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The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

Preparation and characterization of Bentonite-OPBA

nanocomposite as filler

E Frida1, N Bukit2, F R A Bukit3* and B F Bukit4

1
Department of physics Universitas Sumatera Utara, 20155, Medan, Indonesia
2
Department of physics, Universitas Negeri Medan, 2022, Medan, Indonesia
3
Department of Electrical Engineering, Universitas Sumatera Utara, 20155, Medan,
Indonesia
4
Universitas Quality Berastagi, 22153, Berastagi, Sumatera Utara, Indonesia

E-mail: ferryrahmatastiantabukit@gmail.com

Abstract. Bentonite-OPBA nanocomposite has been made. The preparation of OPBA and
bentonite was carried out by calcination process at a temperature of 700oC for bentonite and
500 oC for OPBA and a ball mill process for 10 hours and coprecipitation method with a
solution 6 M HCl. Then nano bentonite was synthesized with surfactant Cetyl Trimethyl
Ammonium Bromide (CTAB). The XRD analysis obtained a Bentonite-OPBA particle size of
14.46 nm, with a Tetragonal crystal system and density of 3.01200 g/cm³. XRF analysis
obtained SiO2 content of 55.1 % FTIR analysis obtained absorption band detected at 981.33
cm−1 indicates that the increase in silica strengthening has in the polymerization process.

1. Introduction
In recent years, many researchers have produced environmentally friendly products such as
geopolymers. The production of geopolymers is an alumina-silicate based material rich in silicon (Si)
and Aluminium (Al) activated by alkaline solutions. Previous studies have shown that geopolymers
have excellent mechanical properties, high chemical resistance and the ability to bind hazardous
wastes (Javed et al., 2020). One of the alumina silicate originating from geopolymer comes from oil
palm boiler ash (OPBA). In Indonesia in 2018, the total area of oil palm plantations was recorded at
14,326,350 hectares (Statistics, 2018), so it is likely to generate OPBA waste. OPBA comes from the
burning residue of palm kernel shells and fruit fibres containing the chemical element silica (SiO 2) as
much as 31.45% and lime (CaO) as much as 15.2%. This material is formed in the exhaust gases and
collected using an electrostatic precipitator. Since these particles solidify while suspended in the
exhaust gases, they are generally spherical in shape [1, 2]. Based on the research conducted, it turns
out that OPBA contains a lot of silica (SiO2) which is a pozzolan and filler material for composites [3],
[4].
Bentonite is an abundant natural resource in Indonesia, but its utilization has not been optimal. One
application of bentonite currently being studied by many international and national research
institutions is its use as a nano-sized filler, better known as a nanofiller—modification of bentonite
into organoclay material with surfactants, as organic layer silica (OLS). In the OLS structure, the
distance between the basalts in bentonite (d-spacing) is enlarged, wherein processing with polymer
materials in the melting phase, the d-spacing will increase in intercalate and finally, the layer structure
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The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

contained in bentonite is separated from each other . exfoliation so that bentonite is dispersed into the
polymer system with a size smaller than 100 nm. Thermal and acid treatment processes can carry out
the synthesis of silica nanoparticles from bentonite to reduce alumina and increase silica content [5].
Bentonite modification by combining other materials can improve the performance of bentonite. For
example, combining bentonite/rice husk in the HDPE matrix can improve the mechanical properties of
the composite [6]. In addition, combining bentonite with carbon black, which is used as a natural
rubber filler, can affect tensile strength, elongation at break, modulus of elasticity, and composite
hardness [7, 8]. In addition, the addition of nano SiO2 and bentonite was able to increase the
compressive strength of the mortar [9].
In this study, bentonite nanoparticles were prepared by calcining bentonite and ball mill,
coprecipitation, and CTAB surfactant. At the same time, the manufacture of OPBA nanoparticles is
carried out by calcining OPBA followed by the ball mill and coprecipitation method. The addition of
CTAB surfactant is expected to prevent agglomeration and control pore volume and size [10–12].

