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. 2023 Sep 25;8(40):37090–37097. doi: 10.1021/acsomega.3c04538

Dielectric and Mechanical Properties of PDMS–La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) Nanocomposites

Suryakanta Nayak †,§,∥,⊥,*, Banalata Sahoo ‡,#, Tapan Kumar Rout ⊥, Amar Nath Bhagat ⊥
PMCID: PMC10569002  PMID: 37841148

Abstract

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Flexible polydimethylsiloxane–La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) [PDMS–LBT] nanocomposites with high permittivity (dielectric constant, k) are prepared through a room-temperature mixing process. The LBT nanoparticles used in this study are prepared through a high-temperature solid-state reaction. It is observed that LBT (X = Mg/Ca) nanoparticles are spherical in nature, with particle size ∼20 nm, as observed from the HRTEM images, whereas LBT (X = Sr) nanoparticles are cubical in nature with particle size ≥100 nm. These LBT (X = Mg/Ca/Sr) nanoparticles are crystalline in nature, as apparent from the XRD analysis and SAED patterns. The permittivity of LBT nanoparticles is higher when “Ca” is present in place of “X”. These three oxides show a temperature-dependent dielectric behavior, where LBT nanoparticles with “Sr” show a sharp change in permittivity at a temperature of ∼105 °C. These kinds of oxide materials, especially LBT (X = Sr) nanoparticles/oxides, can be used in dielectric/resistive switching devices. The effect of LBT nanoparticle concentration on the dielectric and mechanical properties of PDMS–LBT nanocomposites is widely studied and found that there is a significant increase in dielectric constant with an increase in the concentration of LBT nanoparticles. There is a decrease in the volume resistivity with the increase in the LBT nanoparticle concentration. All the PDMS–LBT nanocomposites have low dielectric loss (ε″) compared to the dielectric constant value. It is found that both permittivity (ε′) and AC conductivity (σac) of PDMS–LBT composites are increased with the temperature at a frequency of 1 Hz. The % elongation at break (% EB) and tensile strength (TS) decrease with the LBT nanoparticle concentration in the matrix PDMS, which is due to the non-reinforcing behavior of LBT nanoparticles. The distribution and dispersion of LBT nanoparticles in the matrix PDMS are observed through HRTEM and AFM/SPM.

1. Introduction

Polymer composites (particle-reinforced polymer) have shown great interest because the addition of filler particles to a matrix polymer can enhance the electrical, thermal, mechanical, barrier, and other various properties.1−3,4,5,6,7 These composites may contain oxide/inorganic particles, nanofibers, nanoclays, carbon powder/fillers, carbon nanotubes, or graphene dispersed in appropriate matrix polymers.1,3,8−10,11,12,13,14,15,16 Polymer composites have different applications in the field of electronic materials such as photovoltaic devices, capacitors, actuators, electromagnetic interference (EMI) shielding, static charge dissipation, angular acceleration accelerometers, acoustic emission sensors, electronic packaging materials, and integrated decoupling capacitors.1,3,8,13,17−19 There are many processing advantages of these polymer composite materials, which include mechanical flexibility and can be molded into various complex shapes/geometries. Therefore, polymers/polymer composite materials can be used in compact electronics.17,20

In the past decades, polymer–ceramic composites/nanocomposites have been of great interest to researchers for their novel applications. There are various ceramic oxides/particles which have been used by different research groups in making polymer composites for various applications.21−23,24,25,26 However, there is an increase in demand for electroceramic oxide fillers in making polymer composites due to their various electrical properties.27−29,30,31,32 Technically, these special classes of ceramic oxides have been explored for their ferroelectric, piezoelectric, and dielectric responses and have been used in nonvolatile memories [dynamic random access memories (DRAMs)], high-capacity dielectric devices, and materials for energy storage and conversion.33−35 The incorporation of these electroceramic fillers in the matrix polymer has become a common practice to improve the electrical, mechanical, and other properties. These polymer–ceramic composites/nanocomposites can be effectively used as flexible electronic and electrical materials.36

