Microsoft Word - 164-169 164 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 Studying of Structural Properties of ZnxNi1-x-yCuyFe2O4 Spinel Ferrite Using XRD Powder Ahmed R.Abdil Majeed Dept. of Physics /College of Education for pure Science ( Ibn Al- Haitham)/University of Baghdad Received in:4 April 2013,Accepted in :19February 2014 Abstract ZnxNi1-x-yCuyFe2O4 spinel ferrite were prepared using solid state reaction method with (y=0.1, x=0.2, 0.3, 0.4, 0.5, 0.6 ) . X-ray diffraction with diffractometer CuKα analysis have been carried out and studied showing single phase spinel cubic with space group FD͞3m for all prepared samples . Lattice parameters and crystallite grain size and x-ray density(ρx-ray) bulk density and porosity ratio's were calculated and showed good agreement with the international data reported in the scientific research's. Keywords: Spinel ferrite- 165 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 Introduction Ferrite with spinel type structure may be described by the general formula MeFe2O4 where Me are divalent cations ( Cu2+ , Ni2+ , Cd2+ ….) the space group of this ferrite is ( FD͞3m ) and the lattice parameters are typically ~ 5.8 °A. The Oxygen anions are arranged in Face Center Cubic ( FCC) lattice . Each unit cell contains 8 formula units with O2- anions in the 32 (e) sites and metal cations reside on 8 of 64 tetrahedral sites ( A- sites ) and 16 of 32 octahedral sites ( B- sites ) [1-8].A whole range of possible cation distribution is observed as shown in fig(1).The study of ferrites materials has attracted immense attentions of the scientific community because of their novel properties and technological applications[2]. Due to their various technological applications NiZn ferrite have attracted recently considerable research interests [3].We have been studied the structure of ZnxNi1-x-yCuyFe2O4 ferrite with different dopant concentrations and calculating the lattice parameters ,x-ray densities , grain size for each dopant and the unitcell volume by using the XRD analysis technique in order to study the effects of increasing Zn-Cu on Ni-ferrite. Experimental procedures Spinel ferrite with the formula ZnxNi1-x-yCuyFe2O4 have been prepared by suitable solid state reaction method. The structure of the spinel Me-type in our present work have been studied using powder XRD analysis and carried out using SHIMADZU6000 diffractometer with CuKα radiation. The obtained XRD data was compared with standard patterns of JCPDS-ICDD (International Center for Diffraction Data) card no. 89-8103 for α-Fe2O3 and card no. 08-0234. The lattice parameters of the samples was determined using the relation[4,5] aexp= dhkl(h2+k2+l2)1/2 ………..(1) The average crystallite size was determined from the diffraction peak broadening with use of the Scherrer's equation [2-5]. D=0.98λ/βcosθ ………………….(2) Here λ is wavelength of the CuKα radiation (λ=1.54060 A°) , and β is the FWHM in radians. The x-ray density for spinel ferrite structure is : ρx-ray= Z.M/V.NA ……………..(3) where Z=8 for spinel cubic ferrite , M= molecular atomic mass , V= a3 the volume , NA=Avogadro number [2,4]. Porosity ratio for the prepared samples also calculated using the relation; ٪Where ρbulk=mass/volume of the samples. Results and Discussion Fig.2 shows XRD patterns of spinel cubic ferrite samples ZnxNi1-x-yCuyFe2O4 with different concentrations, comparing with standard pattern( JCPDS file no.08-0234 ) ,all the XRD patterns have been indexed (hkl) manually and the lattice parameters, crystallite grain size, x-ray density and porosity ratio were calculated using equations (1-4).All the prepared samples showed spinel cubic structures with space group FD͞3m,Table.1 summarizes the dependence of lattice parameters determined by XRD analysis. The most intense peaks in all specimens ,indexed as (220), (311), (221), (400), (422), (333), and (440) are found to match well with single phase cubic spinel structure (JCPDS no. 08-0234) no additional phase corresponding to any structures in doped samples was detected. It can be observed that the lattice parameters increases linearly with increasing x-value due to the greater ionic radius of Zinc ion (~0.74 °A) with respect to ionic radius of iron ions (~ 0.55 A°). Fig.3 plots the lattice parameters as a function of x-values for Zn substitutions where y=0.1 for all prepared samples. The porosity ratio for the prepared samples listed in table.1 is between 9 to 14 percentage and 