Journal of Technomaterial Physics Vol.05, No.

01 (2023) 008-014

Journal of Technomaterial Physics

Journal homepage: https://talenta.usu.ac.id/jotp

Study and Characterization of Fe3O4-PEG Nanoparticles Using The

Co-Precipitation Method For The Production of Permanent Magnets
Martha Rianna * and Fitri Handayani
Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara, Jl.
Bioteknologi No. 1, Medan 20155, North Sumatra, Indonesia
*
Corresponding Author: [email protected]

ARTICLE INFO ABSTRACT

Article history: Natural iron sand is one of the natural resources in Indonesia, especially in the
Received 04 February 2023
Cianjur area, West Java which has been used optimally. This study aims to analyze
Revised 17 February 2023
Accepted 24 February 2023 Fe's content, properties, and grain size found in Cianjur, West Java. The natural
Available online 28 February 2023 iron sand samples were prepared using the calcination method, which was dried at
50°C until the samples became powder. Beach sand samples are extracted using a
E-ISSN: 2656-0755
P-ISSN: 2656-0747 permanent magnet to separate magnetic and non-magnetic materials.
Characterization of iron sand using XRD, SEM, VSM, and FTIR. The XRD results
show that the natural iron sand sample has a single magnetite phase (Fe 3O4). A
How to cite:
spinel cubic crystal structure is formed with lattice parameters of 8,513 Ǻ using
M. Rianna and F. Handayani, Co-Precipitation. SEM results show that the sample is inhomogeneous or
"Study and Characterization of homogeneous, as indicated by the gap and agglomeration of particles in each
Fe3O4-PEG Nanoparticles Using sample. VSM results show that the parameter magnetic properties saturation (Ms)
The Co-Precipation Method For
on average is 23.9763735 emu/g, magnetic remanence (Mr) is on average
The Production of Permanent
Magnets," Journal of
5.14865198 emu/g, and coercivity is on average 125.139457033 emu/g. Where in
Technomaterial Physics, vol. 5, sample 1, saturation is 29.7729509 emu/g, remanance is 4.0486018 emu/g,
no. 01, Feb. 2023, coercivity is 92.1368641 emu/g, sample 2 is saturation 21.5994425 emu/g,
doi:10.32734/jotp.v5i1.9889. remanance 8.18772602 emu/g, coercivity 179.567079 emu/g and sample 3 has a
saturation value of 20.55672771 emu/g, remanance 3.20962812 emu/g. Then, the
FTIR results showed a shift in the vibration peak, which experienced a change in
the vibrational energy of Fe-O and then showed the -OH group at an absorption of
3400/cm. The results of this study have the potential to process other magnetic
materials.
Keyword: Fe3O4, particle clusters, particle morphology, magnetic properties, and
particle structure.

ABSTRAK
Pasir besi alam merupakan salah satu sumber daya alam di Indonesia khususnya
pada daerah Cianjur, Jawa Barat yang telah dimanfaatkan secara optimal.
Penelitian ini bertujuan untuk menganalisis kandungan, sifat dan ukuran butir Fe
yang terdapat di Cianjur, Jawa Barat. Pembuatan sampel pasir besi alam ini
menggunakan metode kalsinasi yang dikeringkan pada suhu 50°C hingga sampel
menjadi serbuk. Sampel pasir pantai diekstraksi menggunakan magnet permanen
This work is licensed under a Creative untuk memisahkan material magnetik dan non magnetik. Karakterisasi pasir besi
Commons Attribution-ShareAlike 4.0 menggunakan XRD, SEM, VSM, dan FTIR. Hasil XRD menunjukkan bahwa
International.
sampel pasir besi alam memiliki fasa tunggal yaitu fasa magnetite (Fe3O4), dan
http://doi.org/10.32734/jotp.v5i1.9889 terbentuk struktur kristal kubik spinel dengan parameter kisinya 8.513 Ǻ
menggunakan Co-Presipitasi. Hasil SEM menunjukkan bahwa sampel tidak
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 9

homogen ataupun homogen yang ditunjukkan oleh adanya suatu celah dan
aglomerasi partikel pada setiap sampel yang ada. Hasil VSM menunjukkan
bahwa parameter sifat magnetik saturasi (Ms) rata-rata sebesar 23,9763735 emu/g,
magnetik remanansi (Mr) rata- rata sebesar 5,14865198 emu/g dan koersivitas
rata-rata sebesar 125,139457033 emu/g. Dimana pada sampel 1 bernilai, saturasi
29,7729509 emu/g, remanansi 4,0486018 emu/g, koersivitasi 92,1368641 emu/g,
sampel 2 bernilai, saturasi 21,5994425 emu/g, remanansi 8,18772602 emu/g,
koersivitas 179,567079 emu/g dan sampel 3 bernilai saturasi 20,55672771 emu/g,
remanansi 3,20962812 emu/g. Kemudian, hasil FTIR menunjukkan bahwa terjadi
pergeseran puncak vibrasi yang mengalami perubahan vibrasi energi Fe-O lalu
menunjukkan gugus –OH pada serapan 3400/cm. Hasil studi ini berpotensi dalam
pengolahan material magnetik lainnya.
Kata Kunci: Fe3O4, Metode Kopresipitasi, Morfologi, Kristal Struktur, Magnet
Karakteristik

