Abstract: In this study, nano-dispersed polymer gel electrolytes containing polymethylmethacrylate (PMMA), lithium perchlorate (LiClO4), diethyl carbonate (DEC), dimethylacetamide (DMA), and nano-sized fumed silica (SiO2) have been synthesized and characterized. The electrolytes showed high ionic conductivity for electrolytes with higher dielectric constant solvents. The polymer enhanced the ionic conductivity of liquid electrolytes having a lower dielectric constant solvent (DEC) at all PMMA concentrations than the electrolytes containing a high dielectric constant solvent (DMA). Further, with the addition of nano-sized fumed silica, the ionic conductivity showed a small increase along with an increase in the mechanical stability of the electrolytes. The viscosity behavior of the electrolytes was also discussed, and it was correlated with the results of the ionic conductivity test. Nano-dispersed polymer gel electrolytes exhibited high ionic conductivity (10-2 S/cm). Further, the conductivity showed only a small change (by a factor, not by an order) over the 25-100°C temperature range and did not vary with time, which is desirable for their use in practical applications.

Gum tragacanth (GT) based gel polymer electrolytes (GPEs)/hydrogels have been synthesized using deionized water (DW) and NaOH salt, and characterized through ionic conductivity, Fourier transform infrared (FTIR), pH, thermal and mechanical studies. Ionic conductivity decrement of liquid and GPEs was observed with the increase of temperature that contradicts pre-existing theoretical equation, i.e., σ = σo exp.(−Ea/kT) and maximum ionic conductivity of 8.75 × 10–2 S cm–1 observed for GPE containing 0.625 M NaOH salt at 30°C. Effect of temperature on pH has been investigated for different GPEs and the results were also supported by FTIR studies by formation of new and disappearance of old peaks. Thermogravimetric analysis studies involved the measurements of Tg for GPEs with the incorporation of different concentrations of NaOH salt, supported by DTG thermograms. Viscoelastic behaviour of GPEs with and without salt have been described by rheological studies at 30°C. In spite of that, time-dependent high structure recovery ratio pointed out the sol to gel transition in GPEs after the removal of applied shear rate. Due to high ion conducting, thermally and mechanically strengthened GPEs-based materials may make them applicable for their use in different device applications.

This research reports the preparation and characterization of xanthan gum (XG)-based gel electrolytes (GEs) comprising sodium hydroxide salt (NaOH) in deionized water (DW). The three-dimensional gel network has been formed without using any synthetic polymer or cross-linking agents. Ionic conductivity of GEs was evaluated with different parameters, such as salt concentration, gum concentration, temperature and with the passage of time. The maximum ionic conductivity of 74.8 mS cm–1 was observed at room temperature even after 55 days for XG-based GE containing 0.625 M NaOH. A small change in pH values for XG-based GEs have been observed with temperature in the range of 10–70°C and at different time span. Thixotropic behaviour of GEs under the application of stress has also been analysed by rheological studies. There was no discernible change in ionic conductivity with temperature and with the passage of time, which make it desirable for their use in different device applications.

Polymethylmethacrylate (PMMA) based polymer electrolytes containing ammonium trifluoromethane sulphonate (NH4CF3SO3), have been synthesized by solution casting method. Ionic conductivity of polymer electrolytes has been measured and maximum conductivity of 2.05 x10(-4) S/cm at room temperature has been observed at 10wt% NH4CF3SO3. The conductivity of polymer electrolytes has been found to increase with the addition of plasticizers. The effect of dielectric constant of plasticizer has also been studied and found that the increase in ionic conductivity containing high dielectric constant plasticizer DMA (37.8) is more than that of electrolyte containing low dielectric constant plasticizer DEC (3.2). The conductivity of plasticized polymer electrolytes further increases by a factor with the addition of fumed silica (SiO2) along with an increase in mechanical strength. The increase in ionic conductivity of polymer electrolytes with the addition of nano-filler has been explained by double threshold percolation model. Thermal stability of nano-composite plasticized polymer electrolytes has been checked by simultaneous measurement of DSC/TGA curves. The small change in ionic conductivity of nano-composite plasticized polymer electrolytes with temperature and time suggests that these electrolytes are thermally stable in 30-130 degrees C temperature range, which is useful for their use in electrochemical device applications like fuel cells, supercapacitors, proton batteries etc.

