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Vol. 9. Issue 1.
Pages 789-797 (January - February 2020)
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Vol. 9. Issue 1.
Pages 789-797 (January - February 2020)
Original Article
DOI: 10.1016/j.jmrt.2019.11.019
Open Access
Enhancement of optical and electrical properties of PVC/PMMA blend films doped with Li4Ti5O12 nanoparticles
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A.A. Al-Muntasera,b,
Corresponding author
almuntser2015@gmail.com

Corresponding author.
, A.M. Abdelghanyc,d, E.M. Abdelrazekb,e, A.G. Elshahawyb
a Physics Department, Faculty of Education-Arhab, Sana’a University, Sana’a, Yemen
b Physics Department, Faculty of Science, Mansoura University, Mansoura 35516, Egypt
c Spectroscopy Department, Physics Division, National Research Center, Dokki 12311, Cairo, Egypt
d Basic Science Department, Horus University, International Coastal Rd, New Damietta, Kafr Saad, Damietta Governorate, Egypt
e Physics Department, Faculty of Science at Al-Ula, Taibah University, Medina, Saudi Arabia
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Table 1. The calculated values of direct and indirect band gap for the prepared films.
Abstract

Nanocomposite films of polyvinyl chloride/polymethyl methacrylate (PVC/PMMA)/ lithium titanium oxide (Li4Ti5O12) were prepared through a casting method. The structural features of the prepared films were investigated using XRD, TEM, FTIR, SEM, and UV/Vis. spectroscopy techniques. XRD pattern reveals the formation of the crystalline phase of lithium titanium oxide of average crystallite size 40nm embedded in the amorphous polymeric matrix. The average crystallite size observed from TEM images is in good agreement with the XRD results. The physical interaction between the PVC/PMMA blend and Li4Ti5O12 NPs was confirmed by FTIR through the formation of a hydrogen bond. SEM micrographs showed partial compatibility between the polymer blend and the Li4Ti5O12 NPs. UV/Vis. analysis displayed that the values of the optical energy gap are decreased with increasing the concentration of Li4Ti5O12 NPs, this means that charge transfer complexes are arising between the polymer blend and Li-ions. The DC conductivity results are explained in the light of an intrachain one-dimensional interpolaron hopping model. The obtained results recommend the choice of Li4Ti5O12 NPs as dopants to enhance the electrical properties of virgin PVC/PMMA blend. Also, nanocomposite films can be employed in different electrochemical and industrial fields such as Li-ion batteries.

Keywords:
FTIR
XRD
PVC/PMMA
Li4Ti5O12NPs
DC conductivity
Full Text
1Introduction

Polymer research remains a growing field in which blends play an important role due to their relatively simple preparation and the diverse resulting properties [1]. The important advantages of polymer blending are versatility, simplicity, inexpensiveness, and the properties of the final product, which can be tailored to requirements of applications that cannot be achieved by a single polymer [2].

Polyvinyl chloride (PVC) is one of the most important and extensively used thermoplastics polymer owing to its many significant features such as low flammability, chemical resistance, and low cost [3]. PVC has disadvantages such as low thermal stability at processing temperatures, low impact strength and large melt viscosity [4]. This deficiency is overcome by adding plasticizers or processing aids in PVC. Especially, polymethyl methacrylate (PMMA) is used as processing aids for PVC [5]. The purpose of the PVC modification by blending is the production of new polymers that combine the desired physical properties at a low cost.

Li4Ti5O12 NPs is particularly attractive in electronic applications because it is cheaper, environmental friendliness [6], and has excellent lithium-ion mobility [7]. Also, the properties of Li4Ti5O12 are hardly expanded by the overcharge and high stability in cycles of discharging and charging [8]. These properties make it a good nanofiller to enhance the electrical and optical properties of polymers and polymer blends [9]. The incorporation of nanofiller within the polymeric matrix has gained significant research interest since it introduces new materials with improved optical and electrical properties. There are numerous applications of polymeric nanocomposites based on their electrical, mechanical, optical, and magnetic properties [10–12].