166 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 it seems to be reasonable according to situations in our poor lab's equipment's .The results of the present work were totally acceptable and in agreement with the international works reported in M. Sopan etl and M. A. Batal. and the other researchers[1-8]. Conclusions ZnxNi1-x-yCuyFe2O4 (y=0.1, x= 0.2, 0.3, 0.4, 0.5, 0.6 ) were synthesized by solid state reaction method. The x-ray diffraction analysis for all prepared samples revealed existence of single phase cubic spinel structure identified by (JCPDS card no. 08-0234) with space group FD͞3m in agreement with the data's reported in most scientific research and we showed also that XRD analysis is a very useful tools in materials science and technology research . Reference 1- Sopan, M. Rathod and Ashok B.Shinda (2012) Synthesis and characterization of nanocrystalline Ni Cu Zn ferrite prepared by sol – gel auto combustion method, Journal of advancements in Research & technology ,1, Issue 6, Nov. 2-Batal, M. A.;Alwash, N. H. ;Arasol,K. T.and Ataya, R. E. (2012), Studying the effect of sintering temperature on electrical properties for the system ZnxNi1-x-yCuyFe2O4, Energy procedia, 19 , 109-115. 3- KENFACK Flaurance (2004) Complex oxides of the system Cu-Ni-Fe-O synthesis parameters , phase formations and properties, PhD Thesis , Dresden university of technology 4- Monica Soresco, Diamandescu, L., Peelamedu, R. ;Roy, R. and Yadoji ,P.(2004) ,Structural and magnetic properties of NiZn ferrite prepared by microwave sintering, Journal of magnetism and magnetic materials, 279,195-201. 5- Christopher Hammoned (2009) ,The Basic of Crystallography and Diffraction 3rd edition, International union of Crystallography , Oxford science puplication. 6- Caizer, C.; Stefanescu M.; Muntean, C.and. Hrinca, I. (2001) Studies and magnetic properties of Ni-Zn ferrite synthesized from the glyoxilates complex combination, Journal of Optoelectronics and advanced materials,.3 (4)December, 919-924. 7- Potange, S. M.;Sagar, E.; Shirsath, Jangam, G. S.; Lohar, K. S. ;Santosh Jadhav S.and Jadhav, K. M. (2011) Rietveld structure refinement , cation distribution and magnetic properties of Al3+ substituted NiFe2O4 nanoparticles, Journal of Applied physics 109, 053909. 8- Vladimir Šepelăk and Klăra Tkăcovă (1997) Mechanically induced structural disordering in spinel ferrite, Slovaca Rocnic 2,3, 266-272. Table No. (1): Lattice parameters, crystallite grain size and x-ray density with porosity ratio for ZnxNi1-x-yCuyFe2O4 for the prepared samples Dnm Porosit y ratio x-ray ρ V °A3 a A° Chemical formula X, y value sampe 34.2614% 5.46 573.838.35Zn0.2Nio.7Cu0.1Fe2 O4 0.2, 0.1 b1 24.689% 5.37584.98,36Zn0.3Nio.6Cu0.1Fe2 O4 0.3, 0.1 b2 42.410% 5.27586.378.37Zn0.4Nio.5Cu0.1Fe2 O4 0.4, 0.1 b3 43.614% 5.59588.488.38Zn0.5Nio.4Cu0.1Fe2 O4 0.5,0.1 b4 42.2411.2% 5.36590.588.39Zn0.6Nio.3Cu0.1Fe2 O4 0.6, 0.1 b5 167 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 Figure No.(1) Structure representation for spinel cubic ferrite Figure No.(2): XRD patterns of powdered ZnxNi1-x-yCuyFe2O4 for different substitutions x- value 168 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 Figure No.(3): Lattice parameters as a functions of Zn x-values Show the increasing of lattice parameters with increasing of x-values 169 | Physics 2014) عام 3(العدد 27المجلد مجلة إبن الھيثم للعلوم الصرفة و التطبيقية Ibn Al-Haitham Jour. for Pure & Appl. Sci. Vol. 27 (3) 2014 الصيغة الكيميائية يدراسة الخصائص التركيبية للفيرايت ذ ZnxNi1-x- yCuyFe2O4 باستخدام حيود االشعة السينية للمساحيق XRD احمد رفيق عبدالمجيد جامعة بغداد)/ابن الھيثم (كلية التربية للعلوم الصرفة /قسم الفيزياء 2014شباط 19قبل البحث 2013نيسان 4استلم البحث : الخالصة باستخدام تقنية تفاعل الحالة ZnxNi1-x-yCuyFe2O4الفيرابت المغزلي مكعب التركيب بالصيغة الكيميائية حضر وتم اجراء عملية تحليل حيود االشعة السينية لھا , ( y=0.1, x=0.2, 0.3, 0.4, 0.5, 0.6)الصلبة وبنسب تعويض واظھرت ,JCPDS 08-0234 ورقم الكارت ICDDالحيود مع الكارتات العالمية التابعة للمركز الدولي لبيانات وقورنت وبعد , FD͞3m تركيب طوري واحد من نوع المغزلي المكعب ورمز مجموعة التناظر له ذوجميع النماذج المحضرة انھا لحيود وكذلك باستخدام بيانات ا ناتاجراء عمليات التحليل لھذه البيانات وقياس االبعاد البلورية للشبيكة وحجمھا وكثافة العي راالبعاد البلورية وظھ فيلعنصر الخارصين وتاثيرھا xنسبة المسامات الموجودة في كل عينة ودراسة نسب التعويض .انھا على تطابق تام مع مانشر في البحوث العالمية نيكل خارصين نحاس فيرايت –حيود االشعة السينية - :الكلمات المفتاحية