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Physical analysis of TiO2 and bentonite nanocomposite as adsorbent materials

  • Nurdin Bukit EMAIL logo , Eva Marlina Ginting , Erna Frida EMAIL logo and Bunga Fisikanta Bukit
Published/Copyright: December 16, 2021
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REVIEWS ON ADVANCED MATERIALS SCIENCE
From the journal REVIEWS ON ADVANCED MATERIALS SCIENCE Volume 60 Issue 1

Abstract

The research analyzed the physical properties of TiO2 and bentonite nanocomposite as adsorbent materials. The TiO2 synthesis method was carried out through a sol–gel process. Meanwhile the synthesis of bentonite was carried out by the ball mill, coprecipitation and addition of cetyltrimethylammonium bromide (CTAB) surfactant. X-ray diffraction nanocomposite characterization showed that the particle size was 17.13 nm. Fourier transform infrared analysis showed the required absorption peak in photocatalysis because the OH group can react with holes and prevent electron–hole pair recombination. The morphology of the nanocomposite showed the occurrence of TiO2 pillarization in bentonite. The results of the X-ray fluorescence nanocomposite showed that the content of TiO2 and SiO2 was 65.22 and 17.4%, respectively.

Keywords: nanocomposite; adsorbent; ball mill; sol–gel; coprecipitation

1 Introduction

Titanium dioxide (TiO2) is a white pigment material with high brightness and refractive index. TiO2 accounts for 70% of the total volume of pigment production worldwide and is one among the top five nanoparticles used [1,2,3]. TiO2 materials can occur as paints, coatings, inks, pharmaceuticals, food products, cosmetics, and toothpaste. Currently, the production of TiO2 nanoparticles is quite significant because it has photocatalytic properties. The photocatalyst properties of TiO2 are functional as solar cells, adsorbent, self-cleaning, anti-fogging, and antibacterial [4,5,6].

The movement of electrons and holes in semiconductor nanomaterials depends on the effects of quantum confinement, size, and geometry of the material. The specific surface area and surface–volume ratio increase as the material size decreases. The photocatalytic activity of TiO2 depends on several properties such as crystal phase, surface area, lattice defects, and degree of crystallinity. The use of precursors also affects the quality of TiO2 nanoparticles. TiCl4 is a commonly used precursor of TiO2. It is because TiCl4 has several advantages such as good thermal stability, being highly reactive and can be used over a wide temperature range, and has a high vapor pressure [7,8]. The mixing of TiO2 through the synthesis of composite materials improves the properties of TiO2. In addition, the TiO2 composite structure can extend the absorption spectrum [9]. The manufacture of nano-TiO2 with the sol–gel process has been carried out, among others [10,11]. This is because the method works at room temperature [12]. However, the wet phase or sol method is the best way to control particle size, shape, and composition [13].

Bentonite is composed of montmorillonite with colloidal silica produced from the alteration of volcanic glass. Bentonite has calcic variations as a sign that the parent material is basaltic or adhesive. The main content of bentonite is the mineral montmorillonite (80%) with the chemical formula M x (Al4−x Mg x )Si8O20(OH)4·nH2O. Other contents in bentonite are impurities from several minerals such as quartz, illite, calcite, mica, and chlorite. Montmorillonite structure consists of one layer of alumina (AlO6) octahedral in the middle flanked by two layers of silica (SiO4) in a tetrahedral shape [14]. Bentonite has unique catalytic and adsorption properties. Therefore, bentonite is one of the most promising types of material as a safe nanotechnology material [15]. The adsorption ability of natural bentonite will be maximized when modifying it. Modification of bentonite has been carried out with various solutions, including HCl, H2SO4, and HNO3 [16,17,18,19]. Moreover, pillarization, intercalation of polycations, and calcination also produce a bentonite layer that is stable and constant at high temperatures.

