The study of the particle size effect on the physical properties of TiO2/cellulose acetate composite films

Hajer A. Ali; Nahida J. Hameed

doi:10.1515/jmbm-2022-0019

Article Open Access

The study of the particle size effect on the physical properties of TiO₂/cellulose acetate composite films

Hajer A. Ali and Nahida J. Hameed

Published/Copyright: May 26, 2022

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From the journal Journal of the Mechanical Behavior of Materials Volume 31 Issue 1

Abstract

The cast method was used to synthesize cellulose acetate (CA)/titanium oxide (TiO₂) composites by varying TiO₂ particle sizes at different weight ratios of 1, 1.5, 2, 2.5, and 3 wt%. The relationship between structural diversity and performance was explored. Microstructures and chemical composition of as-prepared composite films were revealed using field-emission scanning electron microscopy and Fourier-transform infrared spectroscopy. The tensile strength increased from 46.8 MPa for pure CA to 54.7 MPa for the CA-1% micro-TiO₂ composite and 81.7 MPa for the CA-2% nano-TiO₂ composite, according to the mechanical properties. The tensile strength decreased due to some degrees of agglomeration of filler particles above a critical content. UV-vis transmittance spectra showed that pure CA was almost transparent, CA-micro-TiO₂ films were less transparent than pure CA, and CA-nano-TiO₂ films could efficiently block the light. XRD diffraction for the synthesized membranes was performed. The patterns of micro-TiO₂ and nano-TiO₂ were shown as 2θ = 25° for the anatase phase and 2θ = 18.5 for the pure CA film, respectively. The hydrophilicity of films was also measured using the sessile drop technique. The contact angle value for the pure CA was 61.3°. As the amount of TiO₂ added to the films increased, the contact angles of the CA-micro TiO₂ and CA-nano TiO₂ films reduced from 53.2° to 29° and from 51.5° to 27°, respectively. The produced films’ improved wettability indicated that these films could be employed as filters.

Keywords: biodegradable; cellulose acetate; mechanical properties; nanocomposite; titanium oxide

1 Introduction

Traditional synthetic polymers, such as polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), polyterephthalate (PET), and polyurethane (PU) which have been available for decades, have been applied as food packaging, medicine, waterproofing, and coating materials. Their superior properties such as good mechanical performance, low density, low cost, high chemical stability and a wide range of fabrication techniques make them a typical choice for many industrial applications [1]. However, the only drawback is the low degradation rate of their wastes, which is growing rapidly and may eventually become a serious environmental challenge. Several methods and techniques have emerged to overcome this challenge such as recycling and reusing polymer waste [2,3,4]. However, the most efficient way is to develop environmentally friendly biodegradable polymers such as chitosan, starch, and cellulose as an alternative to the traditional materials.

Cellulose acetate (CA) is a common natural organic polymer that can be transformed into high-end derivatives [5], but some of its properties, such as good appearance, biodegradability, and great durability, make it more favorable than its derivatives [6]. Using the esterification technique, CA can be produced from naturally produced cellulose substances including wood, cotton, and rice husk, as well as recyclable materials like paper [7,8]. Because of its biodegradation, nontoxicity, transparency, hydrophilicity and cost effectiveness, it appears to be a viable material for a variety of uses such as filters, drug delivery agents, food packaging films, and medical implants [9]. However, due to its brittleness and high sensitivity to moisture, it is not suitable for a wider range of applications in composite films [10]. Composite films that were developed overcome this difficulty by mixing inorganic oxide (TiO₂) with a CA solution. Because of its steady nature, availability, and suitability for various applications, TiO₂ has been the focus of many studies [11,12]. Several research teams have used the phase reversal method to create various polymer–TiO₂ composite films. Water flow and antifouling properties were greatly improved by polyethersulfone/TiO₂ composite ultrafiltration films [13]. The electrospinning process can create PU/TiO₂/fly ash composite water purification films and CA–TiO₂ films for water treatment applications [14,15]. To meet the needs of various industries, researchers created polyacrylonitrile–TiO₂ [16], TiO₂/polyvinyl alcohol [17], and TiO₂/PVDF composite films [18]; polysulfone enhanced films with TiO₂ nanofibers [19]; CA/MIL-53-NH₂ film for efficient chlorpyrifos’ elimination [20]; CA/Ti-MIL-NH₂ films for a chosen pharmaceutical residue removal [21]; CA/Cu-MOF films for selective dimethoate pesticide removal from wastewaters [22]; and CA/employable metal (Ag and Pd)/MIL-125-NH₂ films for reducing nitro-aromatics reducing via visible-light photocatalysis [23]. The current study focuses on the synthesis and application of CA films that combine micro- or nano-TiO₂ nanoparticles. It is different from previous studies because it incorporates different particle sizes and processes and conducts various examinations for filter application. The physical, chemical, and structural properties of CA/micro- or nano-TiO₂ composite films, as well as XRD patterns and contact angles, are investigated.

