Physical and Chemical Investigation of TiO<sub>2</sub> Nanotubes Treated with Isopropyl Triisostearoyl Titanate (KR-TTS)

Sabri, Ban Ali; Satgunam, Meenaloshini; Manap, A.; Gnanasagaran, Constance L.; Ramachandran, Karthikeyan

doi:https://doi.org/10.1155/2023/7961857

Journal of Nanomaterials

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Abstract Introduction Results and Discussion Conclusion Data Availability Conflicts of Interest Authors’ Contributions References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 7961857 | https://doi.org/10.1155/2023/7961857

Physical and Chemical Investigation of TiO₂ Nanotubes Treated with Isopropyl Triisostearoyl Titanate (KR-TTS)

Ban Ali Sabri,¹Meenaloshini Satgunam,²A. Manap,³Constance L. Gnanasagaran,⁴and Karthikeyan Ramachandran⁴

Academic Editor: Sergio M. Acuña

Received26 Oct 2022

Revised15 Dec 2022

Accepted20 Jan 2023

Published28 Apr 2023

Abstract

The aim of this study is to investigate the effect of isopropyl triisostearoyl titanate (KR-TTS) as a titanate coupling agent (TCA) on surface modification of TiO₂ nanotube (TNT) material. From the physical and chemical studies that have been performed on the modified TiO₂ nanotube, scanning electron microscope micrographs, energy-dispersive X-ray and viscosity indicated that there was significant reduction in particle aggregation of the modified TiO₂ Nanotube. FTIR spectroscopy confirmed that the functional group of the TCA reacted with the hydroxyl groups present on the surface of TiO₂ nanotube resulting in an altered surface property from being hydrophilic to hydrophobic. X-ray diffraction indicated that crystalline structure did not change upon the modification with the coupling agent. Isopropyl triisostearoyl titanate (KR-TTS) is found to be superior in performance and has a significant effect on the dispersion and resolving of agglomeration. This paper presents the effect of surface modification with the TCA of isopropyl triisostearoyl titanate (KR-TTS) type on the TiO₂ nanotube material.

1. Introduction

The introduction of nanoscale material offers new, promising additives for improvement of the mechanical properties because of their high surface area to volume ratio [1]. Nanotubes consist of long cylinders with a hollow cavity at the center that exhibits increased surface area compared to nanoparticles (NPs) [2]. The aspect ratio of nanotubes is usually more than 10 and it can reach up to several thousand [3]. The surface area of TiO₂ nanotube is about five times higher than the titanium oxide nanoparticle (NP), and it is around 250 m²/g [4–6].

Nanotitanium oxide (TiO₂) has a wide variety and different applications due to its recognized specifications such as low costs, optical and electronic properties, chemical stability, high photocatalytic activity, nontoxicity, UV protectivity, antibacterial agent, and environmental purification [7–10]. Titanium is a potential material in dental and medical applications due to the excellent bioactivity, biocompatibility, and mechanical properties [6, 11, 12]. This material, which is high in stability, poses great aesthetic capabilities, low toxicity, high efficiency, and abundancy, makes it a favorable antimicrobial additive [6, 13].

Titanium oxide nanotube (TiO₂) has been used recently as a polymer reinforcement and has provided an excellent effect on biomedical compatibility as well as in improving the mechanical properties of acrylic resins [4, 9, 14]. It has been approved from the previous studies that the use of nanotubes additives was a success in the resin-based bone cement and dentals [4]. It also reported that the open-ended tubular structure of the nanotubes may allow the matrix material to enter into the tubes by capillary action and form a stronger composite which leads to increased load transformation [4]. Nonetheless, several studies demonstrated that blank TiO₂ nanotube addition was limited due to its clustering and aggregation which was caused by its high surface energy. Its tendency for aggregation causes the creation of a weak area and limits its application [15, 16].

The surface modification of materials means grafting of organic coatings on its surface which can be performed with the coupling agent to change the surface from having hydrophilic to hydrophobic properties. It can be carried out by utilizing physical and chemical interactions between the nanomaterial and the modifiers through the creation of a molecular bridges to solve the problems of clustering and aggregation [17–19]. Throughout the research findings, it has been concluded that the titanium coupling agents (TCAs) have more significant properties in treating unlimited types of materials. Researches related to dental applications show that the biocompatibility of TCAs were superior in terms of hydrolytic stability in oral and wet environments [1, 20–22]. This paper presents the TiO₂ nanotube modification with the titanate coupling agent (TCA) of isopropyl triisostearoyl titanate (KR-TTS) type.

