17062012121610_001 17062012121611 17062012121611_001 17062012121611_002 17062012121611_003 17062012121611_004 17062012121611_005 17062012121611_006 17062012123239 17062012123239_001 17062012123239_002 17062012123410 17062012123411 17062012123411_001 17062012123411_002 17062012123430 17062012123430_001 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 alhaitham)/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 o2anions in the 32 (e) sites and metal cations reside on 8 of 64 tetrahedral sites ( asites ) and 16 of 32 octahedral sites ( bsites ) [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 1sopan, 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. 3kenfack flaurance (2004) complex oxides of the system cu-ni-fe-o synthesis parameters , phase formations and properties, phd thesis , dresden university of technology 4monica 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. 5christopher 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. 8vladimir 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 xvalue 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-xycuyfe2o4 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 the effect of doping by sr on the structural, mechanical and electrical characterization of la1ba1-xsrx ca2cu4o8.5+δ kareem a. jasim mohammed a.n. thejeel raghad subhi al-khafaji dept. of physics /college of education for pure science (ibn -al-haitham) /university of baghdad received in :4 june 2013 , accepted in :10 october 2013 abstract the sr doped la1ba1-xsrx ca2cu4o8.5+δ samples with 0 ≤ x ≤ 0.3 had been prepared using the solid state reaction. the samples were claimed at 800°c for 3hr, palletized and sintered at 860°c for 20hr in air . dielectric constant and loss by means of capacitance have been investigated with frequencies in the range of 1khz to 1mhz for our samples at room temperature. also, shore hardness has been measured. the dielectric constant and loss decrease slightly with the increase of frequency for all compounds. additionally, the partial substitution of sr+2 into ba+2 sites never have effect on the dielectric properties. x-ray diffraction (xrd) analysis showed a tetragonal structure and the as grown la1ba1-xsrx ca2cu4o8.5+δ correspond to the 1124 phase. it was found that the change of the sr concentrations of all our samples produces a change in a, c and c/a parameters. keywords: la1ba1-xsrx ca2cu4o8.5+δ, dielectric properties, shore hardness. 170 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 introduction high transition temperature tc superconductors have generated tremendous excitement because of the potentially significant technological applications. materials have been discovered that exhibit superconductivity up to temperatures much higher than the boiling point of liquid nitrogen (77k). since 1911, when the dutch physicist heike kemerlingh onnes discovered superconductivity in mercury at 4.2k [1], the highest observed values of tc gradually moved upward. in spite of great efforts to increase tc, 23.2k (reported in the intermetallic compound nb3ge in 1973 by gavaler [2]), stood as the record until 1986. in that year j.g.bednorz and k.a.muller [3] observed that lanthanum barium copper oxide (la-bacu-o) began its superconducting transition as it was cooled below 35k. this discovery opened the way for all of the subsequent work on high temperature superconductors. soon after the discovery of superconductivity at 30k in la-ba-cu-o system, these materials are extensively studied by the substitution of rare-earth compound to understand the nature of transport phenomena in each system. the exact composition of superconducting phase la2xbaxcuo4-y (0.1 < x < 0.2) was found by uchida et al. [4] and takagi et al. [5]. the structure of la1ba1-xsrx ca2cu4o8.5+δ is shown in figure.1. lbcco is physically the hardest of the four materials, and with stronger bonds. neutron scattering experiments, which probe the magnetic structure of the material, are typically limited to study lbcco because of their requirement for large single crystals. but lbcco has not been successfully studied with an stm, because so far there has been no successful recipe to obtain an atomically flat surface with tunnel access through an insulating layer to the relevant unperturbed cuo2 plane. this paper will describe perovskite structure, based on la1ba1-xsrx ca2cu4o8.5+δ composition, and interpret the mechanic and dielectric properties ,then discuss how the difference of substitution that would influence la1ba1-xsrx ca2cu4o8.5+δ based structures of mechanic and dielectric properties. experimental technique the synthesis of la1ba1-xsrx ca2cu4o8.5+δ (x=0, 0.1, 0.2and 0.3) compounds have been prepared by solid state reaction method .we have used appropriate weights of pure powders materials 99% of la2o3, bao, srco3, cao and cuo as starting materials .they were carefully mixed and ground by using a gate mortar .the mixture was dried in an oven at 200˚c,then it is put in farness for calcinations at 800˚c during 3hr,then cooled to room temperature . in the second step, the mixture was pressed into disc shaped pellets(1.6 cm) in diameter and (0.2-0.3 cm) thick, using hydraulic press under pressure of (9 ton/cm2 ).the pellets were sintered in air at 860˚c for 20hr and then cooled to room temperature. the samples were characterized by x-ray diffractometer. the excess of oxygen content (δ) have been described elsewhere [6,7]. the structure of the prepared sample was obtained by using x-ray diffractometer (xrd). a computer program was established to calculate the lattice parameters a and c this program is based on cohen’s least square method [8]. the frequency dependent dielectric measurements were carried out by using a hp-r2c unit 4274a lcr meter (hewlett-packard, usa) in the range of 100 khz–10 mhz and the agilent 4275b lcr meter (agilent technologies japan, ltd.) in the range of 1 khz–100 khz .a conventional two –probe technique was used for these measurements .silver paint was applied to both the surfaces of the sample, and copper leads were fixed to the silver electrode surfaces. by measuring the capacitance ( c ) and (tanδ ) of the samples, the dielectric constant (έ) and loss factor (ε˝) of the samples were calculated using the following expressions[9]: 171 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 (1) c )a / d ( ) / 1 ( ' oεε = ...(2) tan ε ε δ ′ ′′ = where d is the thickness of the pellet (0.2 cm) , εo is the permittivity of space (εo =8.85*10-12 f/m ) ,and a is the cross-sectional area of the electrode (pellet).the frequency dependent dielectric measurements of la1ba1-xsrxca2cu4o8.5+δ compounds were done in the room temperature . shore hardness measurements of the samples produced are performed by using a digital microhardness tester (durometer shor d ) at room temperature. the values of shore hardness are determined with an average of three readings at different locations of specimen surfaces for la1ba1-xsrx ca2cu4o8.5+δ doped with (x=0,0.1,0.2and0.3). results and discussion the series xrd spectra of the samples la1ba1-xsrx ca2cu4o8.5+δ with x varying from 0 to 0.3 are shown in figure.2 . all the samples in the present investigation were subjected to gross structural characterization by x-ray diffraction. the xrd data collected from various samples (samples having various la, ca, ba,cu and sr concentration) were all polycrystalline and correspond to la-1124 phases. the xrd also shows some impurity phases with vanishingly small concentrations. it could be seen from the spectra that there were two main phases in all samples of the la-base systems, high-tc phase (1124), low-tc phase(1202) and a small amount of impurity phases of (ca, ba)2cuo3, calao4 and cuo. the appearance of more than two phases could be related to the stacking faults along the caxis. the comparison between the relative intensities of xrd patterns for the samples with sr=0,0.1, 0.2 and 0.3, with the relative intensity of the same reflections of the sample with non sr shows that all the samples have reflection high intensity, and it decreased by the increase of sr . the lattice parameters have been estimated using d-values and (hkl) reflections of the observed x-ray diffraction pattern through the software program based on cohen,s least square method, the parameters a, c and c/a are shown in table(1). the variations in the real part (έ) and imaginary part (ε˝) of dielectric constant of la1ba1-xsrx ca2cu4o8.5+δ samples as a function of frequency at room temperature are shown in figure.3(a and b) ,we observed a decrease in dielectric constant (έ) and loss(ε˝) with the increase of frequency at room temperature without effect sr doping. the real part of the dielectric constant (έ) gives the magnitude of the part of energy stored within the material when it is exposed to the electrical field .the most likely place at which this energy could be stored is within the grains (intergranular sites). they act like termination ends for the crystal. the imaginary part of the dielectric constant (ε˝) indicates the absorption and the attenuation of energy across the interfaces under an external electric field .examples of interfaces are grain boundaries, localized defects and localized charge densities at the defect sites and at grain boundaries [9,10]. figure.4 shows variation of shore hardness of la1ba1-xsrx ca2cu4o8.5+δ with sr-doping ,in which the hardness decrease with the increase of sr-content (x=0.0,0.1,0.2,0.3). conclusion we have prepared samples of the type la1ba1-xsrx ca2cu4o8.5+δ with x = 0, 0.1, 0.2and 0.3 during a short preparation time by solid state reaction. the structure of the la-1124 did not change with the replacement of ba by sr ions whereas the lattice parameters were found to be changed . it was observed that dielectric constant and loss decrease slightly with the increase of frequency for all compounds. 