Magnetic behavior of natural magnetite (Fe3O4) extracted from beach sand obtained by

mechanical alloying method

Z. Jalil, A. Rahwanto, Mustanir, Akhyar, and E. Handoko

Citation: AIP Conference Proceedings 1862, 030023 (2017); doi: 10.1063/1.4991127

View online: https://doi.org/10.1063/1.4991127
View Table of Contents: http://aip.scitation.org/toc/apc/1862/1
Published by the American Institute of Physics

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 Magnetic Behavior of Natural Magnetite (Fe3O4) Extracted
from Beach Sand Obtained by Mechanical Alloying Method
Z. Jalil1, a), A. Rahwanto1, Mustanir2, Akhyar3, and E. Handoko4
1
Department of Physics, Syiah Kuala University, Banda Aceh, Indonesia
2
Department of Chemistry, Syiah Kuala University, Banda Aceh, Indonesia
3
Department of Mechanical Engineering, Syiah Kuala University, Banda Aceh, Indonesia
4
Department of Physics, Jakarta State University, Jakarta, Indonesia
a)
Corresponding author: [email protected]

Abstract. Investigation on the iron sand characteristic of Syiah Kuala beach in Banda Aceh coastal region has been
performed. Samples were prepared by mechanical alloying method using a planetary type high energy ball milling. As
shown by XRF results, the results indicate that the iron sand is dominated by magnetite up to 85.80 %. The XRD test
showed that the Fe3O4 (magnetite) appears as the majority phase. Furthermore, the magnetic properties observation found
that the magnetization saturation (Ms) and remanent (Br) are decreasing with the increasing of the coercivity (Hc). These
results inform us that the mechanical alloying method is a very attractive technique to reduce the beach sand particle into
nanometer scale.

Keywords: Iron sand, mechanical alloying, magnetic properties, magnetite

INTRODUCTION
Department of mines and energy of Aceh province put minerals gold, copper, molybdenite, iron ore and iron sand
as the Aceh's flagship minerals commodities [1]. Especially iron sand minerals, including class B (vital minerals)
based on the Government Regulation No. 27 in 1980 about the classifications of minerals. Few studies that have been
conducted showed that the mineral content in the sand dominated by magnetite (Fe3O4) [2-3]. Some researchers do
variety identification and characterization of deep to get related information properties magnetic Fe3O4 [4-5] and the
cutting edge is the production of Fe3O4 nanoparticle-scale natural for the application of ferroelectric materials [6]. A
further application is the use of Fe3O4 as the catalyst of hydrogen storage materials based on magnesium [7]. See the
extent of the use of the mineral magnetite and in order to develop the business sector of non-oil & gas then utilization
of sand iron available in nature is worth considering.
As a side note, while India is one country that has exploit sand iron for export-oriented commercial purposes [8,
9]. Meanwhile in Indonesia generally used as additional material in the cement industry. Particularly in the Aceh
Province its mostly occurring in the area of Aceh Besar, North Aceh, and Sabang [10]. In Aceh Besar District for
example their deposits reach 7.2 million tons and is currently it is used for raw material cement mixture at PT. Semen
Andalas Indonesia (SAI). Unfortunately, studies and research related to iron sand in Aceh has not been done in a
concerted and depth.
Therefore, to answer this scientific challenges, we conducted a series of investigations on a local beach sand. In
this paper, we outlined the research results in the form of qualitative data that includes the identification phase, crystal
size and the magnetic properties of natural iron sand in the coastal area of Syiah Kuala beach, Banda Aceh.

International Symposium on Current Progress in Mathematics and Sciences 2016 (ISCPMS 2016)
AIP Conf. Proc. 1862, 030023-1–030023-4; doi: 10.1063/1.4991127
Published by AIP Publishing. 978-0-7354-1536-2/$30.00

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 MATERIAL AND METHODS
In this study, we used iron sand from the coastal area of Syiah Kuala beach, Gampong Dayah Raya, Banda Aceh.
In the early stages of the separation process, the sample was manually separated by using a magnet rods. Magnets are
brought to all parts of the sand until all sand iron lifted or attached to the magnet. Furthermore, the particle size
reduction is done by using ball mill (Planetary Mill, Fritsch-P6) with ball and powder ratio (BPR) was 10:1, and then
put in a vial and then milled for 20 hours with 450 rpm. Then, the qualitative data related phase composition and size
of crystals was identified using X-rays diffractometer (XRD Shimadzu, D6000) and the mineral composition was
observed by XRF (Bruecker, S2-Stranger). Experimental results of data and then compared to the reference database
issued by International Crystallography Diffraction Data (ICDD) using PCPDFWIN. The crystallite size calculated
by Scherrer formula [11]. The morphology was investigated by a scanning electron microscopy (Philips, XL30). While
the magnetization properties observed using Permagraph (Magnet Physik, 2T). For the purposes of the magnetic test,
the sample was firstly compacted in pellet form using a hydraulic press machine with 5 tons of pressure.