2. Methods

Synthesis of Nano Bentonite

Bentonite calcination at a temperature of 700 oC for 5 hours and milling with a ball mill type Planetary
Ball Mill for 10 hours with a rotation of 250 rpm. Furthermore, the synthesis of bentonite by
coprecipitation method using 6 M HCl using a stirrer at 70 oC for 4 hours. Next, mix bentonite with 7
M NaOH using a stirrer at 70 oC for 4 hours. Wash bentonite with distilled water until it produces a
neutral pH. It is drying bentonite at 250 oC for 4 hours. CTAB was dissolved in distilled water and
then heated and stirred at 80 oC for 1 hour. Besides that, mix bentonite with deionized water at 70 oC
for 2 hours. Mixing the CTAB solution and bentonite dispersion at 70 oC for 3 hours and then filtered.
Adding AgNO3 with distilled water. The mixture was then dried in an oven at 100 0C for 10 hours. The
schematic for the manufacture of nano bentonite is shown in Figure 1.

Figure 1. Schematic of nano bentonite preparation.

Synthesis of OPBA nanoparticle

Synthesis of OPBA nanoparticles was carried out by ball mill and coprecipitation methods. OPBA
obtained was calcined at a temperature of 500 oC for 5 hours; the calcined results were milled with a
ball mill type Planetary Ball Mill type Retsch PM200 for 10 hours with a rotation of 250 rpm. The
OPBA ball mill process was mixed with 6 M HCl solution at a temperature of 70 0C for 4 hours. It was
mixing OPBA with 7 M NH4OH for 4 hours at 70 0C. The OPBA was washed with distilled water
until it produced a neutral pH on the OPBA and then precipitated. The precipitate was dried at 200 oC
for 2 hours. The schematic for the preparation of OPBA nanoparticles is shown in Figure 2.

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The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

Figure 2. Schematic of making OPBA nano nanoparticles.

Bentonite/OPBA nanocomposite preparation

Nano bentonite and OPBA were mixed by adding 100 ml of ethanol using a stirrer at a temperature of
70 oC for 2 hours, then washed with distilled water to produce a neutral pH on the nanocomposite
precipitated. The precipitate was dried at 150 oC for 2 hours. The schematic for the manufacture of
bentonite/OPBA nanocomposites is presented in Figure 3.

Figure 3. Schematic of making bentonite-OPBA nano nanocomposite.

3. Result and Discussion

3.1. XRD analysis

X-ray diffraction (XRD) analysis to measure particle size and structure analysis of bentonite and
OPBA used a Goniometer type Shimadzu 6,000 instrument with a Cu/Kα1 X-ray source with a
wavelength, = 1.54056. The analysis was carried out with an angle of 2θ starting from 7 o to 70o. To
identify the diffraction pattern of the synthesized material, the resulting diffractogram is compared
with the JCPDS (Joint Committee on Powder Diffraction Standard) database. The crystal size (D) of
the material is carried out using the equation:

D K
 cos (1)

Where D is the crystal size (Ǻ), is the X-ray wavelength used, namely CuKα radiation (λ =
1.54056), is the Bragg angle, = Scherrer's constant has a general value of 0.9 and is the half-peak width
of Full Width at Half Maximum (FWHM) in radians.

3
The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

Figure 4. X-ray diffraction analysis for bentonite and OPBA.

Bentonite-OPBA XRD diffraction pattern is presented in Figure 4. The peak angles occur at 2 theta
angles of 20.25o, 26.50o, 30.61o 44.43o, which indicate a geopolymer material containing silica,
anorthite/albite, and calcite minerals. Anorthite and Albite are hydrothermal products in nature (in
marshlands etc.) as well as in geopolymers. This zeolitic product exhibits a polymerization process in
which geopolymers are made from aluminosilicates such as fly ash, slag, bottom ash, etc. This proves
the success of combining bentonite with OPBA [13–15]. XRF and FTIR results where the dominant
silica content is obtained [16]. Meanwhile, the data on the physical properties and nanostructures
produced by the match program is shown in Table 1. From equation 1 using an analysis with the origin
graph, the Bentonite-OPBA particle size obtained is 14.46 nm.

Table 1. XRD Analysis of OPBA and Bentonite nanoparticles with ball mill processes.
Date Bentonite-OPBA
Crystal system Trigonal (hexagonal axes)
Space group P 31 2 1 (152)
Unit cell a = 4.6764 Å c = 5.2475 Å
Density 3.01200 g/cm³
2 theta angle 30.61
Maximum dhkl 011
Intensity I/I0 1000
Lattice distance d (Å) 3.2061
2 theta angle 26.50
Maximum dhkl 100
Intensity I/I0 858.2
Lattice distance d (Å) 4.0499
2 theta angle 44.43
Maximum dhkl 200
Intensity I/I0 527.3
Lattice distance d (Å) 2.0249
2 theta angle 20.25
Maximum dhkl 110
Intensity I/I0 375.8
Lattice distance d ( Å) 2.3382

4
The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

3.2. SEM Analysis

To describe the surface morphology of Bentonite-OPBA and the composition of the compounds
contained in it, SEM analysis was carried out using the EVO MA 10 Zeiss instrument. SEM of
Bentonit-OPBA is presented in Figure 5.