Morsi et al. [13] investigated the effect of Li4Ti5O12 NPs on the structural, optical, thermal and electrical properties of the PEO/CMC blend. FTIR results show the interaction between the PEO/CMC blend and Li4Ti5O12 NPs via the formation of a hydrogen bond. The decrease of the optical energy gap, Eg, for the nanocomposite samples compared to that of pure PEO/CMC blend and the determination of the type of electronic transitions were demonstrated by UV/Vis. absorption results. The influence of Li4Ti5O12 NPs on structural, optical, and thermal properties of PVDF/PEO blend was investigated by Abd El-Kader et al. [8]. Elashmawi et al. [9] studied the changes in spectroscopic, electrical, and thermal properties of the PVDF/PEO containing lithium nanoparticles using several analytical techniques. The results of FTIR, XRD, thermal, and SEM studies indicated that the addition of LiTi2O4 can reduce the degree of crystallinity due to suppression of recognition of polymeric chains by LiTi2O4 nanopowders. Abdelrazek et al. [14] prepared samples of different mass fractions (PMMA/PVC) and their physical properties were studied by ordinary FTIR, XRD, UV/Vis., and SEM with a different glimpse. A new route for inquest the degree of miscibility was introduced depending on a spectroscopic quantitative measurement. All results suggested that the ratio (70/30wt.%) of PVC/PMMA blends was preferred to be used in some practical applications to add appropriate dopant on it. To the best of our knowledge, the embedded of Li4Ti5O12 NPs within PVC/PMMA polymer matrix has never been reported.

Presented work aims to study the structural role of Li4Ti5O12 NPs dopant level on the optical, and electrical characteristics of the PVC/PMMA/Li4Ti5O12 polymer nanocomposite for possible use in lithium-ion batteries.

2Materials and methods2.1Materials

High molecular weight poly(vinyl chloride) (PVC), (Fluka, Romania), and polymethyl methacrylate (PMMA) with molecular weight MW=25,000gm/mol, (Poly Science, Warrington, PA), were used as the basic polymeric materials. Lithium titanium oxide (Li4Ti5O12) nanopowder with particle size <100nm is the other basic material was used as a dopant and supplied by Sigma-Aldrich (USA). Tetrahydrofuran (THF) with purity 99.5 % from (Central Drug House, New Delhi, INDIA) was used as a solvent.

2.2Preparation of PVC/PMMA/ Li4Ti5O12 nanocomposite films

Nanocomposite films were prepared by ordinary casting methods as follows: first, both PVC and PMMA were dissolved separately in THF for 2h at room temperature until a homogeneous solution was obtained for each polymer. Second, the two polymers were added together for 2h to obtain (PVC/PMMA) blend with weight percentage (70/30wt.%). Third, the required masses (0.1, 0.2, 0.4, and 0.8wt.%) of Li4Ti5O12 NPs were loaded within the solution of PVC/PMMA under stirring for 2h at room temperature to inhibit any agglomerations. Fourth, probe sonicator model Q500-Sonicator, USA, was placed in the mixture until the completely dispersion of Li4Ti5O12 NPs with polymer blend mixture occurs. Finally, the resulting solution with suitable viscosity was cast to a glass dish and kept at room temperature for 2 days to remove any solvent traces. The prepared films were peeled from Petri dishes and kept in a vacuum desiccator until use. The thickness of the obtained films was in the range of 0.04–0.10mm.

2.3Characterization methods

FTIR absorption spectra were carried out for different films using the single beam spectrometer Nicolet iS10, USA. The X-ray pattern was recorded on PANalytical X’Pert Pro XRD system using Cu-Kα radiation (where, λ=1.540Å). The tube operated at 30kV, scans were collected over a 2θ range of 5°–80°. UV–vis absorption spectra were measured in the wavelength range of 200−900nm using a JASCO 630 spectrophotometer, USA. Morphology of prepared films was investigated by using a scanning electron microscope (SEM) model JSM-6510LV JEOL, USA, at 20kV accelerating voltage, magnification 500×. To determine the size, shape, and distribution of the Li4Ti5O12 NPs, transmission electron microscope (TEM) model JEM-2100 JEOL, Japan, was used. DC electrical conductivity was measured using auto-ranging multi-meter KETHLEY 6517B, USA, with an accuracy of ± 0.5 %.

