Research Journal of Chemical Sciences ______________________________________________ ISSN 2231-606X Vol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 18 A Simple and Effective method of the Synthesis of Nanosized Cu0.5Zn0.5FeParticlesAvnish Kumar Arora and Ritu Department of Chemistry, Maharishi Markendeshwer University, Mullana -133203, Haryana, INDIAAvailable online at: www.isca.in Received 24th June 2013, revised 1st August 2013, accepted 14th August 2013Abstract Nanosized Copper-zinc ferrites Cu0.5Zn0.5Fe have been synthesized by aqueous precipitation method and characterized by using XRD (X-ray diffraction), TGA/DTA (Thermo gravimetric analysis), SEM (Scanning Electron Microscopy)/ TEM (Transmission Electron Microscopy) and magnetic measurements by using VSM (vibrating sample magnetometer). XRD studies confirm the formation of cubic spinnel structure. SEM (scanning electron microscopy)/ TEM (transmission electron microscopy) was used to characterize the microstructure of the ferrite samples. A homogeneous and fine grain microstructure was found. Magnetic measurements shows that Ni05Cu0.5Fe is super paramagnetic in nature at room temperature and hence used in magnetic device. The particle size of synthesized Cu05Zn0.5Fe varied from 18nm to 68nm which is good agreement of the theoretically predicted size of nanomaterials. The method is easier more effective and convenient in comparison to the known methods of the synthesis Cu05Zn0.5Fe nano materials like combustion synthesis, thermal cracking and conventional ceramic methods. Keywords: Nanosized, Spinel, ferrites, Super paramagnetism, copper – zinc Ferrite (Cu05Zn0.5Fe) Introduction Cu05Zn0.5Fe is a spinel ferrite. The general formula of the spinel ferrite is MeFe where Me usually represents one or, in mixed Ferrites more than one of the divalent transition metals Mn, Fe, Cu, Ni, Zn, Ca or Mg and Cd. Other combinations of equivalent valency are possible and it is also possible to replace some or all the trivalent iron ions with other trivalent metal ions1-6. Ferrites are the fundamental functional materials of electronic industry. Ferrites can be cast into complex shapes and can be ground and will take fine finish. Ferrites are ceramic materials. Ferrites may be defined as magnetic materials composed of oxide containing ferric ions as the main constituent. This term is often restricted to materials which have cubic crystal structure of spinel but now days it is also applied to magnetic oxides. Ferrous ferrites are an example of naturally occurring ferrite. Magnetic properties in ferrites arise from interactions between metallic ions occupying particular positions relative to oxygen ion in the crystal structure of the oxide.In majority of the present day magnetically soft ferrite the crystal structure is cubic and has the form of mineral spinel. Cu05Zn0.5Fe is developed for a wider range of applications where high permeability is the main requirement. The ferrite core memory was the basis of the IBM 360 computer which is standard for industry6-15. The application started in the field of telephony transmission operating in large frequency range from about 40 KHz. Most important use of ferrite is for video recorder15-21. Today ferrites are used as noise filters in power lines of electronic equipments22. Ferrites are easy to manufacture, low costs, small volume, high efficiency and with greater uniformity have applications in ceramic magnet as medical treatment, filter inductors, magnetic amplifiers, transformers, antenna cores, magnetic memories and flyback transformers. Material and Methods Chemicals: All chemicals used in the experiment are analytic reagent grade. Ferric nitrate Fe (NO)3, Copper NitrateCu (NO, Zn (NO2 and liquor ammonia were purchased from Merck, India. Deionized water was used throughout the experiment. Synthesis of Cu 0.5Zn0.5Fe: 200 ml of 0.5 M solution of Fe(NO was mixed with 200 ml of 0.5M solution of Zn(NO2 and 200 ml of 0.5M solution of Cu(NO2 then aqueous ammonia was added drop wise with constant stirring until the pH of the solution reached to 10. The precipitate thus obtained were filtered on buckner funnel and washed several times with distilled water. The precipitate was dried in oven at 70C for 24 hrs and was calcined at 600C in a muffle furnance for 5 hours. Obtained material was ground and sieved through 100 mesh