There is no literature based on PDMS nanocomposites using LBT (X = Ca, Mg, and Sr) as electroceramic fillers. There are only two reports based on Ln2Ba2CaZn2Ti3O14 (Ln = La and Pr) and Nd2Ba2CaZn2Ti3O14.4 ceramic oxides.37,38 In the present study, we have prepared similar oxides by varying the reactant at the position of “Ca” and “Ln/Nd” by “Mg/Ca/Sr” and “La”, respectively. We have prepared LBT (X = Mg, Ca, or Sr) electroceramic oxides (nanoparticles) using three different reactants such as CaCO3, MgO, and SrCl2·6H2O along with La2O3, BaCO3, ZnO, and TiO2. The present paper describes the preparation of LBT (X = Mg/Ca/Sr) nanoparticles through a high-temperature solid-state reaction using stoichiometric amounts of La2O3, BaCO3, CaCO3, MgO, SrCl2·6H2O, ZnO, and TiO2. The shapes of different LBT (X = Mg/Ca/Sr) nanoparticles are studied by HRTEM. Both room-temperature and temperature-dependent dielectric properties are discussed in detail. The crystal structures of these nanoparticles are determined through X-ray diffraction analysis. This paper also describes the preparation of nanocomposites using polydimethylsiloxane (PDMS) elastomer as the base matrix and the prepared LBT (X = Mg/Ca/Sr) particles as fillers. The mechanical and dielectric properties of these nanocomposites are studied as a function of filler concentration and frequency. The temperature-dependent dielectric properties are studied at a frequency of 1 Hz. The distribution and dispersion of LBT (X = Mg/Ca/Sr) nanoparticles in the PDMS matrix are studied by atomic force microscopy (AFM)/scanning probe microscopy (SPM) and HRTEM.

2. Experimental Section

2.1. Materials

The base matrix [polydimethylsiloxane (PDMS) elastomer) used in the present study was procured from D J Silicone. The density and shore-A hardness of the PDMS elastomer were 1.12 g/cm3 and 40 ± 3, respectively. Dicumyl peroxide (DCP; purity = 98%, MP = 80 °C, Sigma-Aldrich Chemical Company, USA) was used as the curing agent. TiO2, BaCO3, CaCO3, MgO, SrCl2·6H2O, and ZnO were procured from Merck, India, whereas La2O3 was procured from Alfa Aesar.

2.2. Preparation of La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) Nanoparticles

La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) [LBT (X = Mg/Ca/Sr)] nanoparticles are prepared through a high-temperature solid-state reaction using stoichiometric amounts of BaCO3, TiO2, CaCO3, MgO, SrCl2·6H2O, ZnO, and La2O3. These ingredients were dried at 150 °C for 6 h to remove the adsorbed moisture, and these dried oxides/hydroxides were thoroughly mixed in an agate mortar and loaded in an alumina boat/crucible. The mixture was heat-treated in a muffle furnace at 700 °C for 6 h and 1000 °C for 6 h, followed by heating at 1200 °C (twice) for 6 and 2 h, respectively, with three intermittent grindings. The powder obtained was grinded thoroughly using an agate mortar before further study.

2.3. Preparation of PDMS–La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) (PDMS–LBT) Nanocomposites

PDMS–LBT (X = Mg/Ca/Sr) nanocomposites are prepared through a room-temperature mixing process, where LBT (X = Mg/Ca/Sr) nanoparticles and other ingredients are mixed with the PDMS matrix in an internal mixer with a shear rate of 45 rpm for a mixing time of 10 min. The LBT (X = Mg/Ca/Sr) nanoparticles and cross-linking agents are mixed with the pure matrix PDMS as per the formulations given in Table 1. Finally, these compounds were passed through a two-roll mill to make them into a sheet form. Composite designation: P100LBT10, where P = PDMS and LBT = La2Ba2XZn2Ti3O14 nanoparticles. The optimum cure times of different compounds were evaluated by a rubber process analyzer (RPA) operating at 150 °C. The different test specimens from all the composites were prepared using a compression molding press at 150 °C and cured up to an optimum curing time of 5 min.

Table 1. Formulations of PDMS–La2Ba2XZn2Ti3O14 (PDMS–LBT) Nanocompositesa.

ingredients composition parts by weight per hundred parts of polymer (php)
P100LBT0 P100LBT10 P100LBT30 P100LBT50 P100LBT70
PDMS 100 100 100 100 100
LBT 0 10 30 50 70
DCP 1.5 1.5 1.5 1.5 1.5
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a

10 php = 9.09 wt %, 30 php = 23.08 wt %, 50 php= 33.34 wt %, and 70 php = 41.18 wt %.