172 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 references 1. kemerlingh onnes . h, leiden commun (1911),12061226. 2. gavaler . j.r (1973) , superconductivityin nbge film above 22k ,phy. lett. 23, 480. 3. bednorz j.g. and miiller k.a (1986) , possible high tc superconductor in the ba-la-cu-o ,z.physics b -condensed matter t,189. 4. uchida ,s.;takagi ,h.;kitazawa,k. and tanaka,s. (1987) ,transporte properties of(la1xax)2cuo4, jpn. j. appl.phys,26, l1. 5. takagi ,h.;uchida,s.; kitazava,k. and tanaka,s. (1987) superconducting properties of (la1-x srx)2cuo4,jpn. j. appl. phys,26, l144-l146. 6. kareem, a. j. and tariq, j. a.(2009), effect of pressure on the structural and electrical characteristics of tl0.8sb0.2sr2ca2cu3o9-δ superconductors prepared by solid state reaction technique, materials science and technology (ms&t) , pittsburgh, pennsylvania ,pp(25-29). 7. kareem a. j. (2012 ),structure and electrical properties of lanthanum doped bi2sr2ca2xlaxcu3o10+ δ superconductor” ,turk j. phys. 36, 245 – 251. 8. manivannan,v.; gopalarishnan ,j. and rao,c.n.r (1994) ,synthesis of cuprates of peroveskite structure in ba-pb-cu-o,journal of sold state chemistry ,109, 205-209. 9. kingery,w.;bown ,h. and uhlmann (1976) , introduction to ceramics. john wiely , new york . 10. adnan ,y, and nawazish, a. k. (2010), dielectric properties of cu0.5tl0.5ba2ca3cu4−yznyo12−_ (y = 0, 3) superconductors, journal of the korean physical society, 57( 6):1437-1443. table no.(1) : values of lattice parameter, c/a ,oxygen content (δ), (έ) ,(ε˝) and hardness for the samples for different compositions of la1ba1-xsrx ca2cu4o8.5+  figure no.(1): the structure of la1ba1-xsrx ca2cu4o8.5+δ x δ(o2) a(a0) c(a0) c/a έ(at1mhz) ε˝(at1mhz) hardness shore 0 0.52 3.789 21. 972 5.799 0.955 0.049 91 0.1 0.51 3.785 21.981 5.807 1.031 0.097 89 0.2 0.49 3.773 21.9842 5.827 1.123 0.103 86 0.3 0.537 3.7853 21.9815 5.807 1.572 0.182 78 173 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 figure no.(2): xrd patterns for the la1ba1-xsrx ca2cu4o8.5+δ samples with x=0, 0.1, 0.2 and 0.3. figure no.(3): variations of (a)dielectric constant and (b)dielectric loss versus frequency for la1ba1-xsrx ca2cu4o8.5+δ (x=0,0.1,0.2,0.3) at room temperature figure no.(4): variation of shore hardness with sr–content for la1ba1-xsrx ca2cu4o8.5+δ 174 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 اثیرالتطعیمت sr في الخواص التركیبیة المیكانیكیة والكھربائیة للمركب la1ba1-xsrx ca2cu4o8.5+δ كریم علي جاسم النبي محمد عبد رغد صبحي عباس قسم الفیزیاء/كلیة التربیة للعلوم الصرفة (ابن الھیثم )/ جامعة بغداد 2013تشرین االول 10قبل البحث في ، 2013 حزیران 4استلم البحث في : الخالصة باستخدام . x ≤ 0.3 ≥ 0عند srبالسترنیوم المطعم la1ba1-xsrx ca2cu4o8.5+δ حضرت نماذج من المركب كبست على شكل اقراص وحرقت ,م مدة ثالث ساعات 800تم كلسنة النماذج بدرجة حرارة .تفاعل الحالة الصلبة طریقة 1khzقیس ثابت العزل وفقدان العزل في المدى الترددي ، م مدة عشرین ساعة في الھواء860بدرجة حرارة 1mhz واوضحت النتائج ان ثابت العزل وفقدانھ یتناقص ببطء مع . في درجة حرارة الغرفة فضال عن قیاس الصالدة في ba+2في مستوى sr+2ال یوجد ھناك تاثیر واضح عند االستبدال الجزئي التردد لجمیع النماذج فضال على ذلك كما وجد 1124خصائص العزل الكھربائي كما اظھر تحلیل حیود االشعة السینیة بان تركیب المركب رباعي الطور . c/a, c, aان التغیر في تركیز السترنیوم لكل النماذج ینتج منھ تغیرا في ثوابت الشبیكة ية، صالدة شور، الخواص العزلla1ba1-xsrx ca2cu4o8.5+δ الكلمات المفتاحیة: 175 | physics @a@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@@úó‘ój�n€a@î@úœäñ€a@‚ï‹»‹€@·ró:a@âig@ú‹©@ü‹127@@öü»€a@i1@‚b«@h2014 ibn al-haitham jour. for pure & appl. sci. vol. 27 (1) 2014 kareem a. jasim mohammed a.n. thejeel raghad subhi al-khafaji ihjpas. 36 (3) 2023 85 this work is licensed under a creative commons attribution 4.0 international license the effect of substrate nature on the properties of tin sulfide nanostructured films prepared by chemical bath deposition *corresponding author: msaleh196730@gmail.com abstract the substrate's nature plays an important role in the characteristics of semiconductor films because of the thermal and lattice mismatching between the film and the substrate. in this study, tin sulfide (sns) nanostructured thin films were grown on different substrates (polyester, glass, and silicon) using a simple and low-cost chemical bath deposition technique. the structural, morphological, and optical properties of the grown thin films were investigated using x-ray diffraction (xrd), field emission scanning electron microscopy (fesem), and ultraviolet-visible-near infrared (uvvis-nir) spectroscopy. the xrd and fesem results of the prepared films revealed that each film is polycrystalline and exhibits both orthorhombic and cubic structure types. in addition, the deposited films on polyester and glass showed good absorption in the uv-vis-nir range. keywords: tin sulfide; chemical bath deposition; polyester; glass, nanostructure. 1. introduction recently, significant attempts have been made to synthesize and characterize nanostructured semiconductor materials owing to their unique properties, as well as their performance in a variety of applications, notably sensing, i.e., their ability to sense gas and light [1]. researchers are increasingly interested in iv-vi semiconductors such as sns, gese, and pbs because of their numerous applications, such as photovoltaic devices and near-infrared detectors [2]. among these semiconductors, sns has advantages, including abundance, low toxicity, and a high absorption coefficient (104 cm-1) [3–5]. sns nanostructure films can be deposited through different techniques, such as electrodeposition [6], spray pyrolysis [7], radio frequency sputtering [8], doi.org/10.30526/36.3.3020 article history: received 17 september 2022, accepted 27 november 2022, published in july 2023. zahra'a a.abood department of physics, college of education, university of mustansiriyah, baghdad, iraq. rosezoz1820@gmail.com ibn al-haitham journal for pure and applied sciences journal homepage: jih.uobaghdad.edu.iq baha'a a.m.al hilli department of physics, college of education, university of mustansiriyah , baghdad, iraq. bahahilli@uomustansiriyah.edu.iq mohamed s. mahdi* ministry of science and technology, renewable energy directorate msaleh196730@gmail.com https://creativecommons.org/licenses/by/4.0/ mailto:msaleh196730@gmail.com https://uomustansiriyah.edu.iq/?lang=en mailto:rosezoz1820@gmail.com mailto:rosezoz1820@gmail.com https://uomustansiriyah.edu.iq/?lang=en mailto:bahahilli@uomustansiriyah.edu.iq mailto:bahahilli@uomustansiriyah.edu.iq mailto:msaleh196730@gmail.com mailto:msaleh196730@gmail.com ihjpas. 36 (3) 2023 86 thermal evaporation [9], and chemical bath deposition (cbd)[10-14]. the cbd technique is simple, low-cost, and uses low-temperature deposition (<100 oc) compared to other techniques. additionally, it can be used for continuous deposition. moreover, the substrate's nature plays a crucial role in the characteristics of sns film because of the thermal and lattice mismatching between the film and the substrate. therefore, in this work, the nanostructured sns films were deposited using the cbd method on different substrates (polyester, glass, and silicon). 2. experimental part the cbd technique was used to synthesize sns films on different substrates (glass, polyester, and si). the procedure consists of 1.12 g dihydrate tin chloride, 3.234 g complex agent tri-sodium citrate, and 0.56 g thiocetamide. all chemical materials were dissolved in 50 ml of deionized water. aqueous ammonia was added drop by drop, and the ph of the solution was adjusted to 6.5. the mixture was stirred well using a magnetic stirrer at room temperature. substrates were ultrasonic cleaned in acetone, methanol, and deionized water, respectively, for 30–40 minutes before film deposition. then, the substrates were immersed in the mixture. the deposition was carried out at 80 oc for 4 h. the substrates were removed from the beaker, washed with deionized water, and dried naturally. the structural, morphological, and optical properties of the grown thin films were examined using x-ray diffraction (xrd), field emission scanning electron microscopy (fesem), and ultraviolet-visible-near infrared (uv-vis-nir) spectroscopy. 