2 Materials and methods

2.1 Materials

In this work, CA (CDH India; acetyl content, 29–45%; maximum limit of impurities, 0.1%; free acid [as acetic acid], 5.0%; sulfated ash loss on drying at 105°C, 0.1%) and AR/ACS-grade acetone (2-propanone, dimethylketone; CDH India) (MW: 58.08) were utilized.

Titanium oxide nanoparticles/nanopowders (TiO₂, anatase, 99.5%) of particle size (20–80) nm were purchased from Skyspring (USA). Micro-TiO₂ with particle sizes ranging from 100 to 2,000 nm was supplied by Nanoshel (USA).

2.2 Composite polymer solution preparation

The primary solution of CA was made by dissolving 7 g of CA powder in 100 mL of acetone. After 8 h of stirring with a magnetic stirrer, the solution was cast in a glass Petri dish, and the final film was obtained after 48 h.

At different weight ratios of 1, 1.5, 2, 2.5, and 3 wt%, the micro-TiO₂ or nano-TiO₂ solution was added to CA powder. The solution was cast on a glass Petri dish and permitted to dry for 48 h after being agitated until it became homogenous. Figure 1 depicts the preparation process.

Figure 1

Schematic diagram of the preparation process for films.

3 Characterization

The morphologies of the composite surface and powder were examined with field-emission scanning electron microscopy ([FESEM] Zeiss Sigma 300-HV, Germany). The mechanical characteristics of CA and composite thick films were measured by tensile tests using a universal testing machine (UTM) UE3450 from Laryee Technology Co., Ltd., China. The films were cut to 12 mm × 60 mm, and thickness was measured by a digital micrometer with ±1 μm accuracy. All of the tests were carried out at room temperature (about 27°C), with a cross-head speed of 5 mm/min being utilized to measure the cellulose-based films and a stress–strain curve being produced. A well-known standard procedure was used to determine Young’s modulus, elongation at break, and ultimate tensile strength.

Fourier-transform infrared (FTIR) spectra were obtained by a Japan-made SHIMADZU-8400S FTIR spectrometer. The spectra were obtained in the wavenumber range of 400–4,000 cm⁻¹, at 4 cm⁻¹ resolution. The samples were prepared as tablets by mixing with KBr powder.

UV-vis spectra were obtained by Japan-made Shimadzu spectrometer. The wavenumber range of 200–1,100 Nm was utilized to obtain the spectra.

An X-ray diffractometer (BRUKER, D8 advance, USA) with Cu kα radiation operates at 40 kV/30 mA.

The optical system used to measure contact angles was from Holmarc Opto-Mechatronics Pvt. Ltd., India, with an automated dispenser and software for static and dynamic contact angle measurements. When a drop of water is dropped on the film’s surface, it spreads due to interactions between the solid surface and the water. The water contact angle will be measured to determine the surface’s wettability.

