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    09 Barvinschi 32 35

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    The document presents a comparative study of different methods for precisely determining the lattice parameter of spinel MgAl2O4 from X-ray powder diffraction patterns, including an extrapolation method, Cohen method, and Rietveld method. Diffraction data was collected from MgAl2O4 powder samples prepared by different synthesis methods. The results show that the Rietveld method provides the most precise lattice parameter values with the lowest errors, followed by the extrapolation method, while graphics of Rietveld refinements for two samples are also shown. The study concludes that the Rietveld method yields the best results for lattice parameter determination in the medium diffraction angle range of 10° to 90°.

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    09 Barvinschi 32 35

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    The document presents a comparative study of different methods for precisely determining the lattice parameter of spinel MgAl2O4 from X-ray powder diffraction patterns, including an extrapolation method, Cohen method, and Rietveld method. Diffraction data was collected from MgAl2O4 powder samples prepared by different synthesis methods. The results show that the Rietveld method provides the most precise lattice parameter values with the lowest errors, followed by the extrapolation method, while graphics of Rietveld refinements for two samples are also shown. The study concludes that the Rietveld method yields the best results for lattice parameter determination in the medium diffraction angle range of 10° to 90°.

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    The document presents a comparative study of different methods for precisely determining the lattice parameter of spinel MgAl2O4 from X-ray powder diffraction patterns, including an extrapolation method, Cohen method, and Rietveld method. Diffraction data was collected from MgAl2O4 powder samples prepared by different synthesis methods. The results show that the Rietveld method provides the most precise lattice parameter values with the lowest errors, followed by the extrapolation method, while graphics of Rietveld refinements for two samples are also shown. The study concludes that the Rietveld method yields the best results for lattice parameter determination in the medium diffraction angle range of 10° to 90°.

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    © All Rights Reserved
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    15 views4 pages

    09 Barvinschi 32 35

    Uploaded by

    sensoham03
    The document presents a comparative study of different methods for precisely determining the lattice parameter of spinel MgAl2O4 from X-ray powder diffraction patterns, including an extrapolation method, Cohen method, and Rietveld method. Diffraction data was collected from MgAl2O4 powder samples prepared by different synthesis methods. The results show that the Rietveld method provides the most precise lattice parameter values with the lowest errors, followed by the extrapolation method, while graphics of Rietveld refinements for two samples are also shown. The study concludes that the Rietveld method yields the best results for lattice parameter determination in the medium diffraction angle range of 10° to 90°.

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    of 4

    Analele Universitii de Vest din Timioara

    Vol. XLIX, 2006


    Seria Fizic

    PRECISE LATTICE PARAMETER DETERMINATION OF SPINEL MgAl2O4 FROM


    X-RAY POWDER DIFFRACTION PATTERNS

    P. Barvinschi1, D.Tamas1, R. Baies2

    1
    West University of Timisoara, Faculty of Physics, Bvd. V.Parvan 4, 300223, Timisoara, Romania
    2
    National Institute of Electrochemistry and Condensed Matter, P.Andronescu 1, Timisoara, Romania

    Abstract
    A very precise knowledge of the lattice parameters of materials is important in solid-state
    investigations. In order to achieve high precision in lattice parameters measurements one can use the
    popular methods based on plotting the lattice parameter as a function of some extrapolation functions
    (Bradley-Jay, Nelson-Riley, etc) or applying the analytical Cohen method. Some new methods based on
    the Rietveld-type pattern-fitting approaches can also be used. In this paper we present a comparative
    study of these lattice parameter evaluation procedures. Diffraction data was recorded by Bragg-
    Brentano X-ray diffractometry, using a set of MgAl2O4 powder samples presenting different
    crystallinities. For the Rietveld-type analysis we used the FullProf programs package. Our results are
    important for the studies involving systems of particles in the medium range diffraction angles (2
    between 10o 90o).
    Keywords: lattice parameter, powder diffraction.

    1. Introduction
    In the last few years, the continuously growing demand for new and advanced
    materials with well-defined structures and properties has brought into light new and improved
    methods for quantitative analysis of X-Ray diffraction patterns.
    The subject of the present work is the precise determination of the lattice parameter
    for the cubic spinel structure of MgAl2O4 using different methods: one using an extrapolation
    function, another using the Cohen method and the third is the Rietveld method for whole
    pattern fitting.