Pillarization of bentonite with TiO2 can increase the basal distance and specific surface area of the material. It is because TiO2 has a large specific surface area. So it is possible to be combined with other materials without blocking the pores of these materials. In addition, the effect of GO/TiO2 nanocomposite in a solution based on natural surfactants on rock samples can be a candidate adsorbent [20,21]. The results of this study are expected to be used as new candidates as adsorbent materials.

2 Materials and methods

2.1 Synthesis of TiO2 nanoparticles

The TiCl4 solution was mixed with distilled water and stirred for 2 h using a magnetic stirrer. While stirring, NH4OH is added to the solution until it turns white. Then, the precipitate was dried at 70°C for 7 h. Figure 1 shows the schematic synthesis of TiO2 nanoparticles.

Figure 1 Schematic of TiO2 nanoparticle synthesis.
Figure 1

Schematic of TiO2 nanoparticle synthesis.

2.2 Synthesis of bentonite nanoparticles

The synthesis of bentonite nanoparticles refers to refs. [22,23]. Bentonite was calcined at a temperature of 700°C for 5 h and milled with a ball mill type, planetary ball mill, for 10 h with a rotation of 250 rpm. Furthermore, the synthesis of bentonite was performed by the coprecipitation method by mixing 6 M HCl using a stirrer at a temperature of 70°C for 4 h. Bentonite was mixed with 7 M NaOH using a stirrer at 70°C for 4 h. CTAB was dissolved in distilled water, heated, and stirred at 80°C for 1 h. CTAB and bentonite were mixed at 70°C for 3 h. The preparation of bentonite nanoparticles is shown in Figure 2.

Figure 2 Schematic of bentonite nanoparticle synthesis.
Figure 2

Schematic of bentonite nanoparticle synthesis.

2.3 Synthesis of TiO2 and bentonite nanocomposites

Figure 3 shows the preparation of TiO2 and bentonite composites. TiO2 and bentonite with a composition ratio (1:1) mixed with deionized water and ethanol were stirred using a magnetic stirrer for 5 h. Then, it was dried in an oven at 100°C for 4 h. Each sample is coded as shown in Table 1.

Figure 3 Schematic of bentonite and TiO2 nanocomposites synthesis.
Figure 3

Schematic of bentonite and TiO2 nanocomposites synthesis.

Table 1

Sample code

No Materials Sample code
1 Bentonite coprecipitation Bt
2 Bentonite coprecipitation + CTAB Bt–CTAB
3 TiO2 sol–gel TiO2
4 TiO2 + bentonite coprecipitation + CTAB TiO2–Bt–CTAB

2.4 Characterization methods

The nanocomposite’s phase structure and particle size were investigated by X-ray diffraction (XRD) Goniometer Shimadzu 6000 type using X-ray source Cu/Kα1 at wavelength = 1.54056. The analysis was carried out at an angle of 2θ ranging from 7 to 70°. The diffraction pattern was identified by comparing the diffractogram with the Joint Committee on Powder Diffraction Standard database. Meanwhile, the crystal size (D) was determined using the Scherrer equation:

(1) D = K λ β cos θ ,

where D is the crystal size (Ǻ), λ = 1.54056, θ is the Bragg angle, K is Scherrer’s constant with a general value of 0.9, and β is the half-width of the full width at half maximum peak in radians.

The functional group analysis was carried out using a Fourier transform infrared (FTIR) type Shimadzu IR-Prestige-21 made in Japan. The resolution used is 4.0, while the wavenumber ranges from 500 to 4,000 cm−1. The scanning electron microscope (SEM) analysis was carried out using the EVO MA 10 Zeiss instrument, and the chemical composition was analyzed by energy-dispersive X-ray spectroscopy (EDS; Bruker Quantax 200). X-ray fluorescence (XRF) characterization was carried out using XRF PANalytical Manipal 4. This tool can be used to test the elemental content of a material ranging from sodium to uranium.

