energies from 15 to 20 keV. In order to determine the peak positions with high precision, account must be taken of the observed peak asymmetry. It is shown that significant asymmetry is due to peak broadening and must be taken into account in order to determine accurate peak locations and lattice spacings. The approach shows significant advantages over conventional analysis. The analysis of peak broadening is compared with models used in Rietveld analysis.
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页码:232 / 240
页数:9
相关论文
共 18 条
[1]   THE RIETVELD METHOD IN NEUTRON AND X-RAY-POWDER DIFFRACTION [J].
ALBINATI, A ;
WILLIS, BTM .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 1982, 15 (AUG) :361-374
[2]   Structure of the quaternary alloy Zn0.6Mn0.4In2S4 from synchrotron powder diffraction and electron transmission microscopy [J].
Avila-Godoy, R ;
Mora, AJ ;
Acosta-Najarro, DR ;
Delgado, GE ;
López-Rivera, SA ;
Fitch, AN ;
Mora, AE ;
Steeds, JW .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2006, 39 :1-5
[3]   THE AUSTRALIAN DIFFRACTOMETER AT THE PHOTON FACTORY [J].
BARNEA, Z ;
CREAGH, DC ;
DAVIS, TJ ;
GARRETT, RF ;
JANKY, S ;
STEVENSON, AW ;
WILKINS, SW .
REVIEW OF SCIENTIFIC INSTRUMENTS, 1992, 63 (01) :1069-1072
[4]   CHOICE OF COLLIMATORS FOR A CRYSTAL SPECTROMETER FOR NEUTRON DIFFRACTION [J].
CAGLIOTI, G ;
PAOLETTI, A ;
RICCI, FP .
NUCLEAR INSTRUMENTS & METHODS, 1958, 3 (04) :223-228
[5]   Precise measurement of the lattice spacing of LaB6 standard powder by the x-ray extended range technique using synchrotron radiation -: art. no. 042101 [J].
Chantler, CT ;
Tran, CQ ;
Cookson, DJ .
PHYSICAL REVIEW A, 2004, 69 (04) :042101-1
[6]   Measurement of the x-ray mass attenuation coefficient of copper using 8.85-20 keV synchrotron radiation [J].
Chantler, CT ;
Tran, CQ ;
Barnea, Z ;
Paterson, D ;
Cookson, DJ ;
Balaic, DX .
PHYSICAL REVIEW A, 2001, 64 (06) :15
[7]   A FUNDAMENTAL PARAMETERS APPROACH TO X-RAY LINE-PROFILE FITTING [J].
CHEARY, RW ;
COELHO, A .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 1992, 25 (pt 2) :109-121
[8]   Calculation of absolute intensities from X-ray imaging plates [J].
Cookson, DJ .
JOURNAL OF SYNCHROTRON RADIATION, 1998, 5 :1375-1382
[9]   LATTICE-PARAMETER DETERMINATION FOR POWDERS USING SYNCHROTRON RADIATION [J].
HART, M ;
CERNIK, RJ ;
PARRISH, W ;
TORAYA, H .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 1990, 23 :286-291
[10]   SYNCHROTRON X-RAY-POWDER DIFFRACTION [J].
HASTINGS, JB ;
THOMLINSON, W ;
COX, DE .
JOURNAL OF APPLIED CRYSTALLOGRAPHY, 1984, 17 (APR) :85-95