    2. Lattice parameter determination methods


    For the extrapolation method [1] the lattice parameter, ao, is computed for each line of
    the pattern and is plotted against a so called extrapolation function. A straight line should

    32
    result and the true value of the lattice parameter can be found by extrapolating this line to
    =90. This so called extrapolation functions are functions of , like cos2, sin2, cos2/sin,
    k(cos2/sin+cos2/).
    The Cohen method [1] consist from two sets of equations,
    A 2 + C = sin 2
    (1)
    A + C 2 = sin 2

    where A = 2 / 4a 02 , = (h 2 + k 2 + l 2 ) and = 10 sin 2 2 . With the two sets of equations we


    can find the A and C values. Once the value of A is found, ao can be calculated. The constant
    C is related to the amount of systematic error involved.
    The Rietveld method [2] is more complicated and sometimes difficult to use but, as
    our comparative study is about to show, it yields the best results. The method is a profile
    fitting technique involving the simulation of the diffraction pattern, based on a structural
    model. The calculated intensities are fitted to the observed intensities, which is achieved by
    minimization of the sum of the squares

    [( I )
    i obs ( I i ) calc
    sc
    ( I i ) b ]2 (2)
    i

    Although the principles behind the Rietveld profile refinement method are rather simple, the
    use of the technique requires some expertise.

    3. Experimental and results


    Diffraction data were recorded in the medium range diffraction angles (2 between 10o
    90o) by Bragg-Brentano X-Ray diffractometry, using a Bruker D8 Advance equipment
    (CuK radiation, 40 kV, 30 mA, Ni filter or graphite monocromator).
    The DiffracPlus software package was used for data acquisition and peak search. Two
    home-made computer programs were used for the determination of the lattice parameter by
    the extrapolation and Cohen methods, respectively. For the Rietveld-type analysis we used the
    FullProf programs package [4].
    A set of MgAl2O4 powder samples presenting different crystallinities was used. They
    were prepared by three different methods [3]: sol-gel, combustion, and thermal conversion,
    respectively.
    The average size of the cell parameter for these samples is presented in Table 1.
    Although the calculated values are quite similar to those from the references for well
    crystallized spinel (ao=8.0831 , JCPDS file 21-1152), it is obvious that the extrapolation and

    33
    Rietveld methods give better results, with a plus of reproducibility and precision for the last
    one.

    Table 1. Lattice parameter calculated for the MgAl2O4 powders, using different methods
    Lattice parameter amed ()
    Sample Cohen Extrapolation
    Rietveld
    amed C cos2/sin
    1a 8,121 0,003 8,086 0,002 8,0939 0,0005
    2 8,112 0,000165 8,101 0,037 8,0772 0,0021
    3 8,097 0,000054 8,086 0,004 8,0909 0,0007
    3bis 8,088 0,000095 8,092 0,002 8,0935 0,0005
    4 8,054 0,000262 8,093 0,020 8,0972 0,0026
    6 8,093 0,000033 8,082 0,005 8,0951 0,0008
    52 8,124 0,0003 8,089 0,001 8,0926 0,0004

    (a) (b)
    Fig. 1 Rietveld refinement results for samples 6 (a) and 52 (b) respectively (see text and
    Table 1 for details).

    As an example of the Rietveld method, in the figures 1.a-b we present the graphics
    resulted after refinement with Fullprof software package of the powder diffraction patterns for
    the samples 6 and 52. In these figures the grey dots represent the experimental data points, the
    black line between those points represents the calculated pattern using a model provided by
    user, the black lines under the peaks represent the calculated Bragg positions and the dark-
    grey line under the two patterns represents the difference between calculated and observed
    patterns.

    34
    The correlation between the synthesis method and the lattice parameter for the spinel
    samples will be presented elsewhere.

    4. Conclusions
    Using the Rietveld method in the medium range diffraction angles (2 between 10
    and 90) the results obtained for the lattice parameter determination are the best. The error
    calculated is lower and, as we have observed, the reproducibility of the results is also
    increased using the Rietveld method. Good results are also obtained using the extrapolation
    method.

    References:
    [1] H.P.Klug, L.E.Alexander, X-ray Diffraction Procedures, 2nd ed., New York (1974)
    [2] L.S.Zevin, G.Kimmel, Quantitative X-Ray Diffractometry, Springer-Verlag, New York
    (1995)
    [3] C.Pacurariu, I.Lazau, Z.Ecsedi, R.Lazau, P.Barvinschi, G.Marginean, The IX-th
    Conference & Exhibition of the European Ceramic Society, June 19-23, 2005, Portoroz,
    Slovenia
    [4] http://www-llb.cea.fr/fullweb/fp2k/fp2k.htm

    35

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