Facile synthesis of α-Fe2O3/TiO2 multiphase

nanohybrid particles from local iron sand as

antifungal agent
Cite as: AIP Conference Proceedings 2234, 040026 (2020); https://doi.org/10.1063/5.0008133
Published Online: 18 May 2020

Ahmad Taufiq, Deny Arista, Aulia Rachmawati, Nurlailul Ramadhani, Rosy Eko Saputro, Sunaryono, and
Nurul Hidayat

ARTICLES YOU MAY BE INTERESTED IN

Structure, absorbance, and antibacterial activity modification by including AgNPs on

Fe3O4@polyethylene glycol
AIP Conference Proceedings 2234, 040021 (2020); https://doi.org/10.1063/5.0008126

The addition effect of poly-diallyl dimethyl ammonium chloride on Fe3O4@ZnO core-shell and
its potential as photodegradation methylene orange dyes
AIP Conference Proceedings 2234, 040010 (2020); https://doi.org/10.1063/5.0008124

The effect of CuO thickness to perovskite photodetector performance synthesized at ambient

temperature
AIP Conference Proceedings 2234, 040018 (2020); https://doi.org/10.1063/5.0008694

AIP Conference Proceedings 2234, 040026 (2020); https://doi.org/10.1063/5.0008133 2234, 040026

© 2020 Author(s).
 Facile Synthesis of α-Fe2O3/TiO2 Multiphase Nanohybrid
Particles from Local Iron Sand as Antifungal Agent
Ahmad Taufiqa), Deny Arista, Aulia Rachmawati, Nurlailul Ramadhani, Rosy Eko
Saputro, Sunaryono, and Nurul Hidayat

Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Negeri Malang, Jl. Semarang
No. 5, Malang 65145, Indonesia
a)
Corresponding author: ahmad.taufiq.fmipa@um.ac.id

Abstract. This study was conducted to identify the characteristics of α-Fe2O3/TiO2 nanohybrid particles as antifungal
agents. The nanohybrid synthesis was carried out by using the local iron sand-based coprecipitation method. Some
characterization was carried out to determine the structure, morphology, and functional groups of materials as a preliminary
study. The structure review shows that four phases were formed in the material, namely, the hematite, anatase, rutile, and
brookite phases with particle sizes of 15.20 to 36.12 nm. The morphology of α-Fe2O3/TiO2 nanohybrid particles shows
agglomeration with an average particle size distribution of about 26 nm. The α-Fe2O3/TiO2 nanohybrid particle of
functional group succeeded in showing the presence of two of its precursors, namely, α-Fe2O3 and TiO2. Antifungal
application reviews were carried out by using agar diffusion methods on C. albicans mushrooms. Lastly, Inhibition zone
diameters obtained for each sample were 8.5 and 16.4 nm.

INTRODUCTION

Nanohybrid materials nowadays play a key role in the innovation of advanced materials. Research related to
nanohybrid materials basically combines two or more materials with a nanometer scale [1]. Through this performance,
new materials with physical or chemical properties are better than the constituent materials. Thus, the nanohybrid
technique provides better prospects in developing superior advanced materials. One material that is currently being
developed as a precursor of nanohybrid material is α-Fe2O3 (hematite). In the last five years, there have been previous
publications that succeeded in synthesizing nanohybrids based on α-Fe2O3 nanoparticles with other materials such as
ZnO [2], graphene oxide [3], silver [4], polyaniline [5] and TiO2 [6].
In this study, α-Fe2O3 nanoparticles were hybridized with TiO2 nanoparticles. This is because TiO2 nanoparticles
have excellent chemical stability and are non-toxic [7]. These two advantages can support potential antibacterial
applications [8]. However, the synthesis method carried out in the fabrication process is relatively complicated and
requires relatively expensive supporting materials. Therefore, a breakthrough is needed related to the synthesis method
which is relatively easy, fast, and economical to solve this problem.
Based on the description above, in this study, the coprecipitation method was used in preparing the precursors as well
as in the hybridization process. This method was chosen because of its concise, fast, and minimum use of solvents [9].
Therefore, this process is also known as an economical method. Furthermore, the nanohybrid material obtained was
characterized by the elemental and structural contents as a preliminary study. Finally, as a consideration of the potential
application of antifungal nanohybrid materials, an antifungal activity test was carried out using agar diffusion methods.