1. Introduction
Fe3O4 nanoparticles have a great advantage in salinity technology, so this new material development is
urgently needed concerning the exploration of raw materials, synthesis methods used, required calcification
methods, and signal amplification [1] – [4]. In terms of basic ingredients, of course, the materials used are
synthetic and alternative ones that are environmentally friendly and low in toxins. While in the main
problems regarding the method, it is probable that the method used in the restoration, the method synthesis,
which results in a monodisperse scalable nanoparticle product in the method used and also allows a single
domain from the behavior of the particles in the method used, also requires a method that is environmentally
friendly and does not use the balance of alcohols in the synthesis process.
Fe3O4 is a black powder material with strong magnetic properties. In addition, magnetite also exhibits
super-parallel magnetic behavior for grain sizes below 10 nm. Polyethylene glycol 6000 is polyethylene
glycol H(O-CH2-CH2)nOH, and the value of n is between 158 and 204 [5]. It has the following
characteristics: smooth white powder and ivory-yellow white pieces, practically unbounded in origin.
Solubility is easily soluble in flow, in ethanol (95%) chloroform, and in ether. The average molecular weight
is not less than 7000 and not more than 9000. Its efficacy is as an additive [6]
This research was carried out to disperse Fe3O4 nanoparticles with the variation of the composition of
PEG-6000 using the co-precipitation method. The test used XRD, SEM, VSM, and FTIR.

2. Method
2.1 Research Procedures
In this research, the process of synthesizing natural iron palsy with polyethylene glycol (PEG) was carried
out using the Co-Precipitation method. The research includes raw material preparation, precipitate drying,
calcination, and calcification processes.
2.2 Preparation of Nanoparticle of Fe3O4/PEG
In this research, the synthesis process of Fe3O4/PEG nanoparticles was carried out using the co-
precipitation method. According to the ratio, the material used to manufacture Fe3O4 nanoparticle powder is
a natural iron pallant in PEG. First, mix natural iron and PEG into 50 ml of DI water, then stir using a
magnetic stirrer for 1 hour at a speed of 300 rpm at a temperature of 50°C to produce a homogeneous
solution. The homogeneous solution was then forged into a solution of NH4OH in DI water with a
concentration of 6.5 M. Then the mixed solution was stirred for 1 hour at a speed of 500 rpm and a
temperature of 50°C. Then the result of the mixture will produce a precipitate powder. Next, the precipitate
was separated from the impurities using a permanent magnet and washed with DI water; the wet powder
precipitate was washed with 10 ml of ethanol and heated on a magnetic stirrer at 50°C; after the colloid was
formed, it was dried in an oven for 1 hour at 50°C. After the effluent dried, the powder was ground using a
mortar to produce Fe3O4/PEG nanoparticle powder, then characterized using XRD, SEM, VSM, and FTIR
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 10

tests until complete. There are three different samples made based on the composition of the Fe3O4:PEG,
namely, sample 1 (Fe3O4: PEG = 2: 8), sample 2 (Fe3O4: PEG = 8: 2), and sample 3 (Fe3O4: PEG = 10: 0).
2.3 Characterisation of Fe3O4/ PEG Nanoparticle
FTIR tested the structure of chemical compounds or chemical groups of Fe3O4/PEG nanoparticles. To
evaluate the effect of composition on structure in identifying the crystalline phase of Fe3O4/PEG
nanoparticles using X-Ray Diffraction (XRD). The effect of magnetic properties on the molar ratio of
nanoparticles Fe3O4/PEG was tested using a vibrating sample magnetometer (VSM). The morphological
properties of the material were measured using SEM.

3. Results and Discussion

3.1 X-Ray Diffraction (XRD) Analysis
Figure 1 shows the XRD patterns of the samples. Each material shows hkl peaks (110), (200), (311),
(222), (400), (422), and (511). One of the characteristics of phase Fe3O4 is that it has the highest intensity at
34.59 with the hkl peak point (311). The PEG phase did not appear in the XRD test, so no reaction occurred
and functioned as a template. The width or height of intensity in the XRD test results also determines the size
of a crystal. The higher the narrowing of a peak, the greater the crystallite size, and vice versa. If the peak
narrows shorter and lower, then it can be said that the crystallite size is small [7].

