Purpose: The aim of the present work is the microstructure characterization of commercial powder BaFe12O19
(as-prepared) and composite material with BaFe12O19 powders and polymer matrix, using XRD (X-Ray
Diffraction) and SEM (Scanning Electron Microscopy) methods.
Design/methodology/approach: The morphology of barium ferrite powders and a fracture surface of the
examined composite material was realized by using the scanning electron microscope. The methods of Xray
diffraction were used for the qualitative phase analysis. The parameters of diffraction line profiles were
determined by PRO-FIT Toraya procedure.
Findings: The X-ray diffraction analysis permitted on identification the BaFe12O19 and Fe2O3 phases in an
examined material. Basing on Toraya method is determination of: lattice parameters, crystallite size (D) and the
lattice distortion (). Distribution of powders of barium ferrite in polymer matrix is irregular and powder
particles have irregular shapes and dimensions.
Research limitations/implications: For future research the X-ray analysis should be performed by the Rietveld
method, which allows to characterization the microstructure of tested material and verification of its qualitative
phase composition.
Originality/value: The applied Toraya method of structure analysis appeared to be very useful in the
microstructure analysis

Babilas, R.

Dercz, Grzegorz

Nowosielski, R.

Pająk, Lucjan

Journal of Achievements of Materials and Manufacturing Engineering

English

Repozytorium Uniwersytetu Śląskiego RE-BUŚ

             Title: Microstructure of composite material with powders of barium ferrite  Author: R. Nowosielski, R. Babilas, Grzegorz Dercz, Lucjan Pająk  Citation style: Nowosielski R., Babilas R., Dercz Grzegorz, Pająk Lucjan. (2006). Microstructure of composite material with powders of barium ferrite. "Journal of Achievements in Materials and Manufacturing Engineering" (Vol. 17, iss. 1/2 (2006), s. 117-120). © Copyright by International OCSCO World Press. All rights reserved. 2006VOLUME 17ISSUE 1-2July-August2006Short paper 117of Achievements in Materialsand Manufacturing EngineeringMicrostructure of composite material with powders of barium ferriteR. Nowosielski a, R. Babilas a,*, G. Dercz b, L. Pająk ba Division of Nanocrystalline and Functional Materials and Sustainable  Pro-ecological Technologies, Institute of Engineering Materials and Biomaterials,  Silesian University of Technology, ul. Konarskiego 18a, 44-100 Gliwice, Polandb Institute of Materials Science, University of Silesia,  ul. Bankowa 12, 40-007 Katowice, Poland *  Corresponding author: E-mail address: rafal.babilas@polsl.plReceived 15.03.2006; accepted in revised form 30.04.2006MaterialsAbstrActPurpose: The aim of the present work is the microstructure characterization of commercial powder BaFe12O19 (as-prepared) and composite material with BaFe12O19 powders and polymer matrix, using XRD (X-Ray Diffraction) and SEM (Scanning Electron Microscopy) methods.Design/methodology/approach: The morphology of barium ferrite powders and a fracture surface of the examined composite material was realized by using the scanning electron microscope. The methods of X-ray diffraction were used for the qualitative phase analysis. The parameters of diffraction line profiles were determined by PRO-FIT Toraya procedure.Findings: The X-ray diffraction analysis permitted on identification the BaFe12O19 and Fe2O3 phases in an examined material. Basing on Toraya method is determination of: lattice parameters, crystallite size (D) and the lattice distortion (<∆a/a>). Distribution of powders of barium ferrite in polymer matrix is irregular and powder particles have irregular shapes and dimensions.Research limitations/implications: For future research the X-ray analysis should be performed by the Rietveld method, which allows to characterization the microstructure of tested material and verification of its qualitative phase composition.Originality/value: The applied Toraya method of structure analysis appeared to be very useful in the microstructure analysis.Keywords: Composites; X-ray phase analysis; Toraya procedure; Barium ferrite1. Introduction Composite materials are practically used in all branches of industry. Ferrite-based materials are the most widely used as magnetic materials. They have excellent chemical stability and are relatively cheap to produce. Ferrite magnets such as barium ferrites have applications as accumulating and processing of information [1-7]. Barium ferrites are sintered from barium carbonates and iron oxides. They was produced by methods of powders metallurgy. First stage of process of receiving the barium ferrites is called as ferritization. The aim of that process is producing magnetic materials – (BaFe12O19), which grains are milled and oriented during forming in magnetic field [3,8]. Preparation process of barium ferrite includes a stage of mixing barium carbonates and iron oxides and also annealing  of the mixture in temperature of 1350°C. At the temperature of 600°C, it begins process of dissociation BaCO3, what in presence of Fe2O3 leads to rise the monoferrite BaFe2O4. Afterwards the monoferrite reacts with Fe2O3 and creates at last a compound  .		