3. Results and Discussion

3.1. Properties of La2Ba2XZn2Ti3O14 (X = (X = Mg/Ca/Sr)) Nanoparticles

3.1.1. X-ray Diffraction Analysis

The XRD patterns of three different types of LBT (X = Mg, Ca, or Sr) nanoparticles are shown in Figure 1. The XRD pattern of LBT nanoparticles (X = Ca) well matched with the reported literature, whereas the other two particles (X = Mg/Sr) showed similar XRD patterns.37 It is observed that in all cases impurity peaks are observed for LBT particles prepared at 1000 °C. However, these impurity peaks are absent in the case of particles prepared at 1200 °C. Therefore, it can be concluded that 1200 °C is the appropriate/optimum temperature for the preparation of LBT (X = Mg/Ca/Sr) nanoparticles.

Figure 1.

Figure 1

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XRD patterns of (A–C) La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) nanoparticles.

3.1.2. Dielectric Properties

Semilog plots of logf vs dielectric constant (ε′) and dielectric loss (ε″) against frequency are shown in Figure 2. The prepared LBT (X = Mg/Ca/Sr) nanoparticles have a high dielectric constant (permittivity) with a relatively low dielectric loss.

Figure 2.

Figure 2

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Variation of (a) dielectric constant and (b) dielectric loss against frequency for La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) nanoparticles.

There is also an increase in both dielectric constant and dielectric loss with the decrease in frequency. The high dielectric constant at the low-frequency region is due to the presence of space charges, which undergo orientation during polarization. The low dielectric loss of this material, especially at high frequency, makes it suitable for applications such as capacitors and other electronic devices. It is also observed that LBT nanoparticles with “Ca” has a high dielectric constant compared to the other two LBT nanoparticles with “Mg” and “Sr”.

Figure 3 shows the temperature-dependent dielectric behavior of LBT (X = Mg/Ca/Sr) nanoparticles at 1 kHz. It is observed that the dielectric constant of LBT (X = Mg/Ca/Sr) nanoparticles changed with the increase in temperature due to the phase transition. The three different nanoparticles/oxides behave in a different manner with the increase in temperature. There is a significant increase in the dielectric constant at ∼105 °C for LBT nanoparticles (X = Sr), which is the Curie temperature of this material. Similarly, the dielectric constant of LBT nanoparticles (X = Ca) is more in the temperature range of 80–100 °C, which we can consider as its Curie point. Finally, LBT nanoparticles (X = Mg) show a decrease in dielectric constant with the increase in temperature up to 120 °C, but beyond 120 °C, the dielectric constant again increases with the increase in temperature. It is also observed from the trend of the curve (Figure 3) that LBT nanoparticles (X = Mg) may have a high dielectric constant in the low-temperature range, so the Curie temperature of this material may be present at a low temperature. Due to the lack of measurement facility of the low-temperature dielectric study, the exact Curie temperature of LBT (X = Mg) particles could not be determined in the present work and is for future research scope (low-temperature dielectric study of these oxide materials). The above types of oxide materials, especially LBT (X = Sr) nanoparticles/oxides, can be used in dielectric/resistive switching devices.

Figure 3.

Figure 3

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Variation of the dielectric constant with temperature at 1 kHz for La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) nanoparticles.

3.1.3. High-Resolution Transmission Electron Microscopy

The shape and size of LBT (X = Mg/Ca/Sr) nanoparticles can be seen from the HRTEM images in Figure 4. LBT (X = Mg/Ca) nanoparticles are spherical in nature, where the size of particles is ∼20 nm, as clearly seen from the HRTEM images (Figure 4a,b). LBT (X = Sr) nanoparticles are cubical in nature, where the size of particles is ≥100 nm (Figure 4c). These LBT (X = Mg/Ca/Sr) nanoparticles are crystalline in nature, as is apparent from both the SAED (Figure 4d–f) and XRD (Figure 1A–C) patterns. From the SAED patterns, it is observed that LBT (X = Mg/Ca) nanoparticles are crystalline (mixture of single- and polycrystalline) in nature, whereas LBT (X = Sr) nanoparticles are single-crystalline in nature.

Figure 4.

Figure 4

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HRTEM images and SAED patterns of (a, d) LBT (X = Mg), (b, e) LBT (X = Ca), and (c, f) LBT (X = Sr) nanoparticles.

3.1.4. Field Emission Scanning Electron Microscopy

The presence of different elements (La, Ba, Mg, Ca, Sr, Zn, Ti, and O) in LBT (X = Mg/Ca/Sr) nanoparticles is confirmed through FESEM-EDS analysis (Figure 5). The concentration of each element in LBT nanoparticles is also understood from the FESEM-EDS data given in Table 2.