RESULTS AND DISCUSSION

The mineral composition of iron sand generated x-ray fluorescence (XRF) as seen in Table 1 indicated that
magnetite (Fe3O4) is dominated by 85.80% while minor phases are TiO2, SiO2, Al2O3 and some others.
The XRF results consistent with the x-ray diffraction (XRD) measurements as seen in Fig. 1 where the majority
of the present phase of the magnetite (Fe3O4), its minor phases are TiO2 and SiO2.
In general, it can be said with an advanced technique obtained by mechanical alloying method capable of reducing
nano-powder to the smallest crystallite size at the (311) as 11.1 nm. Interesting to note that the diffraction peaks
became broader by increasing milling time. This condition happens because their relative intensity decreases mainly
due to the reduction of the particles size and accumulation of microstrain [12-14].

TABLE 1. Mineral composition of Syiah Kuala beach sand

Minerals Fe3O4 TiO2 SiO2 Al2O3 MnO P2O5 Cr2O3 CaO V2O5 K2O Nd2O3
composition
(%) 85.80 5.65 2.92 1.51 0.68 0.56 0.52 0.48 0.47 0.38 0.38

FIGURE 1. XRD pattern of magnetite (Fe3O4) from iron sand milled in various time

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 (a) (b)
FIGURE 2. SEM Images of iron sand (a) before milling and (b) after 20 hours milling

A further study of the grained structure for the different sample of as milled and consolidated was carried out by
SEM characterization.
Before milling, the magnetite sample has similar grains (Fig. 2a). Furthermore, after 20 hours milling, the surface
of the powder is in irregular shape, as a result of the fracturing during the milling process (Fig. 2b). The grains look
decrease to be smaller. This is consistent with the structural analysis by XRD of the 0 h to 20 milled powder. From
the SEM data inform that at the milled sample has particle size about 100 µm.
The next observation was done by Permagraph which works on the external magnetic field by 2 tesla (T). The test
results obtained a hysteresis loop curves can be known the quantities include magnetic saturation (Ms), remanence
(Br) and coercivity (Hc) as shown in Fig. 3 and Fig. 4. The curve has magnetic saturation of 0.333 T (before milling)
and 0.188 T (after 20 hours milling). While the value of remanence (Br) is 0.022 T (before milling) and 0.075 T (after
20 hours milling) and coercivity (Hc) before milling 1.34 kA/m, but remarkable increase after 20 hours. It shows the
improvement significantly i.e. reaching 33.31 kA/m. Table 2 shows the details of magnetic properties measurement.
As the milling time increases, the saturation magnetization decreases, coercive field increases and remanent decreases
as well. Under the experimental conditions reported in this work, it is noted that with increasing the milling time, the
crystallite size decreases and reaches a nanometric size.

FIGURE 3. Hysteresis loop of iron sand magnetite FIGURE 4. Hysteresis loop of iron sand magnetite after
before milling milling 20 hours

TABLE 2. Magnetic measurement of iron sand after 20 hours milling

Magnetic Properties
Milling time Saturation
Coercivity (kA/m) Remanent (T)
magnetization (T)
0h 0.333 1.34 0.022
20 h 0.188 33.31 0.075

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 As for the phenomenon of declining value of magnetic saturation (Ms) and the remanence (Br) are accompanied
the increase in the value of the coercivity (Hc), after 20 hours milling, Interesting to see that there is a correlation
between the size of the crystals with the changing magnetic properties. Allegedly with more delicate crystallite size,
the result of a Scherrer calculation of nanometer scale, it will lead to the increasing of the empty spaces between the
crystals. The increasing of the coercive fields Hc from 1.34 to 33.31 kA/m could be due to decrease of cluster size and
also increase of density of defects with the increasing of milling time [15].

CONCLUSIONS
The mechanically alloyed iron sand samples were characterized for compositional and structural characterizations
that in turn influence mechanical and magnetic properties. The main emphasis has been given in synthesizing the sand
through mechanical alloying and evaluation of milling time influence on chemical composition and structural since
microstructure plays vital role in influencing the mechanical and functional properties like magnetic and electric
properties. The magnetization hysteresis loops suggest that Fe3O4 from milled iron sand show a possibility for soft
magnet application. Coercive field, Hc, increased from 1.34 to 33.31 kA/m with the increasing of milling time
indicating the decreasing of particle size. The magnetic properties observation found that the magnetization saturation
(Ms) and remanent (Br) was decreased with the increasing of the coercivity (Hc). This results inform us that the
mechanical alloying method is very attractive technique to reduce the beach sand particle into nanometre scale.

ACKNOWLEDGMENTS
Authors wish to thank LPPM Unsyiah for financial support. The authors also thank Eva Novita Sari, S.Si and
Syarifah Fathmiyah, S.Si (Material Physics Lab., Syiah Kuala University) for assistance in the sample preparation and
XRD testing.

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