3Results3.1XRD analysis

Fig. 1 depicts the XRD spectrum of Li4Ti5O12 NPs. The peak position and Miller indices (h k l) to each peak of Li4Ti5O12 NPs were estimated. Seven sharp diffraction peaks can be seen at 2θ values of 18.24, 35.57, 43.24, 47.36, 57.21, 62.83, and 66.07° which correspond to the (111), (311), (400), (331), (551), (440) and (531), respectively, reveal the crystalline behavior of Li4Ti5O12 NPs. This is consistent with the values in the standard card (JCPDS file No. 49-0207). The crystallite sizes of Li4Ti5O12 NPs are evaluated by using the Scherrer equation [15,16]:

Fig. 1.

XRD spectrum of Li4Ti5O12 NPs.

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The calculated average size of Li4Ti5O12 NPs is 40nm. Fig. 2 depicts the XRD spectra of virgin PVC, virgin PMMA, virgin blend, and the blend doped with different concentrations of Li4Ti5O12 NPs. The XRD pattern of virgin PVC film shows the broad peak from 2θ=17.38–26.02° denotes the amorphous behavior of PVC [14]. While the characteristic peaks of the virgin PMMA film are observed at 2θ=16.09° with a large hump at 2θ=28.91° due to its amorphous nature [17]. The XRD peaks of the virgin blend are shifted as compared to that of virgin polymers owing to the change in the crystallographic organization. XRD peaks of the nanocomposite samples become broader and intensity is reduced upon the addition of Li4Ti5O12 NPs. This significant disorder induces a more flexible polymer backbone and thus enhancing ionic transportation, which is useful for lithium batteries [9]. In doped films with 0.1 and 0.2wt.%, the main peaks of Li4Ti5O12 NPs have disappeared owing to the small amount of Li4Ti5O12 NPs. For the film with a concentration of ≥ 0.4wt.%, new peaks were observed and attributed to Li4Ti5O12 NPs. Also, their intensities increase with increasing Li4Ti5O12 NPs content in the blend sample.

Fig. 2.

XRD of virgin PVC, virgin PMMA, virgin blend, and the blend doped with different concentrations of Li4Ti5O12 NPs.

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3.2Morphological properties

Fig. 3(a,b) illustrate the TEM micrograph for the Li4Ti5O12 NPs and its histogram, respectively. The TEM image shows a nearly cubic-shaped of Li4Ti5O12 NPs. The particle size is in the range of 30−60nm as observed from the histogram. Fig. 3c shows the electron diffraction pattern of Li4Ti5O12 NPs. It can be observed that the Li4Ti5O12 NPs have a polycrystalline phase. These results are in good agreement with XRD findings.

Fig. 3.

(a) TEM micrograph for the Li4Ti5O12 NPs, (b) particle size histogram of Li4Ti5O12 NPs, and (c) electron diffraction pattern of Li4Ti5O12 NPs.

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SEM image can only provide the surface morphology of the sample without giving a fair judgment of the internal structure or phase separation. It just gives an initial indication for the homogeneity or saturation processes. To understand the phase morphology and the effect of Li4Ti5O12 NPs incorporation within the PVC/PMMA polymer metrics, the surface morphology of the prepared films was investigated by using SEM technique. Fig. 4a-g depicts the SEM micrograph of the surface of virgin blend and the blend doped with different concentrations of Li4Ti5O12 NPs. As shown in Fig. 4a, the virgin film has a better crater and pore surface distribution due to the evaporation of THF solvent during the preparation process [18]. As a result, the charge carriers can be transported easily and quickly without the presence of the blocking phase [19]. Fig. 4b-g illustrates the distribution of Li4Ti5O12 NPs inside the PVC/PMMA blend. It can be noticed that the pores are re-shape and disappearance owing to the presence of structural reorganizations after the incorporation of Li4Ti5O12 NPs inside the blend. This behavior is nearly similar to the literature [17–19]. Also, the small white spots are dispersed on the surface of the blend with some agglomerations. By increasing the Li4Ti5O12 NPs content the agglomerations are increased. In the case of Li4Ti5O12 NPs=0.8wt.%, Fig. 4e shows a high agglomeration of the Li4Ti5O12 NPs at the surface, which indicates a close state of saturation. These results are also correlated with XRD results.