Conference on Theoretical Physics and Nonlinear Phenomena (CTPNP) 2019

AIP Conf. Proc. 2234, 040026-1–040026-6; https://doi.org/10.1063/5.0008133
Published by AIP Publishing. 978-0-7354-1993-3/$30.00

040026-1
 EXPERIMENTAL METHOD

The precursor synthesis used in this study was reported in [10] and [11]. At the outset, α-Fe2O3 nanoparticles were
mixed with distilled water and, on the other hand, TiO2 nanoparticles were mixed with ethanol in both of them while
stirring using a magnetic stirrer. After 15 minutes of stirring, a solution containing TiO2 particles was titrated into a
solution containing α-Fe2O3 nanoparticles with continuous stirring. In this research, the variation of the precursor mass
composition between α-Fe2O3 and TiO2 and the sample code were as follows: 1: 1 (FT1), 1: 1,2 (FT2). After the
titration process was over, the stirring was held for 30 minutes so that the α-Fe2O3/TiO2 nanohybrid particles could
settle to the bottom of the container. The nanohybrid particles were then washed using distilled water until it reached
pH = 7. Furthermore, the nanohybrid particles were collected using filter paper and roasted at 100 °C in an oven. To
obtain α-Fe2O3/TiO2 nanohybrid particles, at the end of the stage, the dried material in the oven was put into the furnace
and heated at 600 °C. This heating process aimed to convert Fe2O3 nanoparticles into α-Fe2O3 nanoparticles as well
as grow TiO2 nanoparticles crystalline. All α-Fe2O3/TiO2 nanohybrid particles were characterized by using XRF
instruments to determine the percentage of compound content in them. Crystal structure and α-Fe 2O3/TiO2 nanohybrid
particle phases were characterized by using XRD instruments. Besides, the surface morphology of α-Fe 2O3/TiO2
nanohybrid particles was identified through SEM instruments. Finally, the antifungal potential of α-Fe 2O3/TiO2
nanohybrid particles was carried out through antifungal activity test based on agar diffusion method.

RESULTS AND DISCUSSION

The content of compounds in nanohybrid particles is shown in Table 1. In general, the content identified in the
material is dominated by its two constituent compounds, namely, Fe2O3 and TiO2. Furthermore, in FT1 data, the
percentage value of TiO2 compounds identified was less than that of Fe2O3 even though the amount of mass given was
the same. The explanation related to this is the difference in density of the two materials, namely, 5.250 g/cm3 and
4.230 g/cm3. However, on FT2 data, the percentage value of TiO2 increases with the addition of mass of TiO2.
Although the amount of mass given is relatively small in macroscopic reviews, this constantly makes a significant
contribution.
TABLE 1. Percentage of compounds in α- Fe2O3 /TiO2 nanohybrid particles
Samples Fe2O3 Conc. (%) TiO2 Conc. (%) Others Conc. (%)
FT1 64.75 28.20 7.05
FT2 40.20 47.80 12.0

Furthermore, in addition to the two compounds above, several impurities in the material were also found. Two
assumptions are held with regard to this fact. First, the XRF instrument is relatively inaccurate in analyzing other
compounds in the material. Thus, unwanted compounds appear but with a relatively low percentage. In particular, this
claim is also supported by XRD data which shows no impurity in the material. Second, the extraction of natural sand
is not yet optimum so that the impurity attached to it cannot be completely destroyed.
The X-ray diffraction pattern of α-Fe2O3/TiO2 nanoparticles is shown in Fig. 1. Based on this Figure, we can
observe that a single phase of α-Fe2O3 and TiO2 multiphase formed consists of anatase, rutile, and brookite phases.
Furthermore, as the TiO2 mass increases, the identified derivative phase also increases [12]. This is reviewed by the
emergence of a new brookite phase in the presence of small peaks in the 30.40° region with the Miller index (011).
Furthermore, the addition of TiO2 mass affects the strengthening of the peak which represents the rutile phase in the
region of 27.58°, 41.18°, 54.18° and 69.38° [13]. Meanwhile, the anatase phase tends not to experience significant
changes. The particle sizes obtained for α- Fe2O3, anatase, rutile, and brookite phases were 36.12, 22.59, 15.20, and
24.48 nm, respectively. In an earlier report, Zhou and his colleagues successfully synthesized α-Fe 2O3 nanoparticles
through the hydrothermal method and obtained a particle size of 50 nm [14]. In another report, Duong and his
colleagues succeeded in synthesizing TiO2, by obtaining 5.8 to 63.1 nm [15].