4 Results and discussion

4.1 SEM analysis

SEM micrographs and particle size distributions of micro- and nano-TiO₂ powders are shown in Figures 2 and 3, respectively. As clearly shown, the micro-TiO₂ powder covered a wide range of particle size from about 0.1 to 2 μm. The particles also have a regular crystalline morphology with smooth surfaces and sharp edges. On the other hand, nano-TiO₂ powder has a very fine particle size with a narrow distribution of about 20–80 Nm. Fine particles have a high degree of agglomeration due to their high surface area, so a more sophisticated dispersion technique will be required to prevent agglomeration and achieve a higher homogeneity of the particle distribution within the CA matrix.

Figure 2

SEM images of (a) micro-TiO₂ and (b) nano-TiO₂.

Figure 3

Particle size distribution of (a) micro-TiO₂ and (b) nano-TiO₂.

4.2 Tensile test

The mechanical properties of polymer systems depend on the intermolecular force, stiffness, and molecular symmetry of polymer systems [24]. Figure 4 shows the stress–strain curves for TiO₂/CA composite films with different weight ratios (1, 1.5, 2, 2.5, and 3 wt%) of micro-TiO₂ and nano-TiO₂. The good distribution of inorganic fillers in the (CA) polymer matrix was responsible for improving mechanical properties by up to 1 wt% for micro-TiO₂/CA and up to 2 wt% for nano-TiO₂/CA [25,26,27]. Polymers with a high degree of crystallinity, crosslinking, or rigid chains had a high strength or limited extendibility, resulting in a high yield modulus, a high stress at peak value, and a low elongation value. Due to the electrostatic interactions between the ester atoms of one chain and the hydroxyl atoms of another, CA becomes a rigid, strong material that exhibits dipole–dipole attraction. The dipole–dipole attraction, which reaches its maximum magnitude, was associated with improved mechanical characteristics. The increase in strength can be attributed to a greater capacity of the filler to attach to the matrix, which resulted in less sliding between the composite layers when stress was applied [28,29].

Figure 4

Stress–strain curve of (a) micro- and (b) nano-TiO₂-filled CA films.

The tensile strength reduced due to some degrees of agglomeration of filler particles above the critical content and an increase in inhomogeneity [25,26]. The lack of interfacial adhesion between the polymer and the fillers was responsible for the decrease in tensile strength [29].

As seen from Figures 5–7, the tensile strength after incorporation of (nano-TiO₂) was higher than that after incorporation of (micro-TiO₂), which was attributed to a difference in the reinforcing or strengthening mechanism. The term “micro” refers to the fact that the particle–matrix interaction is too small to be treated at the atomic or molecular level. Most of these composites have a harder and stiffer particulate phase than the matrix. The reinforcing particles tend to retain the mobility of the matrix phase in the vicinity of these reinforcing particles. In essence, the matrix transfers a portion of applied stress to the particles that are only carrying a part of the load. The particle sizes are within a range of 10–100 nm. At an atomic or molecular level, the matrix interaction is strengthened. The matrix bears the majority of the applied load, but the small dispersion particles hinder or impede dislocation movement. Plastic deformation is reduced, resulting in an enhanced yield and tensile strength [30]. Both tensile strength and elongation were improved at the fixed levels of 1 wt% (micro-TiO₂) and 2 wt% (nano-TiO₂) loadings, as shown in Figures 4 and 5. However, above that level of loading, the tensile strength and elongation decreased.

Figure 5

Ultimate tensile strength of CA films with different TiO₂ contents.

Figure 6

Elongation of micro- and nano-TiO₂-filled CA films.

Figure 7

Young’s modulus of micro- and nano-TiO₂-filled CA films.

The general behavior of Young’s modulus was found to depend on the elongation and ultimate strength according to the filler contents and the homogeneity of particle distribution within the CA matrix. This result agrees with those of Rajeswari et al. [31].