Figure 1. XRD pattern of Fe3O4 with PEG-6000 (JCPDS 19-0629)

Table 1. Analysis of XRD Fe3O4 with PEG-6000 of sample 1, 2, 3

Sample FWHM Lattice Grain
2 Intensity
Sample composition  (rad) Parameter Size
(deg) (a.u.) (deg)
(Fe3O4: PEG) (nm) (nm)
1 2:8 31.84 1282.75 0.70822 0.2777 52.64 11.2330

2 8:2 30.39 1282.75 0.70822 0.2650 55.17 11.2323

3 10:0 31.85 1282.75 0.70822 0.2778 52.62 11.2322
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 11

3.2 Scanning Electron Microscope (SEM) Analysis

The SEM results are given in Figures 2, 3, and 4. Based on Figure 2, The agglomeration in sample 1 has
been evenly distributed and not clustered, making it easier to identify the particles; generally, agglomeration
occurs because of the high temperature, where the agglomeration is called the formation of particles. So the
histogram on the particle size of the first sample is good. The particle distribution ranges from 123-138 with
a frequency of 2.0, where the frequency is the number of frequencies in 1 nm.

Figure 2. SEM Picture with the magnification of 5000 times and histogram with Type (Al) Fe3O4-PEG
(sample 1)

Figure 3. SEM Picture with the magnification of 5000 times and histogram with Type (A2) Fe3O4-PEG
(sample 2)

Based on Figure 3, the agglomeration in sample 2 has also been evenly distributed and not clustered,
making it easier to identify the particles, in which case the agglomeration occurs due to the high temperature
where the agglomeration is called particle formation. So that the histogram on the particle size of the first
sample is good because the R-Square in Xc, which is refined, has a value; R-Square = 0.99996; Xc =
172.08928 ± 1.00923 because the acceptable range of R-Square values ranges from 0.85 – 1.0 so that it
fulfills the conditions of the histogram. The particle distribution ranges from 10-80, having a frequency of 2
in terms of frequency, namely the number of frequencies in 1 nm.
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 12

Figure 4. SEM Picture with the magnification of 5000 times and histogram with Type (A3) Fe3O4-PEG
(sample 3)
Based on Figure 4, the agglomeration of sample 3 has also been evenly distributed even though some are
clustered, but it can make it easier to identify the particles where the agglomeration occurs due to the high
temperature; the agglomeration is called particle formation so that the histogram of the particle size of the
first sample is acceptable. The particle distribution ranges from 60-96 with a frequency of 2.

3.3 Vibrating Sample Magnetometer (VSM) Analysis

Figure 5 depicts the hysteresis of nanoparticles Fe3O4-PEG. According to [8], the hysteresis curve has
experienced the particle effect. Particles also tend to affect the magnitude of the curvature of hysteresis in
accordance with [9], even for all particle sizes above 40 nm in the presence of permanent magnetic magnets.

Figure 5. Hysteresis of nanoparticles Fe3O4-PEG

Table 2. Data of testing results from VSM

Sample
Saturation, Ms Remanance, Ms Coercivity, Mr
Sample Composition Bh Max (kOe)
(emu/g) (emu/g) (emu/g)
Fe3O4: PEG
1 2: 8 21.59 8.18 179.56 20.289
2 8: 2 29.77 4.04 92.13 20.261
3 10: 0 20.55 3.20 103.71 10.00

Based on Table 2, in compositions 8:2 and 10:0, there is an increase in the value of coercivity; this occurs
due to agglomeration in the powder. In the saturated value, there is a gradual decrease in remanence and
coercivity that fluctuates up and down due to agglomeration and gaps between particles in the three samples.
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 13

Then there is a decrease in the value of ups and downs in the coercivity affected by the size of a particle. The
smaller the particle size, the easier it is for the material to crack and release its magnetic properties when the
magnetic field is recognized from the outside and vice versa [10].

3.4 Fourier Transform Infra-Red (FTIR) Analysis

FTIR is one tool widely used to determine molecular vibrations that can be used to predict the structure
of chemical compounds or chemical groups. Therefore, focusing on the position of the sample and then
focusing on the detector is a combination of different wavelengths. Wavelength used was 500-4000 (/cm).