Abstract:This paper reviews proton-conducting polymer electrolytes comprising different polymers, salts, and acids. The ionic conductivity of plasticized polymer electrolytes has been found to increase with the addition of plasticizers due to the dissociation of ion aggregates or undissociated salt/acid present in the electrolytes, i.e., σ (plasticized polymer electrolytes) > σ (unplasticized polymer electrolytes). Proton-conducting nonaqueous nanocomposite plasticized polymer electrolytes containing poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF-HFP), polymethylmethacrylate (PMMA), polyethylene oxide (PEO) polymers; different ammonium salts and acids as proton conductors; ethylene carbonate (EC), propylene carbonate (PC), dimethylformamide (DMF), dimethylacetamide (DMA), dimethyl carbonate (DMC), diethyl carbonate (DEC) as plasticizers; fumed silica and alumina as nano-fillers have been discussed in details. Conductivity studies (effect of salt/acid, effect of plasticizers, effect of nano-fillers, and effect of temperature), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and differential scanning calorimetry/thermal gravimetric analysis (DSC/TGA) studies for these electrolytes have been discussed and reported in the paper. Nanocomposite plasticized polymer electrolytes showed high ionic conductivity (in the order of 10-1 to 10-2 S/cm) at room temperature along with good thermal and mechanical stability due to the simultaneous addition of both plasticizers and nano-fillers. These nanocomposite polymer electrolytes are the best candidates for use in various electrochemical devices like solid-state batteries, fuel cells, supercapacitors, sensors, separators, and other electrochromic devices.

Gum acacia (GA) based gel electrolyte was cross-linked with polyvinyl alcohol (PVA) in the presence of different concentrations of NaOH salt for the preparation of stable, biodegradable and saprophyte-free gel matrix, and characterized them with ionic conductivity, pH, FTIR and TGA studies. The maximum ionic conductivity (σ = 4.39 mS/cm at 30 °C) has been observed for GA-PVA based gel electrolyte containing lower concentration of NaOH salt and the analyte reaches toward neutral pH region as compared to acidic nature of gum acacia-based gel electrolyte in deionized water having ionic conductivity of 4.99 mS/cm at 30 °C. Physical cross-linking for better jellification has been analyzed through FTIR and thermogravimetric analysis (TGA). FTIR spectra of GA-PVA based gel electrolyte indicate the stability of the gel matrix at nearly neutral pH region and undergo complex decomposition with the influence of higher salt concentrations. Thermal stability and thermal behavior of gel electrolytes were investigated under non-isothermal conditions by thermogravimetric analysis and differential thermogravimetry (DTG), and the obtained results exhibit variations in the glass transition temperature (Tg) suggesting the miscibility of the compositions and also support the existence of compatibility of such system. Gel electrolyte with suitable composition indicates better stability near neutral pH region and small change in ionic conductivity over the temperature range of 10–70 °C make them suitable and applicable for many solid-state ionic device applications.

Polymer electrolytes (PEs) comprising the polar polymer complexed with ionic salts are important because of their use in different electrochemical devices such as solid-state batteries, fuel cells, supercapacitors, electrochromic devices, smart windows, and sensors. PEs are generally preferred due to some of their special properties such as good electrode–electrolyte contact, ease of preparation, high conductivity, good mechanical stability, wide range of composition, and hence wider control of properties. The PEs are classified as polymer–salt complexes, plasticized PEs, and nanocomposite PEs. The conductivity of PEs is quite small, which restricts their use in potential applications. The conductivity of the PEs is increased by incorporating suitable plasticizers in them, but the mechanical properties are relatively poor. The plasticizers have high dielectric constant, low viscosity, low freezing point, and high boiling point. The mechanical properties of PEs are improved by adding simultaneous plasticizer as well as inert insulating matrix and the electrolytes obtained are known as nanocomposite PEs. Nanocomposite PEs show high ionic conductivity (10−1–10−4 S/cm), low activation energy, and good mechanical and thermal stability. In this chapter, the synthesis and characterization of proton-conducting nanocomposite PEs are discussed. High ionic conductivity and good mechanical and thermal stability of nanocomposite PEs suggest that these electrolytes are desirable for their use in electrochemical devices.