4.3 Membrane morphology

Figure 8 shows the FESEM images of CA, CA-1 wt% micro-TiO₂, and CA-2 wt% nano-TiO₂ films. The film of CA is obtained as a rough pattern with a homogeneity surface [32]. At 1 wt% micro-TiO₂, the existence of a small bright region has been observed in the film with an indication of particle agglomeration on the surface. Hence, the mechanical properties of the composites decrease because of these agglomerated particles [33]. There were no aggregation regions in the CA matrix where nanoparticles were dispersed. This could be due to the efficiency of nanoparticle dispersion in the CA matrix, which would explain the improvement in the films’ tensile properties [34,35]. This result agrees with that of Gao et al. [36].

Figure 8

FESEM images: (a) CA, (b) CA + 1 wt% micro-TiO₂, and (c) CA + 2 wt% nano-TiO₂.

4.4 FTIR spectroscopy

Figures 9 and 10 show the FTIR spectra of pure CA films and CA films containing 1, 1.5, 2, 2.5, and 3 wt% micro-TiO₂ and nano-TiO₂, respectively. The film spectrum is characterized by the presence of bands at 1,741 cm⁻¹ (steric carbonyl stretching), 3,478 cm⁻¹ (cellulose OH stretching), and 2,936 cm⁻¹ (CH stretching) [37]. The bands at 2,936 cm⁻¹ (CH stretching), 3,478 cm⁻¹ (OH stretching), 1,741 cm⁻¹ (steric carbonyl stretching), 1,232 cm⁻¹, and 1,045 cm⁻¹ (C–O stretching), all increased when micro-TiO₂ or nano-TiO₂ was added. Inserting TiO₂ into CA may have strengthened the interactions between two compounds at the region of the band that exhibited these properties since the chemical structure of TiO₂ is an oxide with O–Ti–O bonding. TiO₂ bonding is represented by peaks at 400–600 cm⁻¹ and 750 cm⁻¹ [38,39]. Carbanion and hydroxyl groups have peaks centered at 1,750 and 3,478 cm⁻¹, respectively [38]. This result agrees with that of Prakash et al. [40].

Figure 9

FTIR spectra of micro-TiO₂-based CA.

Figure 10

FTIR spectra of nano-TiO₂-based CA.

4.5 UV-vis spectroscopy

UV-vis spectroscopy gives useful information on the reflectance, absorbance, and transmittance of polymeric materials [41]. It is well known that CAs are very important polymers because they have excellent optical properties, such as great translucency [42]. Figures 11 and 12 depict the UV-vis Transmittance spectra of pure CA film and CA films containing 1, 1.5, 2, 2.5, and 3 wt% micro-TiO₂ and nano-TiO₂, respectively. The transmittance spectra of pure CA were almost transparent in all regions. CA-micro-TiO₂ films were less transparent than pure CA, while CA-nano-TiO₂ films could efficiently block the lights. This could be attributed to the difference between micro- and nano-TiO₂ particles, since particle–matrix interactions that lead to strengthening occur at an atomic or molecular level for small particles but not for large particles [30]. Hence, UV-vis spectra revealed that the transmittance was mostly in the visible region, with a small UV wavelength range. This result agrees with that of Sharma et al., who studied the optical properties of CA and CA-based lignocelluosic nanofiber. On CA films and with lower lignin concentration, there was an enhancement in transmittance [43].

Figure 11

UV-vis spectroscopy of micro-TiO₂-based CA.

Figure 12

UV-vis spectroscopy of nano-TiO₂-based CA.