3 Results

3.1 XRD characterization

The XRD pattern in Figure 4 shows a much lower peak broadening and the peak intensity in Bt–CTAB. Figure 4c shows the rutile phase resulting from the synthesis of the sol–gel method. The broadening and decreasing of the diffraction peaks in Figure 4 are the characteristics of TiO2, which indicate the successful preparation of TiO2–Bt–CTAB nanocomposites. Peak reduction is due to the TiO2 lattice distortion with the addition of bentonite [24,25]. The particle size of the sample is shown in Table 2. Meanwhile, XRD Data Collection shown in Table 3.

Figure 4 XRD diffraction pattern of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.
Figure 4

XRD diffraction pattern of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.

Table 2

Particle size data

Sample code Particle size (nm)
Bt 18.47
Bt–CTAB 17.04
TiO2 29.60
TiO2–Bt–CTAB 17.13

The particle size of the TiO2–Bt–CTAB nanocomposite decreased. The decrease in particle size was also confirmed by the SEM results presented in Figure 6. This decrease shows that bentonite can inhibit the growth of TiO2 [26,27,28].

Table 3

XRD analysis of Bt, Bt–CTAB, TiO2, TiO2–Bt–CTAB

Date Bt Bt–CTAB TiO2 TiO2–Bt–CTAB
Crystal system Trigonal (hexagonal axes) Trigonal (hexagonal axes) Tetragonal Trigonal (hexagonal axes)
Space group P 31 2 1 (152) P 32 2 1S P42/mnm (136) P 31 2 1 (152)
Unit cell a = 4.6764 Å a = 4.9160 Å a = 4.594 Å a = 4.8120 Å
c = 5.2475 Å c = 5.4054 Å c = 2.9589 Å c = 5.3270 Å
Density 3.01200 g·cm−3 2.646 g·cm−3 4.248 g·cm−3 2.80200 g·cm−3
2θ angle 26.47 26.48 27.67 27.37
Maximum d hkl 011 110 110 011
Intensity I/I 0 1,000 1,000 999. 1000.0
Lattice distance d (Å) 3.2061 3.3663 3.2485 3.2823
2θ angle 19.81 30.78 32.74 31.15
Maximum d hkl 100 100 211 100
Intensity I/I 0 858.2 865.03 480.0 204.6
Lattice distance d (Å) 4.0499 2.9051 1.6876 4.1673
2θ angle 24.19 24.6 36.12
Maximum d hkl 200 100 101 112
Intensity I/I 0 527.3 456.40 436.0 107.5
Lattice distance d (Å) 2.0249 3.6537 2.4876 1.7854
2θ angle 34.82 19.68 41.09 54.51
Maximum d hkl 110 011 111 012
Intensity I/I 0 375.8 371.77 171.0 103.0
Lattice distance d (Å) 2.3382 4.5113 2.1875 2.2443

3.2 FTIR analysis

The spectra in Figure 5a and b have the same graph. The absorption band of 1141.47 cm−1 is Si–O–Si. It is confirmed by XRF results, where bentonite has a significant silica content. In addition, a specific absorption peak was found at 3621.59 cm−1, which is the stretching vibration of Al–OH and Si–OH [29].

Figure 5 FTIR of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.
Figure 5

FTIR of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.

The absorption bands 2849.43 and 2910.79 shown in Figure 5b are C–H vibrations of the methyl and methylene groups from CTAB surfactant residues. Figure 5c shows the peak of 747.72 corresponding to the Ti–O vibration in the crystal lattice [30]. Figure 2d shows the absorption bands at 2839.20 and 2,926 cm−1 that are asymmetric and symmetrical strain vibrations of CH3 and CH2 of the CTAB aliphatic chain [23]. The absorption band 3621.59 represents the deformation and strain vibration of the OH group, and this band indicates the presence of weak molecules in TiO2. This property is required in photocatalysis because the OH group can react with holes and prevent the recombination of electron–hole pairs [31,32].