Xanthan gum (XG)-based hydrogels containing sodium hydroxide (NaOH) salt were synthesized with the use of distilled water (DW) at room temperature and characterized through FTIR, TGA/DTG, and rheological studies. Sodium hydroxide is used to control pH toward neutral region along with improvement in ionic conductivity and stability of the electrolyte. The stabilized hydrogel has been obtained by applying heat treatment at ambient temperature for 5 wt% XG in 0.015 M solution of NaOH, which exhibits nearly neutral pH value at room temperature. The modification/shifting of the various peaks in FTIR spectra of xanthan gum with the addition of salt indicates the interaction or cross-linking between the constituents (xanthan gum, distilled water, and NaOH) and disappearing of peaks after heat treatment of the gel confirms its stability. DTG and TGA studies have been carried out to investigate thermal stability of these gels and illustrate the effect of heat treatment as a result of salt addition with thermogravimetric analysis up to 400 °C. However, rheological studies were performed for these hydrogels to analyze their viscosity behavior and mechanical stability. Along with the above characterization, gel sample (5 wt% XG in 0.015 M NaOH solution in DW) exhibits high ionic conductivity of 4.71 × 10−3 S/cm with 6.45 pH value at room temperature after heat treatment. These highly ion conducting, thermally and mechanically stable biodegradable xanthan gum-based hydrogels can also be used as an electrolyte for various device applications like supercapacitors, fuel cells, solar cells, etc.

Gel polymer electrolytes (GPEs) were prepared by dissolving lithium tetrafluoroborate (LiBF4) salt, poly(methylmethacrylate) (PMMA) polymer and distinct non-volatile solvents propylene carbonate (PC), and -N,N-dimethylformamide (DMF) in single as well as binary solvent mixtures. Ionic conductivities of 8.93 mS/cm and 6.68 mS/cm at 25 °C have been obtained for gel polymer electrolytes for 10 wt% PMMA in the solution of LiBF4 in binary solvent mixture of PC:DMF in (1:1) and (2:1) volume ratios respectively. The dispersion of nano-sized silica in gel polymer electrolyte not only exhibits small change in ionic conductivity but also enhances the mechanical strength as well as viscosity of gel polymer electrolytes. At room temperature, the ionic conductivity has been found to be 8.00 mS/cm for 6 wt% nano-sized silica in GPEs. Fourier-transform infrared (FTIR) spectroscopic studies have been used to scrutinize the corroboration of the complexation between PMMA, LiBF4, PC, DMF, PC:DMF, and SiO2. The interactions between salt and solvents in liquid electrolytes have also been analyzed by FTIR spectroscopy illustrating the strong interaction between lithium salt and solvent molecules. The appearance/disappearance and shifting of some peaks confirm the interaction among the constituents of nano-dispersed gel polymer electrolytes. The mechanical strength was confirmed by dynamic mechanical analysis (DMA) and viscosity [ηPC:DMF (2:1) > ηPC:DMF (1:1) > ηPC] for nano-dispersed silica-based gel polymer electrolytes. The electrical and mechanical stability with high ionic conductivity for such gel polymer electrolytes makes these electrolytes suitable for many device applications like high energy density lithium-ion batteries, super-capacitors, electro-chromic devices etc.

AC transport properties and dielectric response of sandwich geometry (Ag/CuPc/Ag) of CuPc(CuPc) thin films deposited using thermal evaporation technique have been studied within frequency range 1 Hz–10 KHz and in temperature range 303–383 K. Scanning electron microscope (SEM) investigations of these films reveal fiber like morphology. Crystalline natures of CuPc films have been characterized using X-ray diffraction for different temperatures. The molecular orientations in films for different substrate temperatures have been confirmed by Raman spectroscopy. The optical band gaps calculated from the UV–Visible absorption spectra is found to lie in the range 3.01–3.15 eV. Electrical conductivity of CuPc films increases with increase of temperature. The hole mobility values of CuPc films at different temperatures have been calculated using negative differential susceptance (–ΔB) technique. Both capacitance and dielectric constant have been found to decrease with the increase of frequency and temperature.

