Tumuluri, Anirudh. Synthesis of borosilicate gels with phenyl modifications and its effects on proton conductivity. Retrieved from https://doi.org/doi:10.7282/t3-15a9-vc57
DescriptionSilicon alkoxides with boron alkoxides or boric acid were used to prepare borosilicate xerogels. Nitric acid was used to promote the hydrolysis of the silicon alkoxides, tetraethylorthosilicate (TEOS) and phenyltriethoxysilane (PhTES). Triethyl borate (TEB) and boric acid were the source of boron in the gels. The compositions were: 85 wt. % TEOS - 15 wt. % TEB, 80 wt. % TEOS - 15 wt. % TEB - 5 wt. % PhTES, 75 wt. % TEOS - 15 wt. % TEB, 10 wt. % PhTES, 85 wt. % TEOS - 15 wt. % Boric Acid, 80 wt. % TEOS - 15 wt. % Boric Acid - 5 wt. % PhTES and 75 wt. % TEOS - 15 wt. % Boric Acid, 10 wt. % PhTES.
Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) were performed to investigate the loss of weight and heat flows in the gels as a function of temperature. The weight loss and the energy absorbed during the endothermic peak decreased with the increasing PhTES content. Gels made from TEB show lower weight losses and enthalpy changes compared to similar gels made from boric acid.
X-Ray Diffraction was performed for phase identification and to determine the amount of crystallinity in the gels. The diffraction patterns contained peaks that were attributed to boric acid precipitates, which occurred in all the gels. Increase in PhTES decreased the amount of crystallinity in the gels. Gels made from TEB show lower amounts of crystallinity compared to similar gels made from boric acid.
Moisture adsorption-desorption was performed to investigate the water retention capabilities of the gels. The increases in PhTES content decreased the water retained in the gels. Adsorption values of the gels made from TEB and boric acid are comparable, but the mass loss due to desorption are higher for the gels synthesized from boric acid.
Electrochemical Impedance Spectroscopy (EIS) was performed to measure the proton conductivity of the gels. The increase in PhTES content reduces the proton conductivity slightly. Proton conductivity is dependent on the number of protons and number of sites available for hopping of protons. The phenyl in PhTES decreased the number of protons and sites. Gels prepared from TEB show higher proton conductivity compared to same gels made from boric acid.