2. Experimental Procedure

2.1. Materials

Titanium dioxide (TiO₂) nanotube with an average diameter of 25 nm was provided by Sigma-Aldrich, USA, and specific surface area of 150 m²/g and molecular weight of 79.9 g/mol were used as the treated material. Isopropyl triisostearoyl titanate (KR-TTS) provided by Kenrich Petrochemicals, USA, was used as the surface treatment material, it is a light brown-reddish liquid with a density of 0.92 g/cm³ and having a chemical composition of C₅₇H₁₁₂O₇Ti. Toluene (TOL/Sigma-Aldrich, USA, 99.89% purity, 92.14 g/mol molecular weight) as an anhydrous colorless liquid used to mix with isopropyl triisostearoyl titanate (KR-TTS) by a specific percentage, its chemical composition was C₇H₈, and it is used to prevent the hydrolysis of coupling agent near the surface of TiO₂. Also, a colorless liquid material ethyl alcohol (ethanol) provided by Sigma-Aldrich, USA, 95% purity, with a chemical composition of C₂H₆O, molecular weight of 46.07 g/mol, has been used for washing the treated material in order to eliminate the residual titante coupling agent (TCA) and toluene (TOL). Paraffin oil is a viscous liquid provided by Sigma-Aldrich, USA, with a density of 0.861 g/cm³, used to evaluate the surface modification of the fillers through the viscosity test.

2.2. Surface Modification of TiO₂ Nanotubes

An identified amount of 2.0 g of inorganic TiO₂ nanotube powder has been weighted with four-digit analog balance (MonoBloc, model no. 8303, China). The weighted TiO₂ nanotubes were heated in a vacuumed electrical tube furnace under a temperature of 80°C for 4 hr in order to remove any moisture that may available on the powder surface. To prepare the coupling agent solution, an amount of 2 wt% of isopropyl triisostearoyl titanate (KR-TTS) (relative to the weighted TiO₂ nanotubes) has been added into a beaker containing of (100 mL) of toluene liquid and stirred by the speed of 300 rpm for 30 min, using magnetic stirrer apparatus (INTLLAB MS-500, China). Then, TiO₂ nanotubes have been dispersed in the coupling moisture and stirred by the indicated magnetic stirrer, with a speed of 300 rpm for 1 hr and at room temperature. TiO₂ nanotubes moisture has been filtered from the TCA and toluene liquids by using a centrifugal filter apparatus (Eppendorf Centrifuge 5415 R, Germany) to separate the filler from the moisture followed by filtering with a laboratory filter paper, and then washing by ethanol for three times. The obtained treated TiO₂ nanotubes have been dried with the use of electrical vacuumed tube furnace at 80°C for 6 hr, by placing the powder in the vacuumed quartz tube. After the dryness process, the treated powder has been kept in a vessel. The last drying process of the TiO₂ nanotubes was conducted to perform a complete evaporation of any supposed residual ethanol and toluene.

2.3. TiO₂ Nanotubes Characterizations

2.3.1. Fourier Transform Infrared Spectroscopy (FTIR) Test

Fourier transform infrared (FTIR) is a nondestructive, optical performance inspection used to recognize the grafting of the functional groups of coupling agents into the surface of the TiO₂ nanotubes and its modification. FTIR spectrometer used was Bruker FTIR Alpha Universal sampling module, USA. The testing sample has been prepared with the KBr disk. Materiel has been scanned for 10 times with a wavelength range of 500–4,000 cm⁻¹ and a resolution set to 4 cm⁻¹.

2.3.2. X-Ray Diffraction (XRD) Test

X-ray diffraction has been used to characterize the atomic structure of the TiO₂ nanotube, analyzing their crystal structures, and to evaluate if the TCA was altered the filler atomic structure. The XRD diffractometer apparatus Bruker D2 PHASER, XRD powder diffractometer, USA, was used to investigate the crystal structure of the treated TiO₂ nanotube materials, where the measuring range was 2θ = 5°–90° and scanning speed was 10/min.

2.3.3. SEM Investigation

Scanning electron microscope (SEM) has been used for investigating the morphology and agglomeration of the modified material. SEM device used was Zeiss GEMINI SEM 500, Germany, model with a voltage range from 0.2 to 30 kV. The apparatus used was using a focused beam of electrons with a high energy in order to create a variation of signals on the surface of the sample. The obtained signals reflect an indication about the external morphology and the orientation of materials forming the powder.