3. results and discussion 3.1 structural properties figure 1 shows the x-ray diffraction patterns of grown sns films on polyester, glass, and silicon substrates. these patterns showed two peaks in the area around 2θ = 31.9 and 39.7, which can be indexed to the orthohombic structure of sns (icdd card: 39-0354) [4, 5, 15]. moreover, the xrd patterns of the deposited films on the glass and silicon substrates exhibit additional peaks around 2θ = 26.85 and 31.1, which can be indexed to the cubic structure of sns [15,16 ]. in addition, the peaks of polyester, and silicon substrates were observed. the high, intense, and wide peak of the polyester substrate at 2θ = 26.3˚ may be responsible for the absence of peaks of the cubic structure in the pattern of the deposited film on polyester. figure 1. xrd patterns of grown sns films on various substrates, polyester, (b) si, (c) glass the average crystalline size (d) was calculated from the xrd pattern using scherrer’s formula, which is expressed as follows [5, 17, 18]: ihjpas. 36 (3) 2023 87 𝐷 = 0.9𝜆 𝛽𝐶𝑂𝑆𝜃 (1) where 𝜆 is the x-ray wavelength, 𝛽 is the full width at half maximum of the xrd peak, and 𝜃 is the bragg angle. the d values for (111) orientation were found to be 223 a°, 172 a°, and 295 a° for deposited films on glass, si, and polyester, respectively. the strain (𝜖) values of the grown films were calculated using the following equation [19]: 𝜖 = 𝛽 4𝑡𝑎𝑛𝜃 (2) the 𝜖 values for (111) orientation are 5.64x10-3, 7.34 x10-3, and 4.24 x10-3 for grown films on glass, si, and polyester, respectively. comparative analysis of the xrd findings for the films is shown in table 1. table 1: xrd findings of deposited sns films on different substrates. substrate (h k l) d (ǻ) 3-ε x 10 polyester (111) 295 4.24 glass (111) 223 5.64 silicon (111) 172 7.34 3.2 surface morphology figure 2 shows fesem images of deposited films on various substrates. it is obvious that the grown films on polyester and glass substrates comprise many flower-like nanostructures agglomerating for sns orthorhombic structure, as well as beneath a layer of spherical grains for cubic sns [16, 20,21]. while the grown film on the glass substrate comprised distributed and uniformly many flower-like nanostructures for orthorhombic structure sns, as well as a beneath layer of spherical grains for cubic sns, the presence of two morphologies that relate to orthorhombic and cubic structures agrees with the xrd analysis of figure 1. figure 2. fesem images of prepared films on different substrates, (a) polyester (b) glass (c) silicon orthorhombic cubic ihjpas. 36 (3) 2023 88 3.3 optical properties the absorbance spectra of deposited films on polyester and glass substrates in the range of (350 -1100 nm) are shown in figure (3). according to the spectra, the absorption in the visible and near-infrared wavelengths is generally good. additionally, the deposited film on glass has a larger absorbance value than the film on polyester in the range of (550 -1100 nm). while the spectra behave differently in the range of (350 550 nm), the film deposited on polyester has a higher absorbance value than the film deposited on glass. figure 3. the absorbance spectra of deposited films on polyester and glass substrates. the nature of the energy gap optical transmission can be determined using the relation [5, 22]: αhʋ = a(hʋ − 𝐸𝑔) n (3) where a is constant, h is planck constant, ʋ denots frequency, 𝐸𝑔 is the energy gap, and α is absorption coefficient. figure (4) illustrates plotting (αhυ)2 versus (hυ) curves for films deposited on two different substrates . the equation (3) is matched with n = 1/2, which indicates permissible transitions. the 𝐸𝑔 value can be determined by extrapolating the straight line of (αhʋ) 2 versus the hʋ curve to intercept the horizontal hʋ axis. from figure (4), the 𝐸𝑔 values were found to be 1.38 and 1.02 ev for grown films on polyester and glass substrates, respectively. figure 4. energy gap of grown films on (a) polyester (b) glass ihjpas. 36 (3) 2023 89 4. conclusion in this work, the nanostructure of tin sulfide (sns) thin films was successfully grown by simple and low-cost chemical bath deposition on different polyester, glass, and silicon substrates. the obtained results showed that the substrate nature had significant effects on the structural, morphological, and optical properties of the deposited films. acknowledgment the authors extend their thanks and gratitude to the ministry of sciences and technology for its great support in completing the research, as well as the mustansiriya university college of education. references 1. law. m.; goldberger. j.; yang. p.; semiconductor nanowires and nanotubes, annu. rev. mater. res. 2004. 34, 1, 83–122. 2. xiao. g.; recent advances in iv–vi semiconductor nanocrystals: synthesis, mechanism, and applications, rsc adv. 2013. 3, 22, 8104–8130, 3. greyson. e. c.; barton. j. e.; odom. t.w.; tetrahedral zinc blende tin sulfide nanoand microcrystals, small. 2006. 2, 368-375. 4. gao, c.; shen, h.; sun, l.; preparation and properties of zinc blende and orthorhombic sns films by chemical bath deposition. appl. surf. sci. 2011. 257, 67-78. 5. mahdi. m. s.; latif, k. h.; jabor, a. a.; ibrahim, k.; ahmed, n. m.; hmood, a.; mustafa, f. i.; bououdina, m.; tin sulfide flower-like structure as high-performance near-infrared photodetector, journal of electronic materials. 2020. 49, 5824–5830. 6. yue, g. h.; peng, d. l.; yan, p.x.; wang, l.s.; wang, w.; luo, x. h.; structure and optical properties of sns thin film prepared by pulse electrode position. alloys compd. 2009. 468, 254-266. 7. patel, m.; mukhopadhyay, i.; ray, a.; annealing influence over structural and optical properties of sprayed sns thin films. opt. mater. 2013. 35, 93-104. 8. hartman, k.; johnson, j. l.; bertoni, m. i.; recht, d.; aziz, m. j.; scarpulla, m.a.; buonassisi, t.; sns thin-films by rf sputtering at room temperature. thin solid films. 2011. 519,74-88. 9. cheng. s.; conibeer, g.; physical properties of very thin sns films deposited by thermal evaporation, thin solid films. 2011. 520, 83-95. 10. guneri, e.; ulutas, c.; kirmizigul, f.; altindemir, g.; gode, f.; gumus, c.; effect of deposition time on structural, electrical, and optical properties of sns thin films deposited by chemical bath deposition, appl. surf. sci. 2010. 257, 118-128. 11. mohamed, s.; mahdi, k.; ibrahim, a.; hmood, n. m.; ahmed, mustafa, f.i.; control of phase, structural and optical properties of tin sulfide nanostructured thin films grown via chemical bath deposition .j. electron. mater. 2017.46, 42-57. 12. gode, f.; guneri, e.; baglayan, o.; effect of tri-sodium citrate concentration on structural, optical and electrical properties of chemically deposited tin sulfide films, appl. surf. sci. 2014.318, 227-235. https://link.springer.com/journal/11664 ihjpas. 36 (3) 2023 90 13. jayasree, y.; chalapathi, u.; raja, v. s., growth and characterization of tin sulphide thin films by chemical bath deposition using ethylene diamine tetra-acetic acid as the complexing agent, thin solid films, 2013. 537, 149-166. 14. avellaneda, d.; delgado, g.; nair, t. s.; nair, p. k.; structural and chemical transformations in sns thin films used in chemically deposited photovoltaic cells, thin solid films. 2007. 515, 57-71. 15. mohamed, s.; mahdi, k.; ibrahim, a.; hmood, naser. m.; ahmed, falah. i.; mustafa, shrook a.; azzez. high performance near infrared photodetector based on cubic crystal structure sns thin film on a glass substrate. materials letters. 2017 200, 10-13. 16. márquez, i. g.; romano-trujillo, r.; gracia-jiménez, j. m.; orthorhombic and amorphous sns thin films on flexible plastic substrates by cbd, j. mater sci: mater electron. 2021. 32, 15898–15906. 17. tauu, j., optical properties and electronic structure of amorphous semiconductor in optical properties of solid, plenum, new york, 1969. 18. saima, m.; bushra i.; misbah, a.; zeb, n. j.; suthan k.; aurang. z.; low-temperature synthesis and characterization of sn-doped sb2s3 thin film for solar cell applications. journal of alloys and compounds. 2015. 632, 723-728. 19. boughalmi, r.; boukhachem, a.; kahlaoui, m.; maghraoui, h.; amlouk, m.; physical investigations on sb2s3 sprayed thin film for optoelectronic applications. materials science in semiconductor processing. 2014. 26, 593-602. 20. mohamed, s.; mahdi, husam s.; hmood, a.; bououdina. m.; structure, morphology, and photoresponse characteristics dependence on substrate nature of grown π-sns films using chemical bath deposition. optical materials. 2022. 123. 111-122. 21. mohamed, s.; mahdi. naser. m.; ahmed, a.; hmood, k.; ibrahim, m.; bououdina. comprehensive photoresponse study on high performance and flexible π-sns photodetector with near-infrared response. materials science in semiconductor processing. 2019.100. 270274. 