Fig. 4.

SEM images of PVC/PMMA blend sample doped with: (a) 0.0, (b) 0.1, (c) 0.2, (d) 0.4, and (e) 0.8wt.% of Li4Ti5O12 nanoparticles.

(1.13MB).
3.3FTIR analysis

To establish the interactions between PVC/PMMA matrices and Li4Ti5O12 NPs, FTIR spectroscopy is a very important tool for this purpose. Fig. 5 illustrates the FTIR spectrum of Li4Ti5O12 NPs. It can be observed that the band at about 3435cm-1 is attributed to OH bending vibration mode [20], the band at 686cm-1 is due to Ti-O stretching vibration [20], and the shoulder at about 462cm−1 is assigned to the Li–O vibration [8]. Fig. 6 depicts the FTIR absorption spectra of virgin PVC, virgin PMMA, virgin blend, and the blend doped with different concentrations of Li4Ti5O12 NPs. The bands of the virgin films are assigned and interpreted in light of the literature [21–24]. FTIR spectrum of the virgin PVC illustrates −CH asymmetric stretching vibrational mode can be observed at 2951cm-1. The band at 1430cm−1 is attributed to the wagging of methylene groups in PVC. The bands at 1329cm−1, 1249cm−1, 1065cm−1, and 959cm−1 represent the −CH2 deformation, C–H rocking and CC bonds, and trans C–H wagging group of PVC. The bands at 691cm−1 and 630cm−1 are attributed to the C–Cl stretching and cis C–H wagging vibrations. The FTIR spectrum of virgin PMMA shows the bands at 2994cm−1 and 2948cm−1 may be due to the stretching of −CH3 and −CH2– groups of PMMA. The bands at 1732cm−1, 1444cm−1, 1161cm−1, and 1264cm−1 may be attributed to the CO stretching, CH3 stretching, absorption of −OCH3, and COC stretching vibration mods of PMMA. Spectra of the films after adding Li4Ti5O12 NPs have some changes in band intensities and band positions (shift) as compared to that of the pure blend. This indicates the considerable interaction between the blend and Li4Ti5O12 NPs takes place. Also, the C-Cl stretching mode at 686cm−1 for the pure blend indicates a decreasing in intensity with increasing amount of dopant. This implies that there is an interaction between Cl in the PVC with Li+ ion from the Li4Ti5O12 NPs as shown in the Scheme 1. The band at 1161cm−1 due to OCH3 in the virgin blend is shifted to 1148cm−1. The band at 1721cm−1 due to CO is shifted to 1732cm−1. These shifts are expected to be due to the interaction between Li+ ion and the oxygen atoms in PMMA (Scheme 1).

Fig. 5.

FTIR spectrum of Li4Ti5O12 NPs.

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Fig. 6.

FTIR absorption spectra for virgin PVC, virgin PMMA, virgin blend, and the blend doped with different concentrations of Li4Ti5O12 NPs.

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Scheme 1.

Possible mechanism of hydrogen bond formation between PVC/PMMA polymer blend and Li4Ti5O12 NPs.

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3.4UV/Vis analysis

Fig. 7 depicts the UV/vis. absorption spectra of the prepared virgin blend and blend/Li4Ti5O12 NPs in the wavelength range 190−800nm at room temperature. The observed spectrum of virgin blend film has two absorption bands at 208nm, which is mainly assigned as n→π*. While the absorption band (shoulder) is observed at 278nm, indicating the presence of unsaturated bonds of the type CO, confirmed at about 1732cm-1 and assigned to π–π* transition [25,26], which is responsible for electrical conduction in the films. The main absorption band around 208nm and the band at about 278nm for all curves were shifted towards longer wavelengths with increasing Li4Ti5O12 NPs content. This may be attributed to the complexation between the dopants and the polymer blend and the change in crystallinity [27].

Fig. 7.

UV/vis. absorption spectra of prepared blend before and after doping with different mass fractions of Li4Ti5O12 NPs.