040026-2
 FIGURE 1. X-ray diffraction pattern of α- Fe2O3/TiO2

Visualization of α-Fe2O3 and TiO2 multiphase crystals is shown in Fig. 2a-d. In general, α-Fe2O3 nanoparticles have
an R-3c plane group and a rhombohedral crystal structure [16]. This is what distinguishes it from other iron oxide
derivatives. Based on the process of formation, α-Fe2O3 arises due to heating which makes ellipsoid-shaped Fe atoms
become oblate spheroid. Furthermore, this new form has the characteristic of a shorter c-axis and the O ellipsoid atom
is in the triaxial position along the a-axis. Consequently, the longest axis of the system leads to the octahedral site and
the shortest axis goes to the edge of the octahedral site at an angle of 30° from the c-axis [17]. Some references stated
that to convert the Fe2O3 phase to the α-Fe2O3 phase, a heating treatment between 450 °C to 750 °C is needed [18,19].

FIGURE 2. Visualization of crystals a) α-Fe2O3 b) anatase c) rutile and d) brookite

040026-3
 A)

B)

FIGURE 3. Morphology and histogram of particle size distribution a) FT1 and b) FT2

The surface morphology of α-Fe2O3/TiO2 nanoparticles was characterized by SEM instruments and shown in Fig. 3.
Through the morphology of α-Fe2O3/TiO2 nanoparticles, it can be seen that the α-Fe2O3/TiO2 nanoparticles show
agglomeration with an average particle distribution of 26 nm. This is a natural tendency for young nanoparticles to
clump due to van der Walls forces [20]. Furthermore, this force has a great effect because the ratio between surface
area to volume is incredibly large [21]. Consequently, nanoparticles form a particle cluster to obtain a more stable
state. It was identified that the size of the formed particle cluster size of above 79 nm.

FIGURE 4. Transmittance spectrum of α-Fe2O3/TiO2 nanoparticles

040026-4
 The α-Fe2O3/TiO2 nanoparticles functional group is represented through the transmittance spectrum in Fig. 4.
There are two main functional groups that indicate the formation of α-Fe2O3/TiO2 nanoparticles, namely, Fe-O in the
429 cm-1 and 495 cm-1 regions [22] and Ti-O which is located widened from 517 to 874 cm-1 [23]. Furthermore, there
are two hydroxyl functional groups which are the result of the reaction in the synthesis of α-Fe 2O3/TiO2 nanoparticles.
The first hydroxyl functional group is located in the region of 1631 cm-1 and then at 3004 to 3669 cm-1 [24]. This
functional group is located in the area of 3693 cm-1. Overall, the functional group data obtained supports XRD data
that α-Fe2O3/TiO2 nanoparticles have been successfully formed.
Antifungal activity of α-Fe2O3/TiO2 nanoparticles was assessed through agar diffusion method by reviewing the
diameter of the fungal inhibition zone. Antifungal activity is carried out on the fungus Candida albicans. The diameter
of the inhibition zone of the fungus after being treated with the sample is shown in Fig. 5. The acquisition of the
inhibition zone diameter of the two samples appears to be increasing. Quantitatively, the average inhibition zone
diameter of FT1 and FT2 is 8.5 mm and 16.4 mm. Theoretically, the increase in inhibition zone diameter is caused by
the presence of reactive oxygen species contained in each precursor [25]. Furthermore, increasing the mass of TiO 2
added will increase the biocompability characteristics of α-Fe2O3/TiO2 nanoparticles while increasing the supply of
reactive oxygen species of material [26]. With nanometer-scale reactive oxygen species, it facilitates penetration in
fungal cell membranes and can destroy pathogenic DNA in the cell nucleus [27]. In an earlier report Chougale and
colleagues synthesized TiO2 nanocomposites based on Brahmi plant extract with polyvinyl alcohol (PVA) and
obtained fungal inhibition zones between 11.2 nm to 15.9 mm [28].

FIGURE 5. Histogram of α-Fe2O3/TiO2 inhibition zone diameter

SUMMARY

In this study, α-Fe2O3/TiO2 nanohybrid particles were made by using coprecipitation method. A series of
characterizations related to structure, morphology, and functional groups have been carried out. The α-Fe2O3/TiO2
nanohybrid particles encompass four phases, namely, hematite, anatase, rutile, and brookite with particle sizes in the
range of 15.20 to 36.12 nm. Based on the morphological analysis, α-Fe2O3/TiO2 nanohybrid particles experienced
agglomeration with a particle size distribution of about 26 nm. The α-Fe2O3/TiO2 nanoparticles of functional group
shows the success of the two precursors in the nanohybrid system for binding. An overview of antifungal activity
shows that increasing the mass of TiO2 influences increases of the antifungal activity of the material. Lastly, Inhibition
zone diameters for each material were obtained 8.5 and 16.4 mm.