22. akkari, a., guasch, c. kamoun turki, n.; chemically deposited tin sulphide. journal of alloys and compounds. 2010. 490, 180-183. microsoft word 11-18     11   ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020       thin cds properties optical nanostructure's on influence annealing technique deposition vapor physical by prepared films esraa a. abbas article history: received 2 may 2019, accepted 10 july 2019, published in april 2020. abstract in this work, the influence of the annealing temperature on the optical properties of the thin films cadmium sulphide (cds) has been studied. thin films of cadmium sulphide (cds) were made using the physical vapor deposition (pvd) method. the optical properties of annealing temperatures (as deposited, 200, 250, and 300℃ ) were scrupulous. the uv/vis spectrophotometer investigated optical parameters such as transmission, the coefficient of absorption and energy gap of the films for the range (400-110 nm) as an assignment of the annealing temperature. the optical properties were calculated as a function of annealed temperature: absorption, transmission, reflection, band gap, coefficient of absorption, excitation coefficient and index of refraction. keywords: physical vapor deposition, cadmium sulphide (cds) films, annealing temperature, optical properties. 1. introduction the semiconductor manufacturing products now spread throughout the world and penetrate pointedly into the daily life of an epidermal existence. for many semiconductor devices, thin films are well known as stamping for enforcement in abundant physically established profession [1]. interest in the physical properties of thin films has increased significantly in recent years as new effects may appear in film statements that are not observed in bulk samples [2]. cadmium sulfide thin film is a suitable n-type semiconductor for an opening layer in solar cells for cdte/cds heterojunction [3,4]. due to its new properties, cds is a substance material such as photoconductivity, refractive elevation single (2.5) [5]. and its high cognition of electrons [6]. thin cds films such as vaporization by vacuum, sputtering, electro-deposition, ibn al haitham journal for pure and applied science journal homepage: http://jih.uobaghdad.edu.iq/index.php/j/index doi: 10.30526/33.2.2438 department of physics, college of education, almustansiriyah university, baghdad, iraq. israa.akram.78@gmail.com   12  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020 radio frequency, pulsed laser evaporation, molecular beam epitaxy (mbe) were obtained using several techniques [7]. cds thin film development was based on organic metal vapor deposition (mocvd), spray pyrolysis deposition (spd), close-spaced sublimation (css), successive ionic layer adsorption and reaction (silar) and chemical bath deposition (cbd) [8]. physical vapor deposition (pvd) has become an engaging technique due to its naivety, low cost and look high accuracy data technology, with a large surface and large surface deposition at low temperatures [9]. the purpose of this work the effect of annealing on cds thin film optical parameters. 2. experimental method one of the physical vapor deposition (pvd) combined method is thermal evaporation. this is a form of thin film precipitation on glass substrates, a vacuum technology that stratifies the clothing of pure materials to the surface of multiple materials. the optical properties of pvd cds thin films are based on the parameters of proportional reactant condensation for chemical reaction, films thickness, aqueous solution ph and annealing temperature. the deposition technique of thermal vacuum evaporation depends on the heating identity. ultimately, the material vapor precipitates on the cold substratum surface and on the vacuum chamber walls in the form of the thin film. usually, low pressure is used; approximately (210-5) mbar or up to (1.510-5) torr, to avoid a vapour-environment response. the mean free way of vapour iotas at these low pressures is the same as the measurements of the vacuum chamber so that these particles go in go in straight lines from the vanishing source towards the substrate. this begins with "shadowing" phenomena with 3d objects, especially in areas that are not opened directly from the (crucible) vanishing source. in addition, the normal vitality of vapour molecules achieving the surface of the substratum is by and large low in warm vanishing strategies (order of kt, i.e. 10ths of ev). at a rate equal to 5.2å / sec deposition and thickness of 0.5 is equal in all samples. (0,200,250 and 300) oc. 3. results and discussion figure1. illustrates the transmittance via wavelength; it can be clearly seen that the transmittance of 250oc is higher than the all deposited thin films showing a shift in peak location as the temperature increase. all the films exhibit peaks maxima and minima. this might be due to the high homogeneity of the deposited thin films. transmittance was given by the proportion of the force of the transmitting rays (it) through the film to the power of the incident rays (io) on it as deposited [10].   13  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020   𝑇 𝐼 𝐼 1 it is also observed in figure 1. that increasing thermal annealing has a tendency to diminish transmittance in all the range of solar powered light energy. this is as an aftereffect of the development of denser movies in view of water evaporation. this behaviour agrees with the results published by ezema et al. [11]. figure 2. shows the relation between absorbance and wavelength. it was observed that absorbance was higher for the untreated one and then began to decrease .this can be explained by the inverse relation between transmittance and absorbance. a can be characterized as the proportion between material absorbed light intensity (ia) and incident light intensity (io). 𝐴 𝐼 𝐼 2 the absorbance versus wavelength was plotted for cds; as-grown and annealed thin films. from the absorbance spectra, it was observed generally that the absorption of films in the vis figure 1. transmittance versus wavelength different annealing of cds thin films. figure 2. absorption versus wavelength different annealing of cds thin films.   14  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020 area of the solar radiation spectrum decreased with increasing wavelength and film absorption. the sharp absorption edges occurred at wavelengths less than 530 nm and the film absorption edge shifted slightly to longer wavelengths revise. for optimum absorbance at 140oc, the highest absorption values were observed in the annealed samples with the critical annealed temperature. they have noted similar behavior in the [12-14]. figure 3. illustrates the relationship between the coefficient of absorption and the energy of the photon. the absorption coefficient value was in the range of 104 cm which predominated the possibility of direct electronic transitions; the absorption edge was shifted to lower photon energy. 𝛼ℎ 𝜈 ℎ 𝜈 𝐸 3 where α is the coefficient of absorption, a will be consistent, the energy of the photon and 𝐸 the hole of the band will be consistent. the value of the gap of optical energy using figure 4. varied from 2.38 to 2.44 ev, the highest value was reinforced at 200oc for the film. (revise: no verb) increases in the absorption coefficient with annealing temperature were also observed. the absorption coefficient (α) is related to the extinction coefficient (k) by 𝑘 𝛼 𝜆 4 𝜋 4 where λ is the wavelength of the electromagnetic wave [15]. figure 3. alpha(α) versus photo energy different annealing of cds thin films.   15  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020 figure 4. αhυ versus photon energy different annealing of cds thin films. figure 5. shows the coefficient of extinction value calculated using the relationship below. in figure 5. it is clear that the coefficient of extinction value increases with the increase in photon energy. at 600 nm of wavelength, the maximum value of k was observed [16]. figure 5. coefficient of extinction versus various annealing of cds thin films by photo energy. figure 6. shows the refractive index value estimated using the following relationship: the ratio represents the refractive index between the speed of light in the vacuum and the speed of the material, and the relationship between the refractive index and the refractive membrane (r) is as follows: [17]. 𝑅 𝑛 1 𝑘 𝑛 1 𝑘 5 it is crystal clear the highest refractive index value is 200oc. similarly, this pattern was observed in the conduct of the annealing refractive index and attributed to denser films resulting from the disappearance of film water particles [18].   16  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020 figure 6. refractive index versus different annealing of cds thin films with photon energy. figure 7. shows the relationship between the real part of the dielectric constant and the photon energy. it was observed that the real part of the dielectric constant was higher because the value was higher for the film at 200oc and then the inverse relationship between them can explain this. 