Figure 5.

Figure 5

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FESEM-EDS images of (a) LBT (X = Ca), (b) LBT (X = Mg), and (c) LBT (X = Sr) nanoparticles.

Table 2. SEM-EDX Data for La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) Nanoparticles.
La2Ba2CaZn2Ti3O14
 La2Ba2MgZn2Ti3O14
 La2Ba2SrZn2Ti3O14
element weight % atomic % element weight % atomic % element weight % atomic %
O 30.56 70.47 O 38.54 77.63 O 31.45 73.89
Ca 2.75 2.54 Mg 3.18 4.22 Sr 2.64 2.47
Ti 14.36 11.06 Ti 8.36 5.62 Ti 7.84 10.57
Zn 6.65 3.75 Zn 3.60 1.77 Zn 5.39 3.28
Ba 18.40 4.94 Ba 6.29 1.48 Ba 20.37 3.63
La 27.28 7.24 La 40.03 9.29 La 32.31 6.16
total 100.00   total 100.00   total 100.00  
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3.2. Properties of PDMS–La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) Nanocomposites

3.2.1. Electrical Properties

The DC resistivity of polymer composites depends on the resistivity of the matrix polymer as well as the particulate filler.39 The DC resistivity of composites containing three types of filler particles [LBT (X = Mg/Ca/Sr)] is presented in Figure 6. There is a gradual decrease in DC resistivity with an increase in the filler concentration, as observed from the figure. The steady decrease in the volume resistivity with the increase in filler concentration is due to the low resistivity of the LBT nanoparticles, as compared with the matrix PDMS. Moreover, inorganic oxide particles usually contain some amount of moisture; as a result, with the increase in the filler concentration, the DC resistivity of the composites is decreased. The presence of moisture on these filler surfaces helps in the ionization of ionic species in the composite system, which decreases the electrical resistivity of composites. It is also observed from the figure that composites with LBT (X = Ca) particles have low resistivity than the composites prepared from the other two fillers (LBT (X = Mg/Sr)).

Figure 6.

Figure 6

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Effect of the LBT (X = Mg/Ca/Sr) filler concentration on DC volume resistivity.

The variation of dielectric constant against frequency for both pure PDMS and PDMS–LBT (X = Mg/Ca/Sr) nanocomposites with two concentrations (9.09 and 41.18 wt %) has been presented in Figure 7. There is an increase in the dielectric constant with the decrease in frequency for composites containing three types of fillers. The high dielectric constant at the low-frequency region is due to the interfacial and dipolar polarization. The change in dielectric constant is also composition-dependent over the entire frequency range. As discussed above, LBT (X = Ca) nanoparticles have the highest dielectric constant value, whereas LBT (X = Mg) nanoparticles have the lowest value. We also have observed a similar trend in the case of composites prepared from these fillers. In the case of composites at a concentration (say 41.18 wt %) of the filler, the composite with LBT (X = Ca) nanoparticles has the highest dielectric constant and the composite with LBT (X = Mg) nanoparticles has the lowest value.

Figure 7.

Figure 7

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Semilog plot of dielectric constant (ε′) against frequency for different composites.

The effect of temperature on the frequency (1 kHz)-dependent AC conductivity and dielectric constant of composites (41.18 wt %) is shown in Figure 8. There is an increase in dielectric constant and conductivity with the increase in temperature, as observed from Figure 8. The increase in conductivity and dielectric constant of the composites with the increase in temperature is due to the increase in the net polarization. There is a change in trend in the case of composites prepared from LBT (X = Sr) nanoparticles and a sudden increase in dielectric constant/conductivity above 100 °C. This is due to the Curie temperature (∼105 °C) of LBT (X = Sr) nanoparticles, as observed in Figure 3.

Figure 8.

Figure 8

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Effect of temperature on (a) dielectric constant and (b) AC conductivity of composites at a frequency of 1 Hz.

3.2.2. Mechanical Properties

The variation of percent elongation at break (% EB) and tensile strength (TS) for different PDMS–LBT (X = Mg/Ca/Sr) nanocomposites against the filler concentration is presented in Figure 9a,b. The continuous decrease in both % EB and TS with the increase in LBT (X = Mg/Ca/Sr) nanoparticle concentration in the matrix PDMS indicates that these three types of filler particles are nonreinforcing in nature for the matrix PDMS.

Figure 9.

Figure 9

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Variation of (a) tensile strength, (b) % elongation at break, (c) hardness, and (d) tear strength against the filler concentration of different PDMS–La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) composites.