2.3.4. Viscosity Test

The viscosity test provides an indication on the range of change in viscosity of the treated filler in comparison to the untreated filler. This test has been conducted by mixing of filler with paraffin oil and measuring the moisture viscosity by the viscometer apparatus. Ten grams from each treated and nontreated filler have been immersed individually in a scald container (beaker) of 100 mm diameter containing of 150 mL liquid paraffin and mixing the filler with the paraffin by a magnetic stirrer of 300 rpm for 10 min. The spindle of the rotary viscometer has been immersed into the center of the scaler container (beaker) which contains the paraffin oil and adjusted until the oil level reaches to the groove on the spindle. This process has been followed by setting the machine rotational speed of 30 rpm for 1 min at an ambient temperature of 25°C before reading the measured viscosity. The viscometer apparatus used was Brookfield DV-E Viscometer, USA, with a maximum rotational speed of 100 rpm.

3. Results and Discussion

3.1. Fourier Transform Infrared Spectroscopy (FTIR) Test of TiO₂ Nanotubes

The schematic for chemical process of grafting TCA, isopropyl triisostearoyl titanate (KR-TTS), on the surface of titanium nanotube (TiO₂)nt, is shown in Figure 1.

In Figure 1, the hydrolysable group of the isopropyl triisostearoyl titanate (KR-TTS) has been denoted by the (X) letter. However, this hydrolysable group (X) reacted with the hydroxide group (hydrogen and oxygen connected together by a covalent bond and localized on the nanotube (TiO₂)nt surface). Then, it will lead to the creation of the bond that is connecting the Ti(X) of the TCA with the oxygen (O) on the nanotube (TiO₂)nt surface and offering the (O-TiX₃).

Figure 2 represents the FTIR test results of TiO₂ nanotube material before and after treatment with the TCA. The graph area in the figure presenting two spectra, the region before 1,500 cm⁻¹ represents the fingerprint of the material itself and the area after the 1,500 cm⁻¹ scales represents the functional group region. The wide peak presented in the graph at the fingerprint region for both of the modified TiO₂ (M-TiO₂) and none modified (TiO₂) material and at the range of (400–700) cm⁻¹ refers to the Ti–O and O–Ti–O bonds [5, 23–25]. The broad peak presented at 3,320 cm⁻¹ and the peak at 1,622 cm⁻¹ can be attributed to the bending vibration peak and stretching vibrations peak of the hydroxyl (O–H and H–O–H) available on the surface of TiO₂ nanotube [26, 27]. Upon comparing the graph lines of the treated (M-TiO₂) and none treated TiO₂ nanotube material, the change in peak after treatment presented at 2,381cm⁻¹ can be attributed to the stretching vibrations peak initiated from C=O of CO₂, that has been absorbed by the TiO₂ nanotube material [28]. The sharp initiated peak in the line of treated TiO₂ nanotube (M-TiO₂) at 2,919 cm⁻¹ represents the absorption peaks of methylene and methyl [29]. Also, at the same modified line b (M-TiO₂) at Figure 2, the small initiated peak at 1,682 cm⁻¹ referring to C=O of the titanate coupling agents [25, 28, 30].

However, all of the mentioned factors proof that the functional groups of the coupling agent (isopropyl triisostearoyl titanate (KR-TTS)) have been reacted with the hydroxyl groups available on the surface of the TiO₂ nanotube and caused a change of ceramic surface properties from hydrophilic to be hydrophobic properties.

3.2. X-Ray Diffraction (XRD) Test of TiO₂ Nanotubes

XRD results are presented in the two graph patterns, as shown in Figure 3, it has been indicated a sharp diffraction peaks at 26.1°, 38.48°, 47.43°, 55.67°, 57.6°, and 67.86°, where those peaks represent the anatase crystal phase of the titanate nanotube (TiO₂)nt according to International Center for Diffraction Data (ICDD PDF No. 89–4921) [5, 22, 31].

The XRD figure of the TiO₂ nanotube (TiO₂)nt presents an inconsiderable change in peaks of the modified-TiO₂ curve (M-TiO₂), line b in Figure 3, in comparison to line a in Figure 3 of the nontreated titania nanotubes TiO₂. The only recognizable change is the shifting up of the whole curve, while the overall shape and broad of peaks were almost still the same. The initiated difference was due to the treatment effect of the TCA, while the TCA amount is very small and does not generate any diffraction peaks in the modified-TiO₂ (M-TiO₂), line b in Figure 3, and that means the crystalline structure does not changed upon the modification of TiO₂ nanotube with the TCA.

3.3. SEM Investigation

Figure 4 presents the SEM micrograph pictures for the none modified (TiO₂) nanotubes and modified one (M-TiO₂). Five magnification ranges have been investigated, but only two ranges were selected, 200 and 500 nm deemed suitable for revealing the distribution and agglomeration of nanopowder.