𝜀 𝑛 𝑘 6 figure 8. represents the value of photo-energy optical conductivity without annealing and various degrees of annealing. the relation is used to determine the optical conductivity where α is the coefficient of absorption and c is the speed of light. the optical conductivity relies immediately on the coefficient of absorption and the increased photon energy that establishes accretion. the optical conductivity value varies from 1.2 to 3ev in photon energy, the elevated value is 200oc for the film. 𝜎 𝛼𝑛𝑐 4𝜋 7 figure 7. the dielectric constant real part vs photon energy for different cds thin films annealing.   17  ibn al-haitham jour. for pure & appl. sci. 33 (2) 2020 figure 8. optical conductivity versus different cds thin film annealing photon energy. 4. conclusion cds thin film was prepared using the technique of thermal evaporation. from the results, it is concluded that the grain size of the cds structure was increased by annealing which in turn causes to decrease the energy band gap to be used in ir optoelectronic devices. an nealing is caused to increase the crystallinity of the resulted structures. the optical transmittance varied with the annealing temperature. cds exhibited characteristics com patible with window material for solar cells and other 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journal of physics and chemistry of solids.2009, 70, 14431447. 11. ezema, f.i.; ezugwu, s.c.; osuji, r.u.; asogwa, p.u.; ezekoye, b.a.; ekwealor, a.b.c.; ogbu, m.p. role of thermal annealing on the optical and solid state properties of chemically deposited cadmium sulphide nanocrystalline thin film grown in a polymer matrix, journal of non-oxide glasses.2010, 1, 45-50. 12. elmas, s.; ozcan, s.; ozder, s.; v, bilgin, s. influence of annealing temperature on the electrical and optical properties of cds thin films, acta physica polonica a.2012, 121, 56-58. 13. abbas, m.m; shahab, a.ab-m.; hassan, n.a.; al-samuraee, a.k. effect of temperature and deposition time on the optical properties of chemically deposited nanostructure pbs thin films, thin solid films.2011, 519, 4917-4922. 14. gray, d.e. american institute of physics handbook (3rd edition mcgraw-hill: new york, ny1982). 15. tauc, j. amorphous and liquid semiconductors (plenum press, london and new york, 1974. 16. cetinorgu, e.; gumus, c.; esen, r. effects of deposition time on the optical properties of air-annealed chemical bath deposited cds films, thin solid films.2006, 515, 16881693. 17. devi, r.; purkayastha, p.; kalita, p.k.; sarma, b.k. synthesis of nanocrystalline cds thin films in pva matrix, bull. mater. sc.2007, 30, 123-128. 18. soubane, d.; ihlal, a.; nouet, g. the role of cadmium oxide within the thin films of the buffer cds aimed at solar cells based upon cigs films fabrication, m.j. condensed matter.2007, 9, 1. 2010) 3( 23المجلد مجلة ابن الھیثم للعلوم الصرفة والتطبیقیة دراسة الخواص الفیزیائیة والتشكیلیة للعازل السیرامیكي عتاب فاضل حسین الجامعة المستنصریة ،كلیة العلوم ،قسم الفیزیاء الخالصة وبنسب وزنیة )سلیكا،فلدسبار،كاؤلین(عراقیة ةمواد محلی عمالبحث تحضیر عازل سیرامیكي باستتم في هذا ال ،و على التوالي وبعد اجراء عملیة التنقیة،(30% ,25%,45%) ة بلتجفیف،والطحن لالطیان العراقیة او الغسل صورة انفرادی تكبس .من الماده المعدنة ةثابت ةوبنسی(%0.1,%0.2,%0.5,%0.7,%1)نسب مختلفة من سلیكات الصودیوم أضیفت (1350 ,1250) ةبدرجات حراری تقى شكل اقراص وحرّ النماذج عل o c ة . على التوالي استخدام المجهر الضوئي لدراس أوضحت .باستخدام طریقة آرخمیدس كافة لنماذجلسطوح النماذج ثم اجریت قیاسات الكثافة الظاهریه والمسامیة الظاهریة لیة مع ارتفاع درجة الحرق نتیجة ي الحاصل بین المواد االو ئاذج ارتفاع نسبة التفاعل الكیمیاالصور المجهریة لسطوح النم ةالنصهار الحاصل الذي یعمل على زیادة التقارب الحبیبي على حساب المناطق عیر المتفاعلة والفجوات وان افضل نسبل .لسلیكات الصودیوم) %0.5(لفحوصات الكثافة والمسامیة الظاهریه هي عند تركیز .عازل السیرامیكي ، الكثافة ، المسامیة ال: الكلمات المفتاحیة ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 study o f the physical and morphological properties of ceramic insulator i. f. hussein departme nt of physics, college of science ,unversity of al mustansiryah abstract in this invest igation insulator ceramic body was p rep ared by using iraqi local materials, these are kaolin, silica sand glass, feldsp ar with weight p ercentage (45%,25%, 30%)resp ectively. after the end of treating dry ing and milling of raw material mixing with different concentrations of sodium silicate(1%,0.7%,0.5%,0.2%,0.1%) whi le zinc o xide was added at fixed weight p ercenta ge. a disc sa mples was p repared after comp action and then fired by sintering temp eratures (1250, 1350) o c resp ectively.a surface morphology was st udied by using optical microscop e and measurements of apparent density and porosity was under taken to the sintered samples by using archimedes method.t he st udy showed that the microscopic images for samples surface showed that gr ains st art in convergence with other and gr ain size increasing with firin g temp erature and the best result of apperant density and p orosity at 0.5% concentration of sodium silicate . key words: ceramic insulator, density , p orosity. introduction ceramic material can be defined as “ in or ganic &non metallic materials that are artificially manufactured by high temp erature reaction” and sometimes heat and p ressure[1] . ceramic materials have the followin g generalized materials p rop erties, low density , low in toughness, high moduli, very hard , very high melting p oints, wear resistance, brittle, good thermal shock résistance, excellent electrical and thermal insulation, good relation of p rop erties at high temp eratures, and chemically st able[2]. the field of cer amic science could be broadly classified as traditional and advan ced ceramic. traditional cer amic are those mad e fro m naturally occurring materials like clays and minerals without required much refin ement characterized by mostly silicate base p orous microstructure that are quite coarse, non uniform and multip hase[3]advanced ceramic are develop ed by chemical sy nthesis, there are man mad e and can be made fro m high refined naturally occurring materials. the microstructures of these advanced cer amics were at least an order of magnitude finer and more homogenous and much less p orous t han those of their traditional counterp art [2]. some material like zinc o xide used to imp rove the chemical dur ability of some comp osition , zinc oxide is p roduced by direct o xidation of zinc metal and it uses a mineralized[4,5]. sodium silicate solution has som e char acterist ic p hy sical p rop erties which make them suitable for certain industries p urp ose. it appears that solution p referentially wets supp ly of sodium silicates; cer amic is decorated with glaze in comp osition of which the silicate solution serves the double p urp ose supp lying its share of sodium o xide and silica, and of keeping the other ingr edients in p osition till the sintering temp erature [6] sodium silicate are used as defloccu lated in the processing of raw clay and other mineral slurries. silicates reduce slurry viscosities making them easier to p ump and process. this help s in the removal of imp urities and provides saving in ener gy costs. sodium silicate is also used in clay slip cast ing lower ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 viscosities imp rove cast ing time because less water is need ed, firing times are r educes and final product is stronger and exhibits less shrinkage and low p orosity [7]. experime ntal procedure raw material treatment: kaolin and silica sand glass treated by washing them with hcl for time duration hour at room temp erature. the washed materials sep arated using filter p apers under sequence of op eration for dilution and filtering until ph valu e become 5. then the sep arated material milled usin g b all mill of p orcelain body for 7 hours and si eved to obtain p owder with p article size about 75 μm. s ample preparation: the raw materials used for the p reparation are k aolin, silica sand glass,and feldsp ar with p ercentage (45%, 25%, 30%) resp ectively. 