ACKNOWLEDGMENTS

This work was financially supported by a research grant from KEMENRISTEKDIKTI RI.

040026-5
 REFERENCES

1. Sanad M M S and Rashad M M, Journal of Electronic Materials 46 4426–34 (2017)

2. Chaudhury C R, Roychowdhury A, Das A and Das D, Journal of Physics and Chemistry of Solids 92 38–44
(2016)
3. Nathan D M G T and Boby S J M, Journal of Alloys and Compounds 700 67–74 (2017)
4. Trang V T, Phan V N, Van Quy N, Huy T Q and Le A-T, Journal of Electronic Materials 46 3323–32 (2017)
5. Bora M A, Adhav P B, Diwate B B, Pawar D S, Dallavalle S and Chabukswar V V, Polymer-Plastics Technology
and Materials 1–11 (2019)
6. Wang Y, Shi H, Cui K, Zhang L, Ge S, Yan M and Yu J, Biosensors and Bioelectronics 117 515–21 (2018)
7. Sun Q, Hu X, Zheng S, Sun Z, Liu S and Li H, Powder Technology 274 88–97 (2015)
8. Abdulhady Y A, El-Shazly M M and El-Kased R F, Journal of Environmental Science and Health, Part A 53
205–12 (2018)
9. Gouda A A, Talanta 146 435–41 (2016)
10. Arista D, Rachmawati A, Ramadhani N, Saputro R E and Taufiq A, IOP Conference Series: Materials Science
and Engineering vol 515 (IOP Publishing) p 012085 (2019)
11. Taufiq A, Arista D, Saputro R E, Hidayat N, Soontaranon S and Handoko E, Materials Science Forum vol 966
(Trans Tech Publ) pp 181–8 (2019)
12. Singh A, Vihinen J, Frankberg E, Hyvärinen L, Honkanen M and Levänen E, Nanoscale research letters 11 447
(2016)
13. Mesquita‐Guimarães J, Leite M A, Souza J C M, Henriques B, Silva F S, Hotza D, Boccaccini A R and Fredel
M C, Journal of Biomedical Materials Research Part A 105 590–600 (2017)
14. Zhou Y, Yu L, Xie X, Tang P and Chen H, Ferroelectrics 530 32–8 (2018)
15. Duong N T, Vuong L D, Son N M, Van Tuyen H and Van Chuong T, Nanomaterials and Energy 6 82–8 (2017)
16. Wu W, Wu Z, Yu T, Jiang C and Kim W-S, Science and technology of advanced materials 16 023501 (2015)
17. Sanson A, Mathon O and Pascarelli S, The Journal of chemical physics 140 224504 (2014)
18. Jafari A, Shayesteh S F, Salouti M and Boustani K, Journal of Magnetism and Magnetic Materials 379 305–12
(2015)
19. Pati S S, Singh L H, Ochoa J M, Guimarãesa E M, Sales M J A, Coaquira J A H, Oliveira A C and Garg V K,
Materials Research Express 2 045003 (2015)
20. Sunaryono, Taufiq A, Putra E G R, Okazawa A, Watanabe I, Kojima N, Rugmai S, Soontaranon S, Zainuri M
and Triwikantoro, Nano 11 1650027 (2016)
21. Brojabasi S, Muthukumaran T, Laskar J M and Philip J, Optics Communications 336 278–85 (2015)
22. Kumaria S, Yadava N, Ghosha D, Srivastavaa C M and Majumdera S, Indian Journal of Chemistry 57 1151–5
(2018)
23. Lu M, Wang F, Liao Q, Chen K, Qin J and Pan S, Journal of Molecular Structure 1081 187–92 (2015)
24. León A, Reuquen P, Garín C, Segura R, Vargas P, Zapata P and Orihuela P, Applied Sciences 7 49 (2017)
25. Saputro R E, Taufiq A, Hidayat N, Hariyanto Y A and Hidayat A, IOP Conference Series: Materials Science
and Engineering vol 515 (IOP Publishing) p 012029 (2019)
26. Villatte G, Massard C, Descamps S, Sibaud Y, Forestier C and Awitor K-O, International journal of
nanomedicine 10 3367 (2015)
27. Mehrabani M G, Karimian R, Rakhshaei R, Pakdel F, Eslami H, Fakhrzadeh V, Rahimi M, Salehi R and Kafil
H S, International journal of biological macromolecules 116 966–76 (2018)
28. Chougale R, Kasai D, Nayak S, Masti S, Nasalapure A and Raghu A V, Green Materials 1–9 (2019)

040026-6