In Figures 4(a) and 4(b), it is clear that a port of unmodified TiO₂ nanotubes has happened to aggregate. While, in Figures 4(c) and (d), the aggregation of TiO₂ nanotubes is less and weaker. However, according to the SEM micrograph pictures, it could be determined that TCA (isopropyl triisostearoyl titanate (KR-TTS)) works as a perfect compatibility agent for the TiO₂ nanotube and breaking up the aggregation and reduced the agglomeration successfully. Same conclusion has obtained by a study conducted by Monte [32], as it has been stated that the dispersion of inorganic filler, like the CaCO₃ and carbon black, will improve and the aggregation will decrease, when the water of hydration available on the particle surface replaced by a monomolecular layer of organofunctional titanate. Similarly, a study carried out by Wah et al. [33] investigating the effect of TCA on the rheological behavior of filling the polypropylene by talc material revealed that TCA had a positive effect in improving the dispersion quality of filler into the matrix material, as well as treatment material causing a decrease in the melt viscosity of the filled polypropylene.

3.4. Viscosity Test

Figure 5 presents the involvement of 10 g from each of modified M-TiO₂ nanotube (test tube a) and nonmodified TiO₂ nanotubes (test tube b) into 150 mL of liquid paraffin. The dispersion of the modified material has been investigated through measuring the viscosity values of immersed TiO₂ nanotubes in liquid paraffin before and after treatment. The obtained results of the measured viscosity of the TiO₂ in liquid paraffine before treatment was 70.30 mPa⋅s (tube b), as shown in Figure 5, while after modifying TiO₂, as shown in tube a of Figure 5, the measured viscosity decreased to 9.43 mPa⋅s. That means the viscosity of the modified TiO₂ material in liquid paraffin has been reduced by 86.58%. Also, it can be recognized from Figure 5(a) that the dispersion of the modified TiO₂ (M-TiO₂) in liquid paraffin is uniform, while tube b in Figure 5 presents a precipitation and poor dispersion of unmodified TiO₂ nanotube.

(a)

(b)

The reason of the high viscosity for the unmodified TiO₂ nanotubes into liquid paraffin was related to the increase of resistance while the spindles rotor of viscometer apparatus flows between two different incompatible materials. However, in the case of M-TiO₂ nanotubes, the dispersion in liquid paraffin was increased and could be related to the change of nanotube surface properties upon treatment. The treatment caused a decrease in resistance which lead to a reduction in the value of viscosity. Therefore, the change in measured viscosities can verify that there was an interaction between the TiO₂ nanotubes and (KR-TTS) TCA and the surface properties of M-TiO₂ nanotubes have been changed from being hydrophilic to be hydrophobic.

4. Conclusion

This study presents the TiO₂ nanotube modification with the TCA of isopropyl triisostearoyl titanate (KR-TTS) type. The chemical investigations conducted by FTIR test verified that the interactions happened between TiO₂ nanotube and some groups of isopropyl triisostearoyl titanate (KR-TTS) have been introduced into the surface of TiO₂-nanotube by coupling reaction with the hydroxyl groups. The XRD structural investigation also confirmed that the crystalline structures of TiO₂ nanotube did not change upon treatment with the TCA (isopropyl triisostearoyl titanate (KR-TTS)). The physical investigations of this study confirmed through the SEM micrographs that the modification process broke up the aggregation of TiO₂ nanotubes into finer particles. Also, the dispersion has been increased in paraffin oil and confirmed through the 86.58% reduction in viscosity measurements of the modified material. However, isopropyl triisostearoyl titanate (KR-TTS) was a perfect treatment material for the modification of TiO₂ nanotube surface and supreme to overcome the agglomeration, improve dispersion, and changing the TiO₂-nanotube materials surface to be of hydrophobic properties.

Data Availability

The graphs and figures data used to support the findings of this study are included within the article. The optimization process results data used to support the findings of this study are available from the corresponding author upon request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Authors’ Contributions

Conceptualization and methodology by B.A.S.; investigation by B.A.S. and M.S.; results analysis by B.A.S., M.S., and A.M.; writing an original draft by B.A.S.; project administration and scientific supervision by M.S and A.M.; methodology, investigation, data curation, and validation by B.A.S.; reviewing and editing by M.S., A.M., C.L.G., and K.R. All authors have read and agreed to the published version of the manuscript as presented.

Funding

This work was supported by Tenaga Nasional Berhad (TNB) and UNITEN through the BOLD Research Grant under the project code of J510050002/2022022.

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Copyright © 2023 Ban Ali Sabri et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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