2%of zinc o xide was added to the mixture followin g by mixing for 2 hours. the final mixture then divided into five group s related to concentration of sodium silicate (1%, 0.7%, 0.5%, 0.2%, and 0.1%). pva binder was p rep ared and app lied with 1%wt for each group . the mixture p rocess was carried und er heating 80 o c until get a slurry form, and then dried at 60 o c with continuous mixing for four hours unt il obtain agglomerated p owder. si ntering process: the final p owder was milled for 2 hour and sieved to size of 250 μm. these samp les were dried after p ressed with p ressure of 8m pa as disc form, the p repared samples sintered using different temp eratures(1250, 1350) o c with sinter time hours. optical microscope tests: the op tical microscopy was p rovided with digital camer a and comp uter sy stem (model nikon m e600, attached with digital camer a dxm /200f).this sy stem is used for p hotographing the samp les, before photographing, the surface of samples must be grinded. measurement of apparent density and apparent porosity. app arent density and porosity of sintered samples were determined by using archimedes m ethod [8].according to astm c20-18t,(american standard test m ethods)[9],which cover the determination of the followin g p rop erties of sintered samp les. 1 -dry weight (wd): samp les dried or sintered by heating them for 2 hour at 100 o c, to insure that residual moist ure must be removed, and determined the dry weight (wd) for t he samp les. 2 -saturation: place the samples in a beaker of distilled water and boil it for 2 hour. during the boiling p eriod , k eep them entirely covered with water, allow no contact with the heated botton of the container , keep the samples immerse in water for 12-24 hours before weighting . 3 -susp ended weight wsu: this weighting is accomplished by connectin g a copp er wire end at the downside of the balance and the other end of the terminals of the meshwork immersed in distilled water, the balance should be previously counter-blace. place the saturated samples on the susp ending meshwork for determin ing the susp ended weight wsu . 4 -saturated weight wsa: aft er determining the susp ended weight, blot the sample lightly with moist ened smooth linen or cott on cloth to remove all drop s of water from the surface and determine the saturated weight (wsa). excessive blott ing or (p ressing) will induce error by withdrawing water from the pores of the samp le. 5 -bulk density (ρb ) the bulk density (ρb )or app erant density of the sample is determined by using rhe followin g equation ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 water sud d b ww w lumeapperantvo dryweigh     where the volume of the liquid d isp lace, which is id entical to t he volume of the samp le. 6 app arent p orosity the app arent p orosity exp resses as p ercentage by using the exp ression app arent p orosity%= %100 etotalvolum lumeopenporevo app arent p orosity%= 100   suwsaw d wsaw result and discussion figures 1 and 2 revel the surface morphology of sample taken by the op tical microscope; it is known that ceramic color is typ ically gr ay, brownish or color less with vitreous luster. figure(1)shows the image taken to samples fired at 1250 o c for 2 hours have different surface st ructure and color than sample firing at 1350 o c in f igure (2). the images show in f ig.(1) include t he existence of white sp ot beside a small amount of gr ay region through a flux whi ch refers to uncomp leted melting of st ating materials and the r eduction amount of energy required to follow comp lete reaction between the composition with resp ect of time of firing. for samples firin g 1350 o c the image exp lain white and brown agglomerate which indicate p resent more than one phase and increase of the rate of reaction between melted material in comp osition firing at 1350 o c and decrease in p rose esp ecially when at sample (d1) which contains a concentration of sodium silicate as t able (1). physical char acterist ic p arameters (app arent density and app arent p orosity): app arent density and p orosity were calculated from the data, that measured by using archimed method from sa mples fired at temp erature 1250 o c, 1350 o c.the results of these group s are listed in table (1). fig (2) shows the images taken to samples surface that are fired at 1350 o c, the melt rate for the material in comp osition increases the chemical reaction and p hase transformation to the major cryst alline phase cordierite. it is well known t hat t he powder density is an indirect measure of the degree of the firin g reaction comp ound formation that takes p lace when a powder mixture is reacted during firing. it is related to the amount of p article growt h [10]. fi gures (3, 4) illust rate the behaviors of density and p orosity for samples with resp ect to firing temp eratures (1250, 1350) o c. conclusion in conclusion , this p aper describes the possibility of manufacturing a good cer amic body from local material and obtain agood p rop erties (density &p orosity)by adding 0.5% concentration of sodium silicate. re ference 1.choudhary, s.k.h.(1985), material scien ce and processes“ndian book,distributing co. 2. m ichel, w.b. (1997), fundamentals of cermics” international edition,the m c graw hill comp anies, inc.newy ork. 3. romasesho s. (1999), sience and technology of ceramic,p art 1, resonance , 4(8) ,p art 2, resonance,decemb er 4.singer,f.and sign er,s. s. (1963) industrial ceramic”chapman and hall ltd,london. ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 5.toy lor,j.r.and bull,a.c. (1986) ceramic glaze technolo gy ,by p ergamon p ress, newy ork,. 6.seli gman and williams.j. (1977) , low densily ceramics p roduced from p aper recy clirg residuals ,inst.m etals,28,297, 51-58 . 7.forge,v. ( 2004), advancein g the art of silicate ch emistry p .9, by pq corp oration 8.blythe, a.r. (1982) advance in physics31(5): 24-28. 9. gray , a.g. (1972) introduction to material scien ce m c.graw hill 10. she, j.h., j. (2002) prep aration of p orous cordierte ceramic usin g silica second ary resource (silican fumrs )fordust filtration p urp oses,m ater.sci., 37,125-131 table (1):apparent density (g/cm 3 ) and apparent porosity for these groups at different firing temperature s amples concentration of sodium silicate apparent densi ty apparent porosi ty 1250 o c 1350 o c 1250 o c 1350 o c a zero 1.179 1.339 9.3 0. 35 b 1% 1.194 1.51 11.6 0. 341 c 0.7% 1.205 1.398 13.9 0. 312 d 0.5% 1.462 1.37 17.1 0. 3 e 0.2% 1.6 1.63 13.8 1.1 f 0.1% 1.2 1.50 10.2 0. 7 ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 a b d c f e fig. (1) optical microscopic image for samples firing at 1250 o c with concentrations of sodium silicate show in table (1) ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 a1 b1 c1 d1 e1 f1 fig.(2) optical microscopic image for samples firing at 1350 o c with concentrations of sodium silicate show in table (1) ihjpas ibn alhaitham j. fo r pure & appl. sc i. vo l.23 (3 ) 2010 0 0.002 0.004 0.006 0.008 0.01 0.012 0 0.005 0.01 0.015 soduim silicate% p o ro s it y % 1.35 1.4 1.45 1.5 1.55 1.6 1.65 d e n s it y ( g /c m 3 ) 0 0.05 0.1 0.15 0.2 0 0.005 0.01 0.015 soduim si lica te % p o ro s it y % 0 0.5 1 1.5 2 d e n s it y (g /c m 3 ) fig.(3) the apparent density and porosity with concentration of sodium silicate for samples firing at 1350 o c fig.(4) the apparent density and porosity with concentration of sodium silicate for samples firing at 1250 o c ▲ density ● porosity ▲ density ● porosity ihjpas ihjpas microsoft word 248-256 ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |248   cardiovascular risk assessement in osteoporotic patients using osteoprotegerin as a reliable predictive biochemical marker noora w. rasheed dr.noora86@gmail.com al-rafidain university college ooroba j. taresh dept. of physics /college of education for pure science (ibn al-haitham) university of baghdad abstract some studies indicated a relationship between increased serum levels of osteoprotegerin with arterial calcification and as a result, it leads to the risk of cardiovascular disease. in our study group we selected patients with osteoporosis, with similar age and body mass index for the assessment of the relationship between cardiovascular disease and osteoprotegerin serum level. we took into account the analysis of correlation and association between the presence of distinct patterns of atherosclerosis and associated diseases like high blood pressure, diabetes mellitus, low hdl cholesterol, increased ldl cholesterol, increased triglycerides and was the case of presence of any type of dyslipidemia, in case of pre-existent treatment. objective of study was the assessment of osteoprotegerin value as predictive marker for cardiovascular and metabolic risk in osteoporotic patients. our results showed significant correlations of parathyroid hormone, osteocalcin and biochemical markers of bone with glucose metabolism and lipid were found in our research, maintaining crosstalk between calcium and biochemical markers of bone and cardiovascular risk. the serum level of osteoprotegerin has been shown to have a large predictive value for the metabolic syndrome as a cardiovascular risk standard in patients with osteoporosis. the osteoprotegerin serum levels were increased in the patients with metabolic syndrome as a protective response facing the atherosclerotic lesions. keywords: osteoprotegerin , cardiovascular disease, metabolic syndrome ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |249   1. introduction osteoporosis is a disorder characterized by decreased bone strength and increased risk of fracture, which occurs due to an imbalance in the bone remodeling process, where bone resorption exceeds bone formation [8]. several evidences have shown in the last years a possible correlation between cardiovascular disease and osteoporosis. studies regarding the cvd and cardiovascular mortality are associated with low bone mineral density (bmd) and bone fractures [1]. patients affected with osteoporosis have a higher risk of cvd than subjects with normal bone mass[2]. osteoprotegerin described as key regulators in metabolic bone disease and also have been discriminated as regulator in immunological function[3].the relationship between cardiovascular diseases and osteoprotegerin explains common risks such as age, lack of exercise, smoking and alcoholism [4]. similarly, inflammation plays a pivotal role in both atherosclerosis and osteoporosis.