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The investigation of optical absorption provides information about the band structure of the organic materials. The process of light absorption occurs only when an electron moves from a lower to higher energy state through the absorption of specified energy in the form of photons. The types of possible electronic transitions can be determined by the changes in the absorbed radiation. A sudden change in the fundamental absorption can be defined as an absorption edge. The absorption is expressed in terms of an absorption coefficient (α) that represent the relative rate of decrease in light intensity given by:

where (A) is the value of absorbance and (d) is the thickness of the sample [28]. The absorption coefficient of amorphous materials can be related to the energy of the incident photon as follows [29–31]:
where Eg is the optical energy gap, C is the band tailing parameter and r=2 for indirect electronic transition and r=1/2 for direct electronic transition in the k space.

Fig. 8 illustrates αhν2 versus (hν) for virgin film and the film doped with Li4Ti5O12 NPs. By the extrapolated linear part of the plot of αhν2 and αhν1/2 versus photon energy to hν=0, the values of the direct and indirect band gaps are determined. The obtained values of direct and indirect band gap for the prepared films are listed in Table 1. It is showed that the direct and indirect band gap values are decreased after the incorporation of Li4Ti5O12 NPs as compared to that of the virgin blend. This can be explained in light of the charge transfer complexes (CTC) occurring between Li4Ti5O12 NPs dopant and the PVC/PMMA blend and may be due to the formation of defects in the polymeric chain resulting in the localized states in the energy gap [8,32]. These localized states overlaps and broadens with increasing the Li4Ti5O12 NPs content [13]. Hence, the degree of disorder of the virgin polymer increases by doping with Li4Ti5O12 NPs. This result is in good agreement with the XRD analysis result.

Fig. 8.

Variation between the calculated values of (a) indirect and (b) direct band gap versus the Li4Ti5O12 NPs content.

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Table 1.

The calculated values of direct and indirect band gap for the prepared films.

Li4Ti5O12 NPs wt.%Eg indirect (eV)Eg direct (eV)
Eg1(eV)  Eg2(eV)  Eg1(eV)  Eg2(eV) 
0.0  3.53  4.60  5.18  4.20 
0.1  3.36  4.13  4.98  4.08 
0.2  2.95  3.95  4.96  3.99 
0.4  2.41  3.81  4.90  3.80 
0.8  1.84  3.38  4.81  3.69 
3.5DC conductivity

The values of DC conductivity were obtained from the following equation:

where L is the thickness of the sample, R is the resistance, which directly measured as a relation with an increase of temperature, and A is the surface area. Fig. 9 illustrates the plot of log (σDC) versus (1000/T) of the virgin blend and blend/Li4Ti5O12 NPs. It can be observed that the values of σDC are gradually increased with increasing the temperature for all films and the behavior of conductivity does not display any peaks with increasing temperature. The estimated values of conductivity are changed from 1.68×10−11S/cm of the virgin film to 6.29×10−9S/cm of the doped films at room temperature and at a higher temperature from 1.54×10−10S/cm of the virgin film to 2.39×10−7S/cm of the doped films. These results suggest that the Li4Ti5O12 NPs is a good filler to enhance the electrical conductivity of PVC/PMMA films. This enhancement in the conductivity is interpreted based on the free volume theory [33], where this improvement can be attributed to the thermal movement of polymeric chains and the dopants dissociation as a result of the temperature effect. Further, the movement of segments in the polymer chain either provides a pathway for the Li-ions to move easily in amorphous regions and/or permits the Li-ions to hop from one site to another. As shown in Fig. 9, the dependence of σDC on the reciprocal of the temperature for all the prepared films follows the Arrhenius equation given by [34]:
where σo is the pre-exponential factor, ΔEa is the activation energy, kβ is the Boltzmann constant and T is the absolute temperature. From the estimated values of the slope and the intercept of the straight lines in Fig. 9, the activation energy (Δ Ea) and pre-exponential factor (σo) can be determined. Fig. 10 shows the variation of pre-exponential factor and activation energy versus Li4Ti5O12 NPs with the content of Li4Ti5O12 NPs. It can be seen that the Δ Ea values are decreased while σo values are increased with increasing Li4Ti5O12 NPs content. This indicated that higher ionic conductivity is due to the amorphous region in the polymer matrix. Besides, the adding of Li4Ti5O12 NPs disrupts the interaction between the Li + and the polymer backbone. Consequently, less energy is required to reform and break the coordination bond in the polymer matrix. As a result, ion diffusion is favorable during the hopping process [18].