3.3 SEM analysis

The morphology in Figure 6a shows a non-uniform lump of particles. However in Figure 6b, the particles are seen to be distributed, and no streaking occurs. This is due to the interaction between CTAB particles and hydroxyl-Al cations inserted into bentonite, between these ions and the bentonite layer, thus causing the composition of the material, which mainly consists of a layer of bentonite [33].

Figure 6 Morphology of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.
Figure 6

Morphology of (a) Bt, (b) Bt–CTAB, (c) TiO2, and (d) TiO2–Bt–CTAB.

Figure 6d shows the number of holes on the silicate surface almost entirely in the etched TiO2-pillared bentonite. This surface implies that the TiO2-pillared bentonite has many holes etched into the silicate externally and internally. In addition, the agglomeration due to the addition of CTAB forms a block layer [34]. The morphology of the pillared bentonite has a flat layered structure, with a large number of holes between the lamellae, showing good adsorption capacity. The phenomenon of delamination can be ascribed to the fact that TiO2 as a pillaring agent enters the bentonite interlayers, which can destroy the original structure and enlarge the distance between the layers [35]. In contrast to Figure 6c, which shows a smooth surface consisting of silicates, the surface has not been scratched with chemical reagents on TiO2 [36]. The number of elements in Table 4 obtained from the EDS analysis is in accordance with that obtained with XRF [37].

Table 4

The number of elements detected through EDX analysis

No. Elements Bt wt(%) Bt-CTAB wt(%) TiO2 wt(%) TiO2–Bt–CTAB wt(%)
1 Ti 0.70 — 34.91 40.82
2 O 51.40 47.33 45.66 30.00
3 Ba — — 15.21 25.35
4 F — — — 1.39
5 Si 27.57 23.52 4.21 1.13
6 Al 11.24 14.77 — 0.90
7 Cl — — — 0.39
8 Ag 1.37 4.37 — —
9 Fe 3.53 3.61 — —
10 Mg 2.38 2.85 — —
11 Na 1 2.50 — —
12 K 0.81 1.07 — —

3.4 XRF analysis

XRF analysis of Bt and Bt–CTAB in Table 5 shows that SiO2 and Al2O3 are the main constituents of bentonite, with small amounts of other metal oxides [38]. Decreasing the content of SiO2 and Al2O3 with the addition of CTAB is in accordance with the results of previous studies [39]. Meanwhile, the TiO2 content in the TiO2 sample synthesized by the sol–gel process was 87.89%, followed by 11.6% Cl. The Cl content probably comes from the TiCl4 precursor. In TiO2–Bt–CTAB, the content of TiO2 and SiO2 is 65.22 and 17.4%, respectively. The dominant amount of TiO2 content is probably caused by the distortion of TiO2 in bentonite.

Table 5

Elements obtained from XRF analysis

Compound Bt (%) Bt–CTAB (%) TiO2 (%) TiO2–Bt–CTAB (%)
TiO2 2.04 1.68 87.89 65.22
SiO2 57.3 51.9 17.4
Al2O3 17 14 8
K2O 1.18 1.1 0.3
CaO 3.78 3.06 0.15 1.27
V2O5 0.05 0.04 0.42
Fe2O3 18.9 14.3 5.26
P2O5 0.6 0.02 0.3
WO3 0.11 0.13
PtO2
Br 13.1 1.6
Cl — 11.6
ZnO 0.03 0.052 0.07

A discussion of the physical properties obtained and the novelty of this article compared to previous studies are presented in Table 6.