I troductionShort paper118Journal of Achievements in Materials and Manufacturing EngineeringR. Nowosielski, R. Babilas, G. Dercz, L. PająkVolume 17 Issue 1-2 July-August 2006of BaFe12O19. Prepared in this way ferrite is grinded in ball mills to reach size of grain about 1 µm,  pressed to form and sintered in temperature of 1200°C [3,4,9]. Barium ferrites are used to produce elastic magnets with polymer matrix. That type of materials is produced by mixing polymer material with powders of ferrite and then rolling to reach a form of a ribbon or a foil. Magnetic properties of that magnets depend on a content of ferrite powders in polymer matrix. They also have low weight, cost, good corrosion resistance and they are relatively cheap [4,5,10]. 2. Material and research methodology The aim of the present work is the microstructure characterization of commercial powder BaFe12O19 (as-prepared) and composite with BaFe12O19 powders and polymer matrix, using XRD (X-Ray Diffraction) and SEM (Scanning Electron Microscopy) methods. In this work is used a Toraya method for a structure determination of commercial materials – barium iron oxide. Basing on above methods is determination of: lattice parameters, crystallite size (D) and the lattice distortion (<?a/a>).Fig.1 External morphology of the tested composite material with powders of barium ferrite in a cuboid form (commercial material) The investigations were realized on samples of commercial composite with polymer matrix (polyvinyl chloride), which contains powders of barium ferrite. The tested material has a cuboid form about thickness 4 mm and width 7 mm (Fig. 1). Phase analysis was carried out by using the X-Pert Philips diffractometer equipped with curved graphite monochromator on diffracted beam and a tube provided with copper anode. It was supplied by current intensity of 30 mA and voltage of 40 kV. The length of radiation (?CuK?) was 1,54178 Å. The data of diffraction lines was recorded by “step-scanning” method with the range of 10° to 140° 2? and 0,05° step. The profile parameters of individual diffraction lines were determined using Toraya PRO-FIT procedure, which applies Pearson VII function for the description of line profiles [11]. The Toraya procedure is a usefull tool for microstructure characterization, so it was used for multicomponent powder analysis [12-14]. For materials with metallic phases it may be assumed that the X-ray diffraction lines are broadened mainly due to  (a) instrumental effect, (b) small crystallite size, and (c) lattice distortion. The NIST SRM660a (LaB6 powder) standard was used for instrumental broadening determination. The crystallite sizes and lattice distortions of BaFe12O19 phase were estimated using Williamson-Hall method [15]. The values lattice parameters calculated by the classical method applying the extrapolation of the Nelson-Riley function. The accuracy of lattice parameter determination found using alumina plate SRM 1976 standard is ? 0.02%. The content of the barium ferrite powders in tested composite material is 90,6 wt.% and 65,2 vol.%. The values of mass and volumetric contents are presented in Table 1. Table 1. Mass, volumetric contents of powders bounded with polyvinyl chloride in tested composite No. Characteristic Phase Unit Value BaFe12O19+ Fe2O3wt.% 90,6 1. Mass contents  PVC wt.% 9,4 BaFe12O19+ Fe2O3vol.% 65,2 2. Volumetric contents  PVC vol.% 34,8 The morphology of  the barium ferrite powders and a fracture surface of the composite material was carried out using the OPTON DS540 scanning electron microscope provided at the magnification of 100x – 5000x with the ISIS software for the computer recording of images. 3. Results and discussion The X-ray diffraction investigations permitted on identification the BaFe12O19 (ICDD PDF 43-0002) and the Fe2O3(ICDD PDF 85-0987) phases in tested composite (Fig. 2).  The values of lattice parameters, their accuracy and these found in ICDD files for BaFe12O19 phase are also given in Table 2. The crystallite size (D) of BaFe12O19 phase is above 100 nm and the lattice strain (<?a/a>) is 0.033%. Table 2. Phase lattice parameters for powder of barium ferrite Lattice parameters [nm] Phase Toraya ICDD file BaFe12O19a0 = 0.5889(1) c0 = 2.321(4) a0 = 0.58920(1) c0 = 2.3183(1) 2.		Material	and	research	methodology.		