size sieve. Equipments: An X – ray measurement was carried out using X-ray diffractometer system Philips PW 11/90, with nickel filtered CuK (l = 1.5405 Å). The crystalline size of Zinc ferrite was calculated using Scherrer equation. t = K/ B cos Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 19 Where t is the average crystallite size of the phase under investigation, K is the Scherrer constant (0.89), is the wave length of X – ray beam used, B is the full-with half maximum (FWHM) of diffraction (in radians) and is the Bragg’s angle. Transmission electron micrograph (TEM) were recorded on Hitachi H7500. The samples were dispersed in ethanol and then treated ultrasonically in order dispersed individual particles over a gold grid. The surface morphology of Ni05Cu0.5Fe4 prepared by precipitation method was investigated by using scanning Electron Microscope Quanta 200 FEG (FEI Netherlands). The magnetic properties of the solid were measured at room temperature using a Vibrating sample Magnetometer Model 155. Results and Discussion X-ray studies: The X-ray diffraction pattern of synthesizedCu05Zn0.5Fe nano particlesis depicted in figure 1. X-ray diffraction pattern of Cu05Zn0.5Fepure indicated that Cu-Zn ferrite in the form of Cu05Zn0.5Fe (figure 1). In X-ray diffraction, some prominent peaks were considered and corresponding d-values were compared with the standard i.e. JCPDS (Joint Committee on Powder Diffraction Standards) (File card 86.) Table 1. X-ray diffraction shows that metal oxide is pure Cu05Zn0.5Fe having cubic spinal structure . Table1 gave a verification of well defined crystalline phase of spinel structure of Cu-Zn ferrite. The average crystallite size was determined from the broadening of the most intense peaks using Debye Scherer equation (Cullity 2001) and values shown in table 1 and it also supports the SEM/TEM observations. The crystallite size was found within 18-68 nm. The powder x-ray patterns confirm the single phase spinel structure for synthesized material. Thickness of the crystal has been calculated using Debye Scherrer’s formula and it support the TEM observations. Thermal Analysis: Thermal analysis includes a group of techniques in which a physical property of a substance is measured as a function of temperature or time while the substance is subjected to a controlled temperature programme. The analysis involves thermogravity (TG), differential thermal analysis (DTA) and derivative Thermogravimetry (DTG). Thermal Gravimetric studies of the calcined oxides prepared were done between a temperature range of 10-1000C under Natmosphere. The TGA/DTA curves of the oxides are shown in figure 2. The maximum total weight loss observed for Nickel oxide and their corresponding temperature is summarized in table 2 . Results showed that in the synthesized oxides shows some weight loss and ferrite undergoing decomposition, dehydration or any physical change. In DTA curve also, there is exothermic peak which shows phase transition, solid state reach on any chemical reaction occurred during heating treatment. SEM/TEM studies: SEM studies were carried out to study the morphology of the sample figure (3a,b) shows the SEM micrographs of Cu05Zn0.5Fe. The micrographs of Cu05Zn0.5Fe (figure 3a,b) displayed spherical particles with high agglomeration. TEM studies were carried out to find the exact size of the synthesizedCu05Zn0.5Fe nanoparticles fig. (4a,b,c,d,e,f,g) shows the TEM images of the synthesized Cu05Zn0.5Fe nanoparticles. It shows that the size of the obtained nano particles is in the range 18-68 nm. Most of the particles are in the range 21-50 nm. TEM images indicate that Cu05Zn0.5Fe samples were all spherical particles with uniform grain size distribution. Magnetic measurements: Magnetic properties of nanometer sized particles have attracted considerable attention in recent years because of their unique properties. The size of the magnetic particles decreases below a critical length. Domain formation was no longer energetically favoured and the particle existed as a single domain. Magnetic nanoparticle has aroused increasing interest among researchers of various fields due to their extensive applications such as in information storage system, medical diagnostics, ferrofluid technology etc. This is mainly because of the properties of nanoparticles differ from those of the corresponding bulk material. The magnetic measurements of Cu05Zn0.5Fewas carried out at room temperature and it has been shown that the magnetic measurements shows that the prepared Cu05Zn0.5Fe nanoparticles posses good super paramagnetic behavior at room temperature (300K) with saturation magnetization MS value 51 (figure 5). Previously reported values of MS For Cu05Zn0.5Fe Nanoparticles prepared by various methods has been reported in table (2). The value of MS ranging from 15-90 emu/g shows that Ms strongly depends on the methods of synthesis. This MS value at room temperature is good and comparable with methods of synthesis as thermal decomposition method (MS value 43 at 300 K and MS value 68.5 emug-1 at 10k) ball milling (MS value 20.7 in at 4.2k) and other co-precipitation routes which shows a maximum MS 47.8 at 4.2 k (figure 5). Magnetic Hysteresis curve clearly indicate the soft nature of the prepared sample saturation magnetization ms value increase with time. Conclusion Cu05Zn0.5Fe nanoparticle with cubic spinel structure is synthesized successfully by aqueous precipitation method. From SEM/TEM studies it is found that particles have average size 18-68nm. Magnetic measurements shows that Cu05Zn0.5Fesuper paramagnetic in nature having saturation magnetization (MS) value 51 emu/g. This method is beneficial over the existing methods of synthesis of nano particles because other methods require expensive materials, highly skilled labour and specialized instrumentation. Therefore, the proposed precipitation method is cheaper, easier, very promising and may have extensive applications. Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 20 Table-1 X-RAY Diffraction Data for Cu05Zn0.5FeS. No. d= / 2sin(Observed) d= / 2sin(Reported) I/IX100% (Observed) I/IX100%(Reported) 1. 2.749624311 2.749624302 55.75575576 55.75575570 2. 2.814146374 2.814146360 39.33933933 39.33933930 3. 3.674620393 3.674620378 99.99999999 99.99999999 4. 2.311895273 2.311895271 19.7197197 19.7197187 5. 1.91106274 1.911062777 28.5285285 28.5285283 6. 1.837310919 1.837310900 25.3253253 25.3253245 7. 1.580591523 1.580591521 3.6036036 3.60360366 8. 1.4772508 1.477250000 1.5015015 1.50150166 Table-2 Observations of Weight Loss forCu05zn0.5feo at Corresponding Temperature RangeSr.No. Maximum % loss in weight Temperature range 1 1.696% 26.68-907.73 Table-3 Practical Size of Synthesized Cu05Zn0.5Fe at Different Scales S.No. Scale (20nm) Scale (20nm) Scale (50nm) Scale (50nm) Scale (50nm) Scale (100nm) Scale (100nm) 1 28.42105263 18 41.6667 41.891891 29.166666 25 25.641025 2 50.52631579 21.7931 47.9166 21.621621 41.666666 21.4285 25.641025 3 60 36.2413 56.25 68 54.166666 22.8571 30.769230 4 31.57894737 50.3793 64.5833 36.486486 54.166666 37.2857 33.333333 5 44.21052632 24.1379 50 33.783783 66.666666 40.1428 33.333333 6 36.84210526 25.5517 52.0833 18.918918 43.75 28.5714 33.333333 7 57.89473684 18 39.5833 31.081081 41.6666 35.7142 38.461538 8 28.42105263 32.7931 41.6667 36.486486 29.166666 28.5714 41.02564 9 50.52631579 36.2413 47.9166 33.783783 41.666666 28.5714 18 10 60 20.3793 56.25 18.918918 54.166666 25 20.512820 Range 28.42105263 nm to 60 nm 18nm to50.3793nm 41.6667nm to 64.5833nm 18.918918nm to 68nm 29.166666nm to 66.666666nm 21.4285nm to 40.1428nm 17 nm to 41.02564 nm Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 21 Figure-1 X-Ray diffraction spectra of Cu05Zn0.5Fe Particles Figure-2 TGA-DTA of Cu05Zn0.5FeParticles Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 22 Figure-3(a) SEM micrographs of Cu05Zn0.5Fe Particles Figure-3(b) SEM micrographs of Cu05Zn0.5Fe Particles Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 23 Figure-4 (a) Figure-4 (b) Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 24 Figure-4 (c) Figure-4 (d) Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 25 Figure-4 (e) Figure-4 (f) Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 26 Figure-4 (g) Figure-4 (h) Figure-4 (a, b, c, d, e, f, g, h) TEM micrographs of Cu05Zn0.5Fe Particles Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. International Science Congress Association 27 Figure-5 Magnetic measurement of synthesized Cu05Zn0.5Fe particles Research Journal of Chemical Sciences ___________________________________________________________ ISSN 2231-606XVol. 3(8), 18-28, August (2013) Res. J. Chem. Sci. 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