ࡱ> 9;8U@!bjbj*& &&&& 8. $R r ( .  $+R}9  && I}}}&R  }}}x" f HA_ T_0 &&&& 0+ "}M i   D^ Standard Reference Materials for Powder Diffraction L. G. Martinez1*, A. S. A. Galvo1, C. J. Rocha1, M. T. D. Orlando2, H. P. S. Corra3, F. F. Ferreira4, C. O. Paiva-Santos5 1- Instituto de Pesquisas Energticas e Nucleares, SP, Brazil 2- Universidade Federal do Esprito Santo, Vitria, ES, Brazil 3- Universidade Federal do Mato Grosso do Sul, Campo Grande, MS, Brazil 4- Laboratrio Nacional de Luz Sncrotron, Campinas, SP, Brazil 5- Instituto de Qumica - UNESP, Araraquara, SP, Brazil The calibration and alignment of powder diffraction equipments is generally performed by means of measurement of standard samples. These samples must have very well defined cell parameters and high stability. Additionally, for neutrons and synchrotron radiation experiments it is also necessary the precise determination of energy or wavelength, which can also be made using a standard samples. For the determination of crystallite sizes and microstrains it is usual to determine the instrumental parameters, both in conventional laboratory and synchrotron diffractometers. In this case, besides having the crystal structure and cell parameters very well defined, it is imperative that the standard sample presents high crystallite size and low (or none) microstrains, in order to obtain diffraction peaks broadening due exclusively to instrumental factors. For this purpose normally are used the NIST Standard Reference Materials for Powder Diffraction [1] like Al2O3, Si, LaB6 etc. In order to have an alternative source of standard reference materials and attend the demand of XRD research community, we are working in the development of a set of materials that attempt to the requirements to be used as powder diffraction standards. We are working in the production and certification of standard samples of -Al2O3, Y2O3, among others. In this work are presented results of these standard samples, measured in conventional XRPD equipment, NPD (IPEN Neutron Powder Diffractometer) and synchrotron (D10B-XPD-LNLS). The experimental data were analyzed by Rietveld refinement [2] in order to determine cell parameters, crystallite size and microstrain, and are compared to the NIST LaB6, Al2O3 and Si standards. The results show that our standard reference materials fulfill the requirements to be used as powder diffraction standards. Other materials are being studied as possible candidates for standard samples for specific applications. Keywords: Powder diffraction, standard reference materials, Rietveld refinement, crystallite size, microstrain. [1] NIST, May 14, 2008, 3456DFMPWXYefghxyx ŶuiZRhqhq6h zh zCJaJmHsHhqCJaJmHsHh^*CJaJmHsHhr@dCJH*aJmHsHhr@dCJaJmHsHhI_nCJaJmHsHhqhqCJH*aJmHsHhqhqCJaJmHsHhqh z5CJaJmH sH h z5CJaJmH sH hq5CJaJmH sH hqhq5CJaJmH sH 4560 x  vw xgdq <`gd z<gdqgd@ $^a$gdq$a$gd z$a$gdq!!!x V [ { | ~  Nk  ,  vwy{|}~ŽŽŽűťťťŽŽŽŽřťťťťŽűťŽh5Sh5SH*mH sH hqh5SmH sH h5SOJQJmH sH h5ShqH*mH sH h5ShqH*mH sH h5SmH sH hqhqmH sH hqh zmH sH hL;YmH sH hqh:-6mHnHsH hqhq6mHnHsH 3 uvw  R S T !!!P!Q!V!W!yui^SSS^^hqhj&mH sH hj&hj&mH sH hj&hj&6mH sH hUhqhqmHsHh5Shj&h5S0JOJQJ#jhj&h5SOJQJUhj&h5SOJQJjhj&h5SOJQJUUhqhj&h:-mH sH hj&hqmH sH h zmH sH hj&mH sH h5SmH sH hqhqmH sH   HYPERLINK "http://ts.nist.gov/measurementservices/referencematerials/index.cfm" http://ts.nist.gov/measurementservices/referencematerials/index.cfm [2] H. M. Rietveld, J. Appl. Cryst.2 (1969) 65-71 Acknowledgements: Work supported by the Brazilian Agency CNPq (proj. # 480337/2007-1) and Brazilian Synchrotron Light Laboratory LNLS. *  HYPERLINK "mailto:lgallego@ipen.br" lgallego@ipen.br     19a ABCr X!Y!!!!!!!!!!!!!!!!!!!!!!$a$gd zgdj&W!X!Y![!\!!!!!!!!!!!!!!!!!!!!!!!!!!ٺ寧{n_[[h:-h:-6CJOJQJmHsHh:-56CJmHsH%h"Rh"R56CJH*aJmHsHh"R56CJmHsHh:-mHsHh,xjh,xUhUh zmHsHhD(h z0JmH sH #jhD(h zUmH sH jh zUmH sH h zmH sH hj&mHsHhj&hj&mH sH (&P . A!"#P$P%DyK Dhttp://ts.nist.gov/measurementservices/referencematerials/index.cfmyK http://ts.nist.gov/measurementservices/referencematerials/index.cfmyX;H,]ą'cDyK lgallego@ipen.bryK Hmailto:lgallego@ipen.bryX;H,]ą'c8@8 Normal_HmH sH tHN@N Ttulo 1$<@&5CJKHOJQJ>@> Ttulo 2$@& 5OJQJ>A@> Fonte parg. padroXiX  Tabela normal :V 44 la ,k, Sem lista :@: Cabealho  !LOL @ body text$P`a$ CJOJQJJOJtitle$a$5CJ_HmHnHsHtHu\O"\ affiliation$a$#CJOJQJ_HmHnHsHtHuLO2L name$$<@&a$;CJKHOJQJFOBF chapter  75CJOJQJHORH no indent text @`4 @b4 Rodap  !8)@q8 Nmero de pginaTYT Estrutura do documento-D OJQJXZ@X Texto sem formataoOJQJmH sH u6U@6 5S Hyperlink >*B*ph  &4560x n o 0800x00x000000000000x0000000 0000 @0@0@0P@0P@0@0@0@0@0@00lذ00L6 @0 0 x W!!  ! !  i q XXl ,2$;UPCKom!@f0(  B S  ?  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