4.6 X-ray diffraction (XRD)

Figures 13 and 14 show the X-ray diffraction patterns of pure CA film and CA films containing 1, 1.5, 2, 2.5, and 3 wt% micro-TiO₂ and nano-TiO₂, respectively. The patterns of micro-TiO₂ and nano-TiO₂ were shown as 2θ = 25° anatase, matching with JCPDS card no. 21-1272, where these are characteristic crystalline peaks [44]. According to these results, it was indicated that TiO₂ is largely composed of anatase. Among the other types, anatase has excellent stability, antifouling properties, and hydrophilic nature, all of which are important filtration film characteristics. Furthermore, this can be used to alter films [45]. As seen in Figures 13 and 14, the wide peak observed below 2θ = 18.5° for the pure CA film corresponds to the semi-crystalline arrangement of the CA film [46]. The strong and sharp characteristic peaks in the composite film indicate the good crystallinity of the manufactured films. This result agrees with that of Das and Gebru [15].

Figure 13

XRD pattern of micro-TiO₂-based CA.

Figure 14

XRD pattern of nano-TiO₂-based CA.

4.7 Water contact angle

The hydrophilicity of the films is determined by measuring the water contact angle [47]. Water contact angles for CA are represented in Figure 15. CA-micro-TiO₂ and CA-nano-TiO₂ at different percentages of 1, 1.5, 2, 2.5, 3 wt% are represented in the figure. The CA film had the lowest surface wettability of all the produced films, with a contact angle of 61.3°, due to its hydrophilic nature, whereby low surface wettability leads to a high contact angle, and vice versa [48]. The contact angle of the CA-micro-TiO₂ and CA-nano-TiO₂ composite films reduced dramatically, from 53.2° to 29° and from 51.5° to 27°, respectively, due to the presence of the anatase phase of TiO₂, which was less hydrophilic than CA. The hydrophilicity of the prepared films has noticeably improved as the micro- and nanoparticle content increased. This result agrees with that of Neelapala et al., who found similar results [49].

Figure 15

Water contact angles for CA nanocomposite thick films with various TiO₂ contents.

5 Conclusion

CA–TiO₂ (micro and nano) composite films were prepared using the casting method in this investigation. The effects of micro- and nano-TiO₂ on the microstructure morphology of casted CA thick films were examined. FESEM images of CA, CA + 1 wt% micro-TiO₂, and CA + 2 wt% nano-TiO₂ revealed that both types of particles exhibit a high degree of particle dispersion homogeneity within the CA matrix. The addition of micro- or nano-TiO₂ increased the ultimate tensile strength and Young’s modulus up to 1 wt% for micro and 2 wt% for nanocomposite films but then slightly decreased along with increasing TiO₂ content, according to the tensile test results. FTIR spectra demonstrated the interaction between CA and micro- or nano-TiO₂. UV-vis transmittance spectra showed that pure CA was almost transparent, CA-micro-TiO₂ films were less transparent than pure CA, while CA-nano-TiO₂ films were dim. XRD diffraction for the composite films was performed. The patterns of micro-TiO₂ and nano-TiO₂ were presented as 2θ = 25° for anatase phase and 2θ = 18.5° for pure CA film, respectively. The addition of micro- or nano-TiO₂ from 1 to 3% of the total weight resulted in an increase in hydrophilicity. The prepared films could be used in filter applications due to their hydrophilicity.

Acknowledgment

The authors express their appreciation to Senior Researcher Ali J. Addie, Eng. Mukhallad H. Shwaish, Dr. Mohammed S. Ali, Dr. Mohammed S. Mohammed, Asst.Tech. Amani K. Hussein, Dr. Hanaa J. Kadhim for their help in examinations and our appreciation to all staff of the Journal.

Funding information: The authors state no funding involved.
Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.
Conflict of interest: There are no conflicts of interest declared by researchers.

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Received: 2021-10-28

Revised: 2022-03-11

Accepted: 2022-04-09

Published Online: 2022-05-26

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

Articles in the same Issue

https://doi.org/10.1515/jmbm-2022-0019

Keywords for this article

biodegradable; cellulose acetate; mechanical properties; nanocomposite; titanium oxide

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BY 4.0