It is also observed that composites filled with LBT (X = Sr) particles have more TS and % EB as compared to the composites prepared from the other two filler particles (LBT (X = Mg/Ca)). The higher tensile strength and % EB in the case of composites filled with LBT (X = Sr) particles may be due to better polymer–filler interaction as compared to other composites. There is a continuous increase in hardness (Figure 9c) with the increase in the concentration of LBT (X = Mg/Ca/Sr) nanoparticles, which is due to the restricted movement of polymer chains. The decrease in tear strength with the increase in filler concentration is due to the increase in the number of particle clusters in the matrix polymer which generates a path for crack propagation (Figure 9d).

3.2.3. Morphological Analysis via HRTEM and AFM

The HRTEM images of nanocomposites containing 23.08 wt % of three different types of LBT (X = Mg/Ca/Sr) nanoparticles are presented in Figure 10a–c. The distribution of LBT nanoparticles is good in all the cases, whereas particle dispersion is better in the case of the composite containing LBT (X = Mg) nanoparticles than the composites containing LBT (X = Ca/Sr) nanoparticles. It is apparent from these figures that the shape of nanoparticles is spherical in nature, and the particle size is ∼20 nm.

Figure 10.

Figure 10

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HRTEM images of (a) PDMS + 23.08 wt % LBT (X = Mg), (b) PDMS + 23.08 wt % LBT (X = Ca), and (c) PDMS + 23.08 wt % LBT (X = Sr) composites.

The particle distribution and dispersion can be understood from the AFM images. Figure 11a,b represents the tapping mode 2D and 3D images of PDMS–LBT (X = Sr) nanocomposites containing 23.08 wt % of LBT (X = Sr) nanoparticles, and their corresponding height profiles are shown in Figure 11c,d. The height profile of the PDMS–LBT (X = Sr) nanocomposite confirms the thorough distribution of LBT (X = Sr) particles (positions 1, 2, and 3) in the matrix PDMS. The height profile of the nanocomposite along the line drawn on the picture is shown in Figure 11c. The presence of LBT (X = Sr) particles in different locations can be detected, e.g., particles with height ∼62 nm (position 1), particles with height ∼66 nm (position 2), and particles with height ∼53 nm (position 3).

Figure 11.

Figure 11

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AFM/SPM (a, c) 2D and (b) 3D images and (d) height profiling of PDMS–La2Ba2XZn2Ti3O14 (X = Sr) composites containing 23.08 wt % LBT (X = Sr) nanoparticles.

4. Summary and Conclusions

The formation of La2Ba2XZn2Ti3O14 (X = Mg/Ca/Sr) nanoparticles is confirmed through X-ray diffraction and SEM-EDS analysis. The shape of LBT (X = Sr) nanoparticles is cubical in shape, with size ≥100 nm, whereas the other two particles (LBT (X = Mg/Ca)) are spherical in shape with size ∼20 nm, as clearly seen from the HRTEM images. These nanoparticles are crystalline in nature, as confirmed through SAED analysis and X-ray diffraction. The dielectric constant of LBT (X = Ca) particles and composites containing LBT (X = Ca) particles are more than that of the other two particles (LBT (X = Mg/Sr)). The dielectric measurement reveals that the dielectric loss of these particles is less than the dielectric constant, especially at high-frequency regions. Different particles behave differently with the increase in temperature, and they have different Curie temperatures. These kinds of oxide materials, especially LBT (X = Sr) nanoparticles/oxides, can be used in dielectric/resistive switching devices. PDMS–LBT (X = Mg/Ca/Sr) nanocomposites show both composition- and frequency-dependent dielectric properties. The LBT (X = Mg/Ca/Sr) nanoparticles are nonreinforcing fillers for the matrix PDMS. The nanocomposites with LBT (X = Ca) nanoparticles have low resistivity (high conductivity) than the composites prepared from the other two fillers (LBT (X = Mg/Sr)).

Acknowledgments

The authors would like to thank Indian Institute of Technology Kharagpur, India, for providing research facility. The authors are also thankful to Prof. Panchanan Pramanik (Retd. from Department of Chemistry, IIT Kharagpur, India) for providing his high-temperature furnace facility.

Author Present Address

○ Department of Chemistry, Binayak Acharya Degree College, Berhampur, Odisha 760006, India

Author Contributions

∇ S.N. and B.S. contributed equally.

The authors declare no competing financial interest.

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