A cost-effective drop-cast technique has been used to deposit copper phthalocyanine (CuPc) films on a glass substrate. The obtained films have undergone structural, optical and electrical characterization after annealing at different temperatures – that is, 100, 150 and 200°C. The X-ray diffraction spectra confirm the formation of CuPc films. The absorption spectra of the drop-cast CuPc films show two dominant bands – Q-band and Soret band – within wavelengths of 300–800 nm, respectively. Phase transformations from the α-phase to β-phase have been observed from structural and optical characterization. The current–voltage parameters of the films show ohmic contact, and their activation energies lie in the range of 0·21–0·54 eV annealed within temperatures of 100–200°C. The vapor-sensing characteristics of the CuPc-based sensor toward ammonia at different concentrations (15–230 parts per million) have been evaluated. These measurements reveal that CuPc films are a good candidate as ammonia sensors.

Polymethylmethacrylate (PMMA) based nano-dispersed polymer gel electrolytes containing lithium tetra-fluoroborate (LiBF4), non-volatile solvents: propylene carbonate (PC) as single solvent, binary solvent mixtures with N,N-dimethylformamide (PC:DMF) in different volume ratios and nano-sized silica have been prepared and characterized. Ionic conductivity of gel as well as liquid electrolytes depends mainly upon the donor number and viscosity of the solvents used. Maximum ionic conductivity of 9.4 x 10(-3) S/cm at 25 degrees C has been obtained for nano-dispersed silica based polymer gel electrolyte having (PC:DMF = 1:1) volume ratio. Small content of PMMA in gel electrolyte improves the ionic conductivity, whereas small content of nano-sized silica not only enhances the ionic conductivity, but also improves the mechanical strength of the electrolyte. Two conductivity maxima observed at very low content of nano-sized silica in PMMA based gel electrolytes for binary solvent mixture having 2:1 and 1:1 volume ratios have been explained by double percolation threshold model. Moreover nano-dispersed silica based polymer gel electrolytes show good thermal properties, which have been confirmed by Differential Scanning Calorimetry (DSC) & Thermo Gravimetric Analysis (TGA) and mechanical properties have been studied by Dynamic Mechanical Analysis (DMA) studies. Also, the ionic conductivity of nano-dispersed silica based polymer gel electrolytes show typical curvature behavior as compared to polymer gel electrolyte over the temperature range of 10 degrees C-70 degrees C indicating their high amorphous nature. Also, the comparative results have been observed via activation energies for polymer gel electrolytes with and without silica, which have been calculated from logo vs. 1000/T plot. The behavior of the plot does not show much change at all temperature regions (change is only by a factor), which compile acute in distinct electrochemical devices.

Ionic conductivity of polymer electrolytes obtained by complexation of trifluoromethanesulfonic acid (HCF3SO3) (triflic acid) with polyethylene oxide (PEO) has been found to increase with the addition of dimethylacetamide (DMA) as plasticizer. The increase in conductivity has been explained to be due to dissociation of ion aggregates with the addition of plasticizer, which has also been supported by FTIR studies. Plasticized polymer electrolytes have high ionic conductivity but not show better mechanical properties. Nano-sized fumed silica (SiO2) is added to improve its mechanical strength alongwith an increase the ionic conductivity of plasticized polymer electrolytes. Maximum ionic conductivity of plasticized nano-composite polymer electrolytes of 8.14×10−3Scm−1 at room temperature has been observed for the composition PEO+8wt% HCF3SO3+50wt% DMA+3wt% SiO2. X-ray diffraction studies of polymer electrolytes suggests that the amorphous content increases with the addition of plasticizer and nano-filler, which is in agreement with the conductivity results. The small change in conductivity over 30–130°C temperature range suggests that these electrolytes are suitable for their use in device applications like fuel cells, supercapacitors, sensors, separators and other electrochromic devices. DSC/TGA studies show that these nano-composite plasticized polymer electrolytes possess good thermal properties alongwith high conductivity.

