Pechini Method Research Articles

Comparative Study of Zn2Ti3O8 and ZnTiO3 Photocatalytic Properties for Hydrogen Production

In the present work, zinc titanates (ZTO) as photocatalysts were synthesized, characterized, and evaluated aiming to study their photocatalytic properties for hydrogen production under visible-light irradiation and employing MeOH (methanol) and TEOA (Triethanolamine) as sacrificial agents. ZTO were synthesized by modified Pechini method. Characterization of materials consisted in TGA, XRD, TEM, EELS, BET, and UV–Vis. Surface interaction studies consisted of FT-IR spectroscopy and determination of MeOH and TEOA adsorption–desorption capacities on the ZTO by TGA. Zinc titanates were evaluated as photocatalyst for H2 production using an artificial visible light and monitored by GC. TGA results led to establish calcination temperatures of 550 °C (Zn2Ti3O8) and 700 °C (ZnTiO3) to reach their crystalline phases. XRD analysis of sample cds-ZTO found cubic Zn2Ti3O8 and traces of the ZnO crystalline phase, while p-ZTO exhibited a mixture of cubic and hexagonal ZnTiO3 crystalline phases. Surface area for cds-ZTO was 88 m2/g, while ZnTiO3 had 13 m2/g. Photocatalytic H2 production for cds-ZTO and p-ZTO using TEOA as sacrificial agent showed the highest photocatalytic activities generating 548 and 441 µmolH2/h.gcat. TEOA adsorption–desorption capacity was found superior on cds-ZTO and p-ZTO than that for MeOH on both samples.

Application of Spinel MgMn2-X Al x O4 As Cathode for Mg Rechargeable Battery

【Introduction】Lithium-ion battery (LIB) has mainly used in our life, but its high price due to Li and Co metals are crucial problem. Magnesium rechargeable battery (MRB) has been recently studied as a post LIB due to elemental abundant supply and superior theoretical volumetric energy density of magnesium. For cathode materials, spinel oxides is one of a candidate of MRB due to its high redox potential and three-dimensional diffusion paths.[1] Especially, MgMn2O4 is expected to perform high theoretical capacity because utilization of both Mn3+/Mn4+ and Mn2+/ Mn3+ redox is possible in the potential window of the common electrolyte.[2] But structural change from tetragonal to cubic occurs due to Jahn-Teller effect of Mn3+ ion during charge/discharge, which decreases reversibility. In this study, we tried to enhance reversibility of MgMn2O4 spinel by substituting Al for Mn to release its Jahn-Teller distortion, and the optimal substitution ratio and their electrochemical property were evaluated.【Experimental】MgMn2-xAlxO4 (x = 0, 0.1, 0.2, 0.5) were synthesized by Pechini method[3] with an annealing process of 400 ºC, 10 hour. Cathodes were prepared by mixing the obtained samples with acetylene black and polytetrