Structural Transition Magnetic Properties

91 ISSN 2086-5953 STRUCTURAL TRANSITION AND MAGNETIC PROPERTIES OF ZN-DOPED FE 3 O 4 BY CO-PRECIPICATION METHOD Sigit Tri Wicaksono 1 , Haizan 2 1,2 Materials and Metallurgical Engineering, FTI, ITS Jl. T.Industri Kampus ITS Sukolilo Surabaya 60111 Email: sigitmat-eng.its.ac.id ABSTRACT Magnetic properties of Zn-doped Fe 3 O 4 have been synthesis by using co-precipitation method at low temperature. X-Ray diffraction result shows that the sample was crystalline structure and form Zn x Fe 3-x O 4 stoichiometry. Further refinement of diffractions data show that the crystal structure has change from cubic to hexagonal structure and lattice volume decrease 10 times by increasing of doping and occur . The magnetic properties of sample have also studied. The results show that Zn x Fe 3-x O 4 was exhibit ferrimagnetic characteristic at room temperature. Keywords: Co-precipitation method, doping, magnetic properties. 1 INTRODUCTION Lie and Kuo [1] were conduct toward the doping of ZnO into Fe3O4 to see the effect of Fe3O4 magnetic resistance using mechanical alloying method. They succeed to exhibit the paramagnetism phenomenon in room temperature. In pervious study we have synthesis the manganese- based magnetic materials to exhibit the magnetic properties of Mn 3 O 4 with nano-Fe3O4 by using co-precipitation method. The results show that sample exhibit the same condition as paramagnetism phenomenon. In this study we have doped Fe3O4 with ZnO by the same method. The sample exhibit the Zn x Fe 3-x O 4 stoichiometry as shown form X-ray diffraction pattern. Further refinement of diffractions data by using Rietica program show that there was transition phenomenon of crystal structure from cubic to hexagonal lattice. Another phenomenon was decreasing of lattice volume 10 times by increasing of doping. The magnetic properties of sample such as Magnetic saturation, magnetic remanent, and coercivity have also studied. The results show that Magnetic saturation Zn x Fe 3-x O 4 was decrease by increasing of doping and exhibit ferrimagnetic characteristic at room temperature. 2 EXPERIMENTAL PROCEDURE Magnetite Fe3O4 as the parrent phase has synthezed by chemical procedure as done in previous research [2] by following chemical procedures: 3Fe3O4+8HCl 2FeCl+FeCl2+3Fe2O3+3H ₂ O+H 2.1 ZnO + 2HCl  ZnCl2 + H2O 2.2 2FeCl2+FeCl3 + ZnCl2 + NH 4 OH  Zn x Fe 3-x O 4 + H 2 O + NH 4 Cl + H 2 + Cl 2 2.3 3 RESULT

3.1 Structural Transition

Diffraction pattern of particles Zn x Fe 3- x O 4 0x2 synthesized by co-precipitation method shown in Figure 1. Analysis of search match to sample with the variation of x = 0 parent sample has the same diffraction pattern with diffraction pattern Fe3O4 PDF No. 11-0614. While the sample with the variation of x = 1 has the same diffraction pattern with diffraction pattern ZnFe2O4 PDF No. 10-0467. Final sample with the variation of x = 2 has the same diffraction pattern of ZnO PDF No. 05-0664 Figure 1. X-ray diffraction patteron of Zn x Fe 3-x O 4 0x2 ISSN 2086-5953 Table 1. shows that the sample with the variation of 0x1 have lattice length a, b, and c are nearly equal which is about 8.4 Å. While the sample with x = 2 the lattice length a and b were the same which was about 3.25 Å and c lattice length of about 5.2 Å. The length of the lattice parameters a, b and c are distinct form the tetrabonal structure of spinel. The transition structure of Zn x Fe 3-x O 4 from cubic to hexagonal because of the substitution of Zn ions, in which Zn ions tend to occupy octahedral positions. The transition structure also resulted in lattice volume decreases, because the length of a and b lattice decreased higher than the long decline in the lattice c [2] Further analysis of refinement shows that the samples with cubic spinel structure variation of x = 0 which has the smallest crystal size about 99.86 nm. Samples with hexagonal spinel structure x = 2 has the largest crystal size about 32.27 nm. Crystal size difference is influenced by the radius of the constituent ions. The radius of the ion Fe 2+, Fe3+ and Zn2+ are 7.6 Å, 7.0 Å and 6.2 Å respectively. It can be observed that the ion radius of Zn2+ ion close to the radius of Fe 3+. This causes Zn 2+ occupy the tetrahedral Fe3+ ion.

3.2 Magnetic Properties

According to picture 1 and its data extraction shown on table2, shows that the parent sample x = 0 has a saturation magnetization much higher than the samples doped with ZnO x = 1 and x = 2. The decline trend in the value of magnetization saturation of the doped sample could theoretically occur because at this range, the value of the total magnetic moment also decreases, especially for sample Zn2FeO4 saturation magnetization caused by VSM measurements performed at room temperature, while ZnO is diamagnetic material at room temperature. Figure 2. Magnetization curve Results of measurement Hc, Ms and Mr show that in general pattern of particle saturation magnetitasi Zn x Fe 3-x O 4 tend to follow the same pattern with the pattern of magnetization on the predicted previously. Magnetic a material is closely related to magnetic domain, domain either singular or plural domain. In general, the smaller the crystal size of a material, the more toward a single domain state. Conversely the greater the crystal size, will be more towards a situation plural domain. At the regional domain single-value field coercivity also has narrowed in line with decreasing crystal size, but the crystal size that very small below the critical size of a material which is ferro or ferrimagnetic turn into superparamagnetik. Other magnetic properties of Zn x Fe 3-x O 4 is the remanent magnetization Mr. Mr follow the same pattern with the pattern of Ms and Hc. The greater the value of remanent magnetization, the greater the larger the field required to eliminate them. This happens because the remanent magnetization is the amount of residual magnetization which is still owned by a material when it is not influenced by the external field. 4 CONCLUSION AND DISCUSSION X-Ray diffraction result shows that the sample was crystalline structure and form Zn x Fe 3- x O 4 stoichiometry. Further refinement of diffractions data show that the crystal structure has change from cubic to hexagonal structure and lattice volume decrease 10 times by increasing of doping and occur . The results show that Zn x Fe 3-x O 4 was exhibit ferrimagnetic characteristic at room temperature ISSN 2086-5953 REFERENCES [1] Lie, C.T. Kuo, P.C. 2002. Effect doping on the magnetoresistance of sintered Fe 3 O 4 ferrites. Journal Magnetism and Magnetic Material. [2] Sigit Tri W, Darminto.2008. Synthesis and Characterization of Nano magnetic Mn 3-x M x O 4 , 0 x 1 M= Ni,Fe, ITS Surabaya [3] Sunaryono, Darminto.2008. Synthesis and Characterization of magneto- elastisitas hydrogel nano magnetic Fe 3 O 4 ITS Surabaya [4] Cammarata,.Edelstein.1997. Nanomaterials: Synthesis, Properties, and Aplications . Institut of Physics Publishing Briston and Philadelphia. [5] R. W. Chantrell and K. O‘Grady, ―The magnetic properties of fine particles,‖ in AppliedMagnetism , p. 113, Kluwer Academic Publishers, Dordrecht, The Netherlands, 1994. [6] H. Ehrhardt, S. J. Campbell, and M. Hofmann, ―Magnetism ofthe nanostructured spinel zinc ferrite,‖ Scripta Materialia, vol. 48, no. 8, pp. 1141 –1146, 2003. [7] C. Upadhyay, H. C. Verma, V. Sathe, and A. V. Pimpale, ―Effect of size and synthesis route on the magnetic properties of chemically prepared nanosize ZnFe 2 O 4 ,‖ Journal ofMagnetism and Magnetic Materials , vol. 312, no. 2, pp. 271 –279, 2007. ISSN 2086-5953 [This page is intentionally left blank] 95 ISSN 2086-5953 THREE DIMENSION SIMULATION OF INJECTION-COMPRESSION MOLDING PROCESS OF DISK Bambang Arip Dwiyantoro 1,2 , Shiu Wu Chau 1 1 Department of Mechanical Engineering, National Taiwan University of Science and Technology Taipei 10607, Taiwan, Republic of China 2 Department of Mechanical Engineering, Institute of Technology Sepuluh Nopember Surabaya, 60111, Indonesia Email: D9603803me.ntust.edu.tw, bambangadsme.its.ac.id ABSTRACT Abstract should be written using Times New Roman 10, in two column format, and up to 200 words. The closer the authors stick to this guideline, the better the quaility of the proceeding and the less the time uninterestingly spent by the organizing committee. A numerical model for the fully three-dimensional simulation of melt filling in an injection-compression process is proposed in this paper, where a moving grid strategy is employed. Similar to other fully three- dimensional methods, the fully three-dimensional Navier-Stokes equations are solved together with the front transport equation using a front capturing approach. To avoid the difficulty in specifying gas outlet required by SIMPLE-type algorithms with incoming melt, the escape of air is modeled through source terms described by a compressible model. Filling predictions of disk part are conducted to demonstrate the advantages of proposed scheme in simulating injection-compression processes. After conducting several computations under different processing conditions, it was found that the compression speed and compression stroke are the two factors affecting the molding pressure most significantly. The simulated molding pressures were also compared with those required by conventional injection molding CIM assuming the same entrance flow rate. Using higher switch time, lower compression speed and higher compression stroke will result in lower cavity pressures. Keywords: three-dimensional, moving grid, disk part, injection-compression process 1 INTRODUCTION Injection molding, being one of most important polymer processing operations, consists of three major stages: filling, packing, and cooling. In a pure compression molding process [1-4], polymer melt is compressed to flow by moving the movable platen of the mold to complete melt filling. The melt is then continued to be compressed by the pressure exerted from the mold wall of the core side. This process provides a more uniform pressure along the cavity wal and requires only a low molding pressure for the postfilling process. The injection-compression molding [1-3], combining conventional injection molding and compression molding, has been developed to incorporate the advantages of both molding processes. An injection-compression molding machine is constructed by modifying an injection molding machine with an additional compression system. The compression stage is usually introduced after partial melt filling of the cavity. Generally speaking, the injection-compression molding process retains the advantages of conventional injection molding, such as high production rate, steady process operation, and easy process automation. Despite of some related researches in the injection-compression molding, the full understanding of the optimized control over the injection-compression techniques is still far from completeness. Form the engineering point of view, numerical tools are essential to locate the adequate processing parameters due to the complexity of this highly nonlinear problem. 2 MODEL AND ANALYSIS

2.1 Fully Three-Dimensional Model