Fig. 9.

Plot of log (σDC) versus reciprocal absolute temperature (1000/T) of the virgin blend and blend/Li4Ti5O12 NPs.

(0.12MB).
Fig. 10.

Variation of pre-exponential factor and activation energy versus Li4Ti5O12 NPs.

(0.11MB).

Furthermore, the presence of double-bond segments (detected by FTIR analysis) in the present system are considered as suitable sites for polarons and/or bipolarons creation in the polymeric nanocomposite. The modified interpolaron hopping model of Kuivalainen et al. [35] is used to explain the present conductivity results as follows:

where, A= 0.45, B= 1.39,  R∘ is the typical separation between impurities, yp and ybp are the polarons and bipolarons concentration [36], respectively, ζ=ζ∥ζ⊥213 is the average decay length of a polaron and bipolaron wave function, ζ∥ is the decay lengths parallel and ζ⊥ is the decay lengths perpendicular to the polymer chain, respectively. Bredas et al. [37] explained that polarons and bipolarons induce defects of the same extension. The rate of electronic transition between the states of polaron and bipolaron is given by [37]:
where n is a constant ≈ 11. The order of magnitude of σ for the prepared films was determined by using a computer-based program and adjusted with a fitting parameter. The estimated parameters of ζ and ζ are found to be 1.06 and 0.22nm, respectively. This result depends on the interchain distance and the interchain resonance energy [38]. By using Eq. (6) and (7), the values of the hopping distance (Ro) are calculated. Fig. 11 illustrates the variation of Ro versus Li4Ti5O12 NPs content at various temperatures. It can be observed that the Ro is linearly decreased with increasing the temperatures for the various concentrations of Li4Ti5O12 NPs. This evidences the concentration of thermally activated polarons and/or bipolarons (act as hopping sites for the charge carriers) increase with increasing the temperature. The estimated values of Rₒ are in the range of 1.4–5.6nm for the virgin film and the doped film with 0.8wt.% at a higher temperature. Considering the length of the monomer unit is 0.25nm [39], the evaluated average hopping distance between two sites is in the range of 5.6–22.40 times the monomer unit lengths. This suggests that the intrachain one-dimensional hopping conduction mechanism takes place [40] and indicates the choice of Li4Ti5O12 NPs as dopants to enhance the electrical conductivity of PVC/PMMA films.

Fig. 11.

Variation of Ro versus Li4Ti5O12 NPs content at various temperatures.

(0.13MB).
4Conclusion

PVC/PMMA films doped with Li4Ti5O12 were prepared by ordinary casting technique. The prepared films were examined by using different techniques such as XRD, TEM, FTIR, SEM, and UV/Vis. spectroscopy. TEM images of Li4Ti5O12 NPs illustrate nano size with an average of 40nm, cubic shape, and non-monodispersed. FTIR indicated the good complexation between the PVC/PMMA blend and Li4Ti5O12 NPs. XRD results showed that the addition of Li4Ti5O12 NPs can reduce the degree of crystallinity for the doped films. Optical measurements indicated the presence of a well-defined π→ π* transition, which comes from unsaturated bonds, CO, and the optical band gap is decreased with increasing the Li4Ti5O12 NPs content. Moreover, it has been observed that charge transfer complexes are arising inside the prepared films. DC electrical conductivity depends on temperature as well as Li4Ti5O12 NPs dopants. The enhancement of DC conductivity was ascribed to an increase in the amorphous nature of polymer blend as well as the increasing of the mobile charge carriers of Li4Ti5O12 NPs. The obtained values of the energy gap and DC conductivity suggest that the prepared films with a high content of Li4Ti5O12 NPs can be used in lithium-ion battery and electronic devices.

Conflicts of interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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