[5]. arterial calcification is a part of the atherosclerotic process leading to clinical cardiovascular disease. the presence of opg in atherosclerotic plaques has been described, and studies have shown that it is located in areas of calcification. some studies indicated a relationship between increased serum levels of osteoprotegerin with arterial calcification and as a result, it leads to the risk of cardiovascular disease [6]. vascular calcification and bone mineralization share a number of interesting anatomical and pathophysiological common features. in fact, the calcification of the arterial tissue is not just a passive process of precipitation or absorption of phosphate and calcium but it is a highly organized and regulated by mechanisms similar to those involved in bone mineralization [7]. in vitro studies show as the opg may be important for endothelial cells survival and inhibition of calcification; it appears that the opg protect from vascular calcification and elevated levels have been found in patients with cvd [9]. the aim of the study was to evaluate osteoprotegerin value as predictive marker for cardiovascular and metabolic risk in osteoporotic patients. 2. materials and methods analyse the subgroup of patients with measured serum osteoprotegerin seventy one women (48 postmenopausal and 23 premenopausal) in our study group we selected patients with osteoporosis, with similar age and body mass index in the elias hospital, bucharest romania, in order to evaluate the relationship between osteoprotegerin serum levels and the cardiovascular pathology. we took into account the analysis of correlation and association between the presence of distinct patterns of atherosclerosis and associated diseases like diabetes mellitus, high blood pressure, low hdl cholesterol, increased ldl cholesterol, increased triglycerides and was the case of presence of any type of dyslipidemia, in case of pre-existent treatment . for bone metabolism, total serum calcium, total alkaline phosphates (total alp), the parathyroid hormone (pth), 25-hydroxy vitamin d (25-oh vitamin d), serum osteocalcin, serum osteoprotegerin and serum betacrosslabs. serum osteocalcin, osteoprotegerin and 25-oh vitamin d were assessed using immunologic elisa methods, pth was analysed through a chemiluminometric method, while calcium and alp were measured using spectrophotometric methods. ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |250   ethics statement. our research involved human participants and has been approved by elias hospital ethics committe. all clinical investigation has been conducted acccording to the principle expressed in the declaration of helsink statistical analysis. data analysis are presented as mean and standard deviation. clinical characteristics were compared using the t student test. significant was defined at the 0.05 level of confidence. all calculations were performed using the statistical package for social science software (spss). 3. results and discussion serum total calcium did correlate to the time spent in postmenopausal period in these patients. comparing to the all group analysis, there is no meaningful difference between these findings: years since menopause are highly correlated to age. serum total calcium was found to be directly correlated with urinary calcium excretion, in accordance to the previously described correlation with pth and osteocalcin. calcemia was also significantly corelated with serum osteocalcin in all group analysis; instead in the opg group a correlation to the crosslaps has the same meaning, that serum total calcium is correlated to an increased bone turnover. serum 25 oh vitamin d levels were found to be negatively correlated with age (table 2) in the opg subgroup. increased age is a well known risk factor for low 25 (oh) vitamin d levels which was confirmed in our data.several factors found in the elderly people may be the cause of this aspect: low sun exposure due to invalidity, skin alteration with age, decreased activation of vitamin d in the kidney[4]. the inverse relationship between pth and 25 (oh) vitamin d was not significant anymore compared to the extended group; the explanation might be the lower case number or the lower prevalence of vitamin d defficiency in this subgroup which alleviates it. serum osteocalcin levels were found to be directly correlated to hdl-cholesterol in the opg subgroup (table 1), a relationship explained by the utility of osteocalcin in the evaluation of the cardiovascular risk, an intensively explored aspect in the latest years[10]. compared to the extended group, osteocalcin was no more correlated to blood calcium, pth levels and serum crosslaps the osteoprotegerin serum levels were found to be directly and significantly correlated to hdl –cholesterol, total alp and serum pth (table 1). these correlations sustain the protective role of the opg for cardiovascular diseases and, in the same time, the link to the bone metabolism. ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |251   table (1): a comparison between study subgroups according to the mets presence criteria among opg available subjects: clinical, lipid and glucose parameters biochemical parameter control group (no mets) study group (mets present) age* (years) 61 [19] 70 [17.5] bmi** (kg/m2) 24.5 [4.7] 26.3 [3.7] years since menopauze* 40 [45] 41 [48] blood glucose* (mg/dl) 87 [12] 107 [17] total cholesterol** (mg/dl) 200 (53.8) 231.8 (42.89) hdl cholesterol* (mg/dl) 56 [18] 58 [17] ldl cholesterol** (mg/dl) 119 (43.3) 138 (43.1) triglicerides** (mg/dl) 94.4 (35.1) 146.1 (52.5) ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |252   among calcium and bone biochemical markers, 25 (oh) vitamin d and osteoprotegerin serum levels were significantly different across the study groups (table3). table (2):a pearson correlation coefficients between calcium and bone, clinical, lipid andglucose parameters in osteoprotegerin subgroup age (yrs) bmi (kg/m2) years since menopau se (yrs) blood glucose (mg/dl) total cholest erol (mg/d l) hdl cholestero l (mg/dl) ldl cholester ol (mg/dl) triglice rides (mg/dl ) serum total calcium (mg/dl) 0.151 -0.176 -0.546* -0.200 -0.169 0.395 -0.283 -0.233 calcium urine excretion (mg/24 hrs) 0.098 0.268 0.373 0.080 -0.544 -0.425 -0.181 0.008 total alp (ui/l) 0.310 0.090 0.103 0.211 0.134 -0.103 0.090 0.143 pth (pg/ml) 0.065 0.128 0.090 0.491** 0.127 0.225 0.030 0.268* 25oh vit d (ng/ml) 0.358 ** -0.100 0.261 -0.152 -0.170 -0.101 -0.128 -0.267 osteocalcin (ng/ml) 0.194 -0.116 0.206 -0.011 0.035 0.344* -0.035 -0.136 crosslaps (ng/ml) 0.598 0.458 0.212 -0.101 0.040 0.830** -0.586 -0.008 osteoproteg erin (pmol/l) 0.101 0.078 -0.079 0.245 0.246 0.333* 0.264 0.023 *. correlation is significant at the 0.05 level (2-tailed). **. correlation is significant at the 0.01 level (2-tailed). ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |253   table( 3):a comparison between study subgroups according to the mets presence criteria among opg available subjects: bone markers parameters. osteoprotegerin levels were higher in the mets group it has been suggested that increased level of opg in patients with cardiovascular risk is due to the protective effect of osteoprotegerin, but mechanisms are still under debate. figure (1): correlation of opg (pmol/l) with the occurence of metabolic syndrome. biochemical parameter control group (without mets) study group (mets present) serum total ca** (mg/dl) 9.3 (0.5) 10 (0.8) 24 hrs urine calcium* (mg/24 hrs) 158 [151] 118 [168] total alp* (ui/l) 87 [90] 134 [109] ipth* (pg/ml) 77.2 [13.3] 80.6 [16.9] 25 ho vit d* (ng/ml) 30 [39] 17.4 [11.1] osteocalcin* (ng/ml) 10.4 [12.4] 10.1 [10.1] crosslaps* (ng/ml) 0.448 [0.137] 0.132 [0.389] osteoprotegerin baseline** (pmol/l) 5.15 (0.54) 5.6 (0.68) ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |254   figure (2): correlation of 25 (oh) vitamin d (ng/ml) with the occurence of metabolic syndrome. relationships between opg and 25 (oh) vitamin d with the presence of metabolic syndrome as an indicator for cardiovascular risk was further analysed in order to exclude aother cofounding factors. due to correlations between opg and total alp, pth and hdl cholesterol, suggesting that opg difference between mets segregated groups