results	and	di cussion119MaterialsMicrostructure of composite material with powders of barium ferriteComparison of received lattice parameters of examined phase (BaFe12O19) and lattice parameters from the ICDD card files for model materials allows to formulate following statement. The elementary cell is elongated in a direction of Z axis and shortened in a direction of X and Y axis. Fig.2 XRD pattern of the tested material: a) powder sample, b) composite sample with polymer matrix That results might be happened by modification of atoms position in investigated elementary cell. That fact will be analyse by using the Rietveld method and present in the next papers.  Fig.3 Comparison of XRD patterns for powders of barium ferrite and a composite material with powders of BaFe12O19Comparison of fragment of XRD patterns for powders of barium ferrite and the composite material is presented in Figure 3. Difference in the intensity of (008) (2?  = 30.830) diffraction line for composite and powders induced axial texture on direction [001] in composite material.Technological process of forming the tested composite material by mixing polymer material with powders of barium ferrite and next by rolling to form of a ribbon caused a formation of the axial texture. The intensity change of the other diffraction lines is not observed. Fig.4 Morphology of a barium ferrite (BaFe12O19) powders used as a component in the investigated composite material Short paper120 READING DIRECT: www.journalamme.orgJournal of Achievements in Materials and Manufacturing Engineering Volume 17 Issue 1-2 July-August 2006Fig.5 Morphology of a fracture surface of the composite material Figure 4 shows the morphology of BaFe12O19 powder observed by the scanning electron microscope. Moreover, the morphology of a fracture of the tested composite is presented in the Figure 5. During metallographic observation of morphology of powders and fracture’s surfaces of the composite’s samples it was observed that the distribution of powders of barium ferrite in matrix is irregular. Powder particles have irregular shape and size.4. Conclusion The investigations of the barium ferrite powders and tested composite material allowed to formulate the following statements: ? analysis of the XRD pattern revealed the presence of two phases: BaFe12O19 and Fe2O3;? the lattice parameters are a0=0.5889(1) nm, c0 =2.321(4) nm; ? the crystallite size of BaFe12O19 phase is above 100 nm and the lattice strain (<?a/a>) is 0.033%; ? the SEM images showed that distribution of powders of barium ferrite in polymer matrix is irregular and powder particles have irregular shapes and sizes. References [1] L.A. Dobrza?ski, Fundamentals of materials science and physical metallurgy, WNT, Warsaw, 2002, (in Polish). [2] K.H. Lachowicz, Magnetic materials - progress and challenges, Electrotechnical Review 11 (2002), (in Polish). [3] M. Leonowicz, Modern hard magnetic materials, Published by Warsaw University of Technology, 1996, (in Polish). [4] J. Ding, W.F. Miao, P.G. McCormick, R. Street, High-coercivity ferrite magnets prepared by mechanical alloying, Journal of Alloys and Compounds 281 (1998) 32-36. [5] M.H. Makled, T. Matsui, H. Tsuda, H. Mabuchi, M.K. El-Mansy, Magnetic and dynamic mechanical properties  of barium ferrite-natural rubber composites, Journal  of Materials Processing Technology 160 (2005) 229-233. [6] J. Qiu, M. Gu, Magnetic nanocomposite thin films of BaFe12O19, Applied Surface Science 252 (2005) 888-892. [7] P.E. Garcia-Casillas, A.M. Beesley, D. Bueno, C.A. Martinez, Remanence properties of barium hexaferrite, Journal of Alloys and Compounds 369 (2004) 185-189. [8] O. Carp, R. Barjega, E. Segal, M. Brezeanu, Nonconventional methods for obtaining hexaferrites, Thermochimica Acta 318 (1998) 57-62. [9] A. Mali, A. Ataie, Structural characterization of nanocrystalline BaFe12O19 powders synthesized by sol-gel combustion route, Scripta Materialia 53 (2005) 1065-1075. [10] L.S. Pinchuk, L.V. Markova, Yu.V. Gromyko, Polymeric magnetic fibrous filters, Journal of Materials Processing Technology 55 (1995) 345-350. [11] H. Toraya, Array type universal profile function for powder pattern fitting, Journal of Applied Crystallography 19 (1986) 485-491. [12] G. Dercz, B. Formanek, K. Prusik, L. Paj?k, Microstructure of Ni(Cr)-TiC-Cr3C2-Cr7C3 composite powder, Journal of Materials Processing Technology 162-163 (2005) 15-19. [13] G. Dercz, L. Paj?k, B. Formanek, Dispersion analysis of NiAl-TiC-Al2O3 composite powder ground in high-energy mill, Journal of Materials Processing Technology (in press). [14] L. Paj?k, B. Formanek, G. Dercz, Dispersion analysis of NiAl-TiC-Al2O3 composite powder, Proceedings of 12thScientific International Conference „Achievments in Mechanical and Materials Engineering” AMME’2003, Gliwice-Zakopane, 2003, 723-726. [15] G.K. Williamson, X-ray line broadening from filed aluminium and wolfram, Acta Metallurgica 1 (1953) 22-31. .		conclusionsr ferences

Microstructure of composite material with powders of barium ferrite

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Microstructure of composite material with powders of barium ferrite

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