Figure 5. Scanning Electron Microscope of Bentonit-OPBA.

SEM analysis showed that structure is less aggregated this is probably caused by modifications with
the use of CTAB surfactants on bentonite [17–19].

3.3. FTIR Analysis

Each functional group of the compound has specific energy to vibrate in several modes. The energy
absorbed by each functional group is detected to vibrate in various modes. The amount of energy
absorbed as a function of frequency can be determined by what compounds are contained in the
material. Several other aspects of the measurement can be used as material to analyze the material
being tested. It can be characterized using FTIR. To see the functional groups of organic bentonite and
OPBA, characterization was carried out using the FT-IR Shimadzu IR Prestige 21. FTIR spectrum of
bentonit-OPBA showed in Figure 6.

60 Transmittance

50
Transmittance (%)

40

30 C=C

C-H

20 1466.66
O-H
2842.66 1637.33
3637.33 800
2933.33 1152 981.33
10
4000 3500 3000 2500 2000 1500 1000 500
-1
Wavenumber (cm )

Figure 6. Fourier transform-infrared analysis for bentonite and OPBA.

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The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

The degree of polymerization can be expressed quantitatively from the Si–O–Si stretching peaks in
the FTIR spectrum. The absorption band detected at 981.33 cm−1 indicates that the increase in silica
strengthening has increased in the polymerization process. The stretching deformation (SiO–
Al/Fe/Mg) of 800 cm−1 is related to the vibrational characteristics of the Si–O quartz. The deformation
of Al–O 981.33 cm−1 is associated with Mg-Al–OH. The signal at 1637.33 cm−1 corresponds to the
deformation of H2O (adsorbed between the aluminum-silicate layers). The band at 3630 cm−1 is
associated with Al-OH stretching [20].

3.4. XRF Analysis

XRF characterization on Bentonit-OPBA samples was carried out using XRF PANalytical Manipal 4.
This tool can be used to test the elemental content of a material ranging from Sodium-Uranium. Table
2 showed the content of Bentonit – OPBA.

Table 2. Elements obtained from XRF analysis.

Compound Bentonit-OPBA
SiO2 55.10
K2O 3.22
CaO 9.19
Fe2O3 12.10
Al2O3 12.00
Ti 1.60
MnO 0.20
Cr2O3 0.06
ZnO 0.03
V2O5 0.03
P2O5 3.20
Br 3.53
Re2O7 0.10
Eu2O3 0.20

The main content of Bentonite-OPBA is SiO2, Fe2O3, Al2O3. This is by the main constituents of
bentonite and OPBA, respectively (Aljlil, 2020; Bukit et al., 2019; Javed et al., 2020; Kueaket &
Tonnayopas, 2021). The SiO2 content obtained is 51.1 %, this is greater than the results of previous
studies because OPBA is calcined to a temperature of 500 oC [21, 22].

4. Conclusion
From the results of the study, it was found that the peak angle occurred at an angle of 2 thetas 20.25 o,
26.50o, 30.61o, 44.43o which indicated a geopolymer material containing silica, anorthite/albite, and
calcite minerals. In addition, the particle size obtained is 14.46 nm. SEM results show a structure like
an irregular ball that spreads evenly. The absorption band detected at 981.33 cm−1 indicates that the
increase in silica strengthening has led to an increase in the polymerization process. This is by the
XRF results obtained, where SiO2 is the dominant element. Therefore, Bentonite-OPBA
Nanocomposite can be used as a filler in thermoplastics and elastomers.

Acknowledgement
Thank you to the Directory of Research and Community Service Deputy for Research Strengthening
and Development of the Ministry of Research and Technology/National Research and Innovation
Agency for Financing Penelitian Dasar Unggulan Perguruan Tinggi (PDUPT). The fiscal Year 2021
No: 12 / E1/KP.PTNBH/ 2021, dated 08 March 2021.

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The 1st International Conference Science Physics and Education 2021 (ICSPE 2021) IOP Publishing
Journal of Physics: Conference Series 2165 (2022) 012023 doi:10.1088/1742-6596/2165/1/012023

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