may be mediated by one of these parameters, a discriminant analysis was performed (table 4) . results showed a significant predictive value for opg and 25 (oh) vit d for mets. pth was not significantly predictive. cholesterol parameters were not included in this analyse because the significant difference found between mets subgroups were due to selection criteria (mets definition). table(4):astandardized canonical discriminant function coefficients and significance in predicting mets occurance coefficient sig. pth, pg/ml 0.144 0.193 opg (pmol/l) 0.673 0.022 25(oh) vit d (ng/ml) -0.765 0.009 excluding the non-osteoporotic patients, we exclude the influence of the bone mineral density status onto this evaluation. even the link is not very specific, we had a confirmation through our data of the possible predicted value of osteoprotegerin as an independent risk for cardiovascular diseases ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |255   figure (3): the pearson correlation’s coefficient between serum osteoprotegerin and pth (pg/ml) 4. conclusions significant correlations of parathyroid hormone, osteocalcin and biochemical markers of bone with glucose metabolism and lipid were found in our research, maintaining crosstalk between calcium and biochemical markers of bone and cardiovascular risk. the serum level of osteoprotegerin has been shown to have a large predictive value for the metabolic syndrome as a cardiovascular risk standard in patients with osteoporosis. the osteoprotegerin serum levels were increased in the patients with metabolic syndrome as a protective response facing the atherosclerotic lesions. 25 hydroxy vitamin d serum levels have great predictive values of cardiovascular and metabolic risk in our research maintaining the broad role of vitamin d outside bone metabolism. references [1] v. baldini; m. mastropasqua; cm. francucci; e d'erasmo., cardiovascular disease and osteoporosis. 2005;28:69-72. [2] r. baron; anatomy and ultrastructure of bone. in: favus mj, ed. primer on the metabolic bone diseases and disorders of mineral metabolism. 2nd ed. new york: lippincott, raven 1993:3-9 [3] d. l.bartel, d.; d. t., and m., k. t. the musculoskeletal system. in orthopaedic biomechanics: mechanics and design in musculoskeletal systems. pearson.2006;22. [4] p.assantachai, --w.angkamat, --p. pongpim, --c.weattayasuthum, --et al. risk factors of osteoporosis in institutionalized older thai people. 2006:17:1096-1102. [5] i .samy; mcfarlane, et al. osteoporosis and cardiovascular disease.2004, 23;1–10. [6] g. j.atkins; k. j, welldon and p. halbout, , et. al.. strontium ranelate treatment of human primary osteoblasts promotes an osteocyte-like phenotype while eliciting an osteoprotegerin response. 2009;20: 653–664. ihsciconf 2017 special issue ibn al-haitham journal for pure and applied science https://doi.org/ 10.30526/2017.ihsciconf.1798 for more information about the conference please visit the websites: http://www.ihsciconf.org/conf/   www.ihsciconf.org   chemistry |256   [7 ] jb. arlet; m .courbebaisse; g .chatellier and d. eladari, et al. relationship between vitamin d deficiency and bone fragility in sickle cell disease: a cohort study of 56 adults.2013;52:206-211. [8] adler ra. osteoporosis in men. in: adler ra, editor. osteoporosis — pathophysiology and clinical management. 2nd edition.2010; 545–57. [9] jf.aloia; sa.talwar; s .pollack; m .feuerman; yeh jk. optimal vitamin d status and serum parathyroid hormone concentrations in african american women.2006;84(3): 602. [10] american society for bone mineral research president’s committee on nomenclature. proposed standard nomenclature for new tumor necrosis factor family members involved in the regulation of bone resorption. 2000     ihjpas. 53 (3)2022 206 this work is licensed under a creative commons attribution 4.0 international license. iterative method for solving a nonlinear fourth order integro-differential equation areej salah mohammed department of mathematics, college of education for pure science, ibn al haitham,university of baghdad, iraq. areej.s.m@ihcoedu.uobaghdad.edu.iq abstract this study presents the execution of an iterative technique suggested by temimi and ansari (ta) method to approximate solutions to a boundary value problem of a 4th-order nonlinear integro-differential equation (4th-onide) of the type kirchhoff which appears in the study of transverse vibration of hinged shafts. this problem is difficult to solve because there is a nonlinear term under the integral sign, however, a number of authors have suggested iterative methods for solving this type of equation. the solution is obtained as a series that merges with the exact solution. two examples are solved by ta method, the results showed that the proposed technique was effective, accurate, and reliable. also, for greater reliability, the approximate solutions were compared with the classic runge-kutta method (rk4m) where good agreements were observed. for more accuracy the maximum error remainder was found, and the absolute error was computed between the semi-analytical method and the numerical method rk4m. mathematica® 11 was used as a program for calculations. keywords an iterative technique, approximate solutions, fourth order integro-differential equation, maximum error remainder. 1.introduction many real-life phenomena engineering and physics are mathematically modeled into functional equations. many mathematical formulas for physical phenomena and fluid dynamics contain differential and integral equations [1]. [2]. in this paper, the integro-differential equation of the fourth order of kirchhoff type is considered as ibn al haitham journal for pure and applied sciences journal homepage: http://jih.uobaghdad.edu.iq/index.php/j/index doi: 10.30526/35.4.2776 article history: received 16 january 2022, accepted 3 february 2022, published in october 2022. https://creativecommons.org/licenses/by/4.0/ mailto:areej.s.m@ihcoedu.uobaghdad.edu.iq ihjpas. 53 (3)2022 207 𝜐(4)(𝑡)−𝛿𝜐′′(𝑡)− 2 𝐵 ∫ [𝜐′(𝑡)] 2 𝑑𝑡 𝐵 0 𝜐′′(𝑡)=𝑘(𝑡), 0<𝑡<𝐵, 𝜐(0)=𝜐(𝐵)=𝜐′′(0)=𝜐′′(𝐵)=0, ] (1) where 𝜐(𝑡) represents the constant deviation of the shafts, 𝑘(𝑡) is a continuous function defined over [0, 𝐵]and 𝛿 and 𝐵 are positive constants. this type of problem represents a bending equilibrium model for expandable shafts that are simply supported on nonlinear bases. the force that the foundation applies to the shafts is represented by the function, 𝑘(𝑡). small changes in shafts length and their effects are represented by : 2 𝐵 ∫ [𝜐′(𝑡)]2𝑑𝑡 𝐵 0 [3]. it is obvious that it is difficult to find the exact solution to equation (1), so many numerical and semi-analytical methods have been developed, such as [4] reduced the order of the equation to find the root of a nonlinear equation and solve it by newton's method. [5] used the optimal homotopy asymptotic strategy to solve equation (1) and proved the efficacy of the procedure by comparing it with a finite element technique. [6] proposed a numerical scheme for solving equation (1) by transforming the problem into a nonlinear algebraic system and then solving it in an iterative method with the collocation technique. [7] suggested an iterative method namely tamimi and ansari (ta) method for solving nonlinear equations, and this technique was applied to solve numerous differential equations, for example, korteweg-de vries equations [8], thin-film flow problems [9], falkner-skan problem [10]. in this work, the ta method is used to solve the 4th-onide of the type kirchhoff which appears in the study of transverse vibration of hinged shafts. the results acquired from the method showed that ta method is accurate, fast, and convenient. two examples are solved and the results obtained are compared with the rk4m method, and the maximum error reminder is calculated. this article is arranged as follows: section 2 provides a clear formulation of the iterative method in general and specifically on equation (1); section 3 illustrates the effectiveness of the method with various examples before giving a brief conclusion in section 4. 1. the proposed method to clarify the fundamental thought of ta method. let us consider the general equation ℒ(υ(t)) + ℵ(υ(t)) + g(t) = 0, (2) with boundary conditions ℬ (υ, d𝜐 𝑑𝑡 ) = 0, where υ is unknown function, ℒ is the linear operator, ℵ is the nonlinear operator and g is a known function. assuming that υ0(𝑡) is a solution of equation (3) of the initial condition ℒ(υ0(𝑡)) + g(t) = 0, with ℬ (υ0, d𝜐0 𝑑𝑡 ) = 0 . (3) to find the next iteration, we resolve the following equation: ℒ(υ1(𝑡)) + ℵ(υ0(𝑡)) + g(t) = 0, ℬ (υ1, d𝜐1 𝑑𝑡 ) = 0. ihjpas. 53 (3)2022 208 thus, an iterative procedure can be an effective solution to the following problem, ℒ(υ𝑛+1(𝑡)) + ℵ(υ𝑛(𝑡)) + g(t) = 0, ℬ (υ𝑛+1, d𝜐𝑛+1 𝑑𝑡 ) = 0. (4) each of 𝜐𝑖 are solutions to equation (1) [7]. we will apply the steps of the method in solving equation (1), so it can be formulated as: ℒ(υ(t))−δr(υ(t))− 2 b (∫ ℵ(υ(t))dt) b 0 r(υ(t))=k(t), 0