Figure 6. FTIR spectrum of Fe3O4 with additions of PEG

Figure 6 depicts the FTIR spectrum of Fe3O4 with additions of PEG. Based on Figure 6, there is a shift in
peak vibration caused by changes in the energy of the Fe-O vibrations located in absorption between 500-
1000 cm, allowing PEG absorption by Fe atoms to occur. It has been synthesized in the presence of
ultrasonic waves. However, the FTIR spectra show that there is another absorption at 3400 cm−1 which is
indicated to be from the –OH group of water, and absorption in the 1600 cm−1 area, which is considered to
arise from an impurity H-C=O.

4. Conclusion
In summary, the structure of the Fe3O4-PEG nanoparticles produced using the Co-Precipitation method has a
single phase, namely the magnetite phase (Fe3O4), and forms a spinel cubic crystal structure with a lattice
parameter of 8.513 Å. The results of the SEM test show that the sample is not homogeneous or
homogeneous, as indicated by the presence of a gap and agglomeration of particles in each sample. Magnetic
properties of nanoparticles Fe3O4-PEG with VSM testing showed that the parameters of the magnetic
properties of saturation (Ms) averaged 23.9763735 emu/g, magnetic remanence (Mr) averaged 5.14865198
emu/g with an average coercivity of 125.139457033 emu/g. The functional group of nanoparticles Fe3O4-
PEG from the FTIR test showed a shift in the vibration peak, which experienced a change in the vibrational
energy of Fe-O at an absorption of 500-1000, then showed a –OH group at an absorption of 3400/cm.

5. Acknowledgments
The authors would like to thank the National Innovation Research Agency-BRIN for laboratory equipment
and testing facilities and BRIN Advanced Materials Research Center researchers for their support and
assistance in conducting research.
 Journal of Technomaterial Physics Vol.05, No.01 (2023) 008-014 14

References
[1] Y. Wei, B. Han, X. Hu, Y. Lin, X. Wang, and X. Deng, "Synthesis of Fe3O4 nanoparticles and their
magnetic properties," Procedia Engineering, vol. 27, pp. 632-637. 2012.
[2] J. Sun, S. Zhou, P. Hou, Y. Yang, J. Weng, X. Li, and M. Li, "Synthesis and characterization of
biocompatible Fe3O4 nanoparticles," Journal of biomedical materials research Part A, vol. 80, no. 2,
pp. 333-341. 2007.
[3] H. El Ghandoor, H. M. Zidan, M. M. Khalil, and M. I. M. Ismail, "Synthesis and some physical
properties of magnetite (Fe3O4) nanoparticles," Int. J. Electrochem. Sci, vol. 7, no. 6, pp. 5734-5745.
2012.
[4] M. R. Ghazanfari, M. Kashefi, S. F. Shams, and M. R. Jaafari, "Perspective of Fe3O4 nanoparticles role
in biomedical applications," Biochemistry research international. vol. 2016, no. 7840161. 2016.
[5] C. Kurniawan, A. S. Eko, Y. S. Ayu, P. T. A. Sihite, M. Ginting, P. Simamora, and P. Sebayang,
"Synthesis and Characterization of Magnetic Elastomer Based PEG-Coated Fe3O4 from Natural Iron
Sand", IOP Conference Series: Materials Science and Engineering, vol. 202, no.012051. 2017.
[6] E. A. Setiadi, P. Sebayang, M. Ginting, A. Y. Sari, C. Kurniawan, C. S. Saragih, and P. Simamora, "The
synthesization of Fe3O4 magnetic nanoparticles based on natural iron sand by co-precipitation method
for the used of the adsorption of Cu and Pb ions," Journal of Physics: Conference Series, vol. 776, no.
1, pp. 012020. 2016.
[7] P. Simamora, and P. T. A. Sihite, "Sifat Magnetic Elastomer Nanokomposit Fe3O4 Dengan Binder
Silicone Rubber," EINSTEIN, vol. 4, no. 2. 2016.
[8] L. Yang, Q. Fu, and H. Fu, "Preparation of Novel Hydrophobic Magnetic Fe3O4/Waterborne
Polyurethane Nanocomposites," Journal of Applied Polymer Science, vol.137, no. 48546. 2020.
[9] A. L. Ortega, E. Lottini, C. J. Fernandez, and C. Sangregorio, "Exploring the Magnetic Properties of
Coballt-Ferrite Nanoparticles for the Development of a Rare Earth-Free Permanent Magnet," Chem
Mater, vol. 27, no. 11, pp. 4048-4056. 2015.
[10] C. Kurniawan, A. S. Eko, Y. S. Ayu, P. T. A. Sihite, M. Ginting, P. Simamora, and P. Sebayang,
"Synthesis and characterization of magnetic elastomer based PEG-coated Fe3O4 from natural iron sand,"
IOP Conference Series: Materials Science and Engineering, vol. 202, no. 1, pp. 012051. 2017.