Nano-sized silica poly(methylmethacrylate)-based gel electrolyte containing lithium hexafluorophosphate (LiPF6) was synthesized by using different binary solvent mixture (propylene carbonate(PC) and dimethylformamide (DMF) in different volume ratio). Role of DMF in PC: Higher DMF content in PC-based electrolyte shows higher ionic conductivity at all polymer content and at wide temperature regions (10-70 °C). A small increment in ionic conductivity at lower content of polymer in liquid/gel electrolyte was observed and having maximum conductivity of 13.12 mS/cm at 25 °C. Stability (mechanically and electrically), viscosity and ionic conductivity of gel electrolytes were improved with the addition of nano-sized silica at ambient temperature. Ionic conductivity of nano-sized silica-based gel electrolyte does not change much over 5o–70 °C temperature range and is factor-wise only which make indispensable in different electrochemical devices. Also polymer gel electrolyte membranes as such and with dispersed silica nano-particles were characterized through scanning electron microscope to study the morphology of gel matrix.

The present paper reports the structural, optical and electrical properties of zinc phthalocyanine (ZnPc) thin films which were grown by the thermal evaporation technique at different substrate temperatures of 312, 363 and 413 K and dielectric response of sandwich geometry of ZnPc thin films have also been studied within frequency range 1 Hz-50 KHz. The crystal structures of these ZnPc films have been characterized using the X-ray diffraction technique. Raman spectra and photoluminescence have been recorded to study the molecular orientations in the ZnPc films for different substrate temperatures. The absorption spectra of the ZnPc films have shown two absorption bands - namely, the Soret band and Q-band. The activation energy values of these films have been determined to be lying in the range of 0.70-0.75 eV. Hole mobility values of ZnPc films have been calculated by using differential susceptance method. The capacitance and dielectric constant have been found to decrease with increase in frequency.

The titanium dioxide films have been obtained by spray pyrolysis technique on to the glass substrates kept at different temperature (300- 4000C) .The conditions have been optimized to obtain quality films. Films so obtained have been characterized for their structure through x-ray diffractograms. Optical absorption studies of the films have been made through UV-Visible spectroscopy in the spectral range 300 -1100 nm. Effect of substrate temperature on the structure and optical properties of these films has been studied. Results indicate that the films so obtained are promising candidates for solar cells.

Nano-composite polymer gel electrolytes were synthesized by using polyethylene oxide (PEO), ammonium tetrafluoroborate (NH4BF4), fumed silica (SiO2), dimethylacetamide (DMA), ethylene carbonate (EC), and propylene carbonate (PC) and characterized by conductivity studies. The effect of donor number of solvent on ionic conductivity of polymer gel electrolytes has been studied. The mechanical strength of the gel electrolytes has been increased with the addition of nano-sized fumed silica along with an enhancement in conductivity. Maximum room temperature ionic conductivity of 2.63 × 10−3 and 2.92 × 10−3 S/cm has been observed for nano-composite gel electrolytes containing 0.1 and 0.5 wt% SiO2 in DMA+1 M NH4BF4+10 wt% PEO, respectively. Nano-composite polymer gel electrolytes having DMA have been found to be thermally and electrically stable over 0 to 90 °C temperature range. Also, the change in conductivity with the passage of time is very small, which may be desirable to make applicable for various smart devices.

The zinc oxide films have been obtained by spray pyrolysis technique on to the glass substrates kept at different temperature (380-4800 degrees C). The conditions have been optimized to obtain quality films. Films have been characterized for their structure through XRD analysis and for optical parameters through optical absorption studies by UV-Visible spectroscopy in the spectral range 300 -1100 nm. Effect of substrate temperature on the structure, extinction coefficient, optical band gap and refractive index of these films has been studied.

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