Table 6

Discussion of the physical properties obtained and the novelty of this article

Physical properties Research result Previous result
Particle size 17.13 nm 15.9 nm [40]
Distance between layers 4.1673 Ǻ 16.9807 Å [36]
Morphology The number of holes on the silicate surface is almost entirely in the etched TiO2 pillared bentonite. This surface implies that the TiO2 pillared bentonite has many holes etched into the silicate externally and internally. In addition, the agglomeration due to the addition of CTAB forms a block layer TiO2 particles have been inserted into the bentonite surface of the smaller TiO2 grains on the outer surface of the bentonite [41]

4 Conclusion

Physical analysis of TiO2 and bentonite nanocomposite shows that these materials can be used as adsorbents. The results of the analysis with XRD show a decrease in the particle size of the nanocomposite. In addition, the FTIR shows deformation and strain vibration of the OH group, and these bands indicate the presence of water molecules that are weakly bound to TiO2. This characteristic is needed in photocatalysis because the OH group can react with holes and prevent the recombination of electron–hole pairs. SEM results describe the pillarization of TiO2 on bentonite, which was confirmed by XRF.

Acknowledgment

This research was supported by the Ministry of Education and Culture, Research and Technology for basic research (PD) based on the Implementation Contract No. 003/UN33.8/PL/DRPM-DJ/2021, July 15, 2021.

  1. Funding information: This research was supported by the Ministry of Education and Culture, Research and Technology for basic research (PD) based on the Implementation Contract No. 003/UN33.8/PL/DRPM-DJ/2021, July 15, 2021.

  2. Author contributions: Nurdin Bukit: writing – original draft, writing – review and editing, methodology, and formal analysis; Eva Marlina Ginting: writing – original draft, formal analysis, visualization, and project administration; Erna Frida: formal analysis, visualization, and project administration; Bunga Fisikanta Bukit: formal analysis, visualization, and project administration

  3. Conflict of interest: Authors state no conflict of interest.

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Received: 2021-08-15
Revised: 2021-10-07
Accepted: 2021-10-17
Published Online: 2021-12-16

© 2021 Nurdin Bukit et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/rams-2021-0076
Keywords for this article
nanocomposite; adsorbent; ball mill; sol–gel; coprecipitation
Creative Commons
BY 4.0

Articles in the same Issue

  1. Review Articles
  2. A review on filler materials for brazing of carbon-carbon composites
  3. Nanotechnology-based materials as emerging trends for dental applications
  4. A review on allotropes of carbon and natural filler-reinforced thermomechanical properties of upgraded epoxy hybrid composite
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  6. A review of current physical techniques for dispersion of cellulose nanomaterials in polymer matrices
  7. Review on structural damage rehabilitation and performance assessment of asphalt pavements
  8. Recent development in graphene-reinforced aluminium matrix composite: A review
  9. Mechanical behaviour of precast prestressed reinforced concrete beam–column joints in elevated station platforms subjected to vertical cyclic loading
  10. Effect of polythiophene thickness on hybrid sensor sensitivity
  11. Investigation on the relationship between CT numbers and marble failure under different confining pressures
  12. Finite element analysis on the bond behavior of steel bar in salt–frost-damaged recycled coarse aggregate concrete
  13. From passive to active sorting in microfluidics: A review
  14. Research Articles
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  16. Mesoporous silica nanoparticles functionalized with folic acid for targeted release Cis-Pt to glioblastoma cells
  17. Magnetic behavior of Fe-doped of multicomponent bismuth niobate pyrochlore
  18. Study of surfaces, produced with the use of granite and titanium, for applications with solar thermal collectors
  19. Magnetic moment centers in titanium dioxide photocatalysts loaded on reduced graphene oxide flakes
  20. Mechanical model and contact properties of double row slewing ball bearing for wind turbine
  21. Sandwich panel with in-plane honeycombs in different Poisson's ratio under low to medium impact loads
  22. Effects of load types and critical molar ratios on strength properties and geopolymerization mechanism
  23. Nanoparticles in enhancing microwave imaging and microwave Hyperthermia effect for liver cancer treatment
  24. FEM micromechanical modeling of nanocomposites with carbon nanotubes
  25. Effect of fiber breakage position on the mechanical performance of unidirectional carbon fiber/epoxy composites
  26. Removal of cadmium and lead from aqueous solutions using iron phosphate-modified pollen microspheres as adsorbents
  27. Load identification and fatigue evaluation via wind-induced attitude decoupling of railway catenary
  28. Residual compression property and response of honeycomb sandwich structures subjected to single and repeated quasi-static indentation
  29. Experimental and modeling investigations of the behaviors of syntactic foam sandwich panels with lattice webs under crushing loads
  30. Effect of storage time and temperature on dissolved state of cellulose in TBAH-based solvents and mechanical property of regenerated films
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  36. Dynamic characteristics of tailings dam with geotextile tubes under seismic load
  37. Study on impact resistance of composite rocket launcher
  38. Effects of TVSR process on the dimensional stability and residual stress of 7075 aluminum alloy parts
  39. Dynamics of a rotating hollow FGM beam in the temperature field
  40. Development and characterization of bioglass incorporated plasma electrolytic oxidation layer on titanium substrate for biomedical application
  41. Effect of laser-assisted ultrasonic vibration dressing parameters of a cubic boron nitride grinding wheel on grinding force, surface quality, and particle morphology
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  44. Effect of scan speed on grain and microstructural morphology for laser additive manufacturing of 304 stainless steel
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  46. Improving the precision of micro-EDM for blind holes in titanium alloy by fixed reference axial compensation
  47. Electrolytic production and characterization of nickel–rhenium alloy coatings
  48. DC magnetization of titania supported on reduced graphene oxide flakes
  49. Analytical bond behavior of cold drawn SMA crimped fibers considering embedded length and fiber wave depth
  50. Structural and hydrogen storage characterization of nanocrystalline magnesium synthesized by ECAP and catalyzed by different nanotube additives
  51. Mechanical property of octahedron Ti6Al4V fabricated by selective laser melting
  52. Physical analysis of TiO2 and bentonite nanocomposite as adsorbent materials
  53. The optimization of friction disc gear-shaping process aiming at residual stress and machining deformation
  54. Optimization of EI961 steel spheroidization process for subsequent use in additive manufacturing: Effect of plasma treatment on the properties of EI961 powder
  55. Effect of ultrasonic field on the microstructure and mechanical properties of sand-casting AlSi7Mg0.3 alloy
  56. Influence of different material parameters on nonlinear vibration of the cylindrical skeleton supported prestressed fabric composite membrane
  57. Investigations of polyamide nano-composites containing bentonite and organo-modified clays: Mechanical, thermal, structural and processing performances
  58. Conductive thermoplastic vulcanizates based on carbon black-filled bromo-isobutylene-isoprene rubber (BIIR)/polypropylene (PP)
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  60. Study on underwater vibro-acoustic characteristics of carbon/glass hybrid composite laminates
  61. A numerical study on the low-velocity impact behavior of the Twaron® fabric subjected to oblique impact
  62. Erratum
  63. Erratum to “Effect of PVA fiber on mechanical properties of fly ash-based geopolymer concrete”
  64. Topical Issue on Advances in Infrastructure or Construction Materials – Recycled Materials, Wood, and Concrete
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  67. Development of an innovative composite sandwich matting with GFRP facesheets and wood core
  68. Relationship between percolation mechanism and pore characteristics of recycled permeable bricks based on X-ray computed tomography
  69. Feasibility study of cement-stabilized materials using 100% mixed recycled aggregates from perspectives of mechanical properties and microstructure
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  71. Research on nano-concrete-filled steel tubular columns with end plates after lateral impact
  72. Dynamic analysis of multilayer-reinforced concrete frame structures based on NewMark-β method
  73. Experimental study on mechanical properties and microstructures of steel fiber-reinforced fly ash-metakaolin geopolymer-recycled concrete
  74. Fractal characteristic of recycled aggregate and its influence on physical property of recycled aggregate concrete
  75. Properties of wood-based composites manufactured from densified beech wood in viscoelastic and plastic region of the force-deflection diagram (FDD)
  76. Durability of geopolymers and geopolymer concretes: A review
  77. Research progress on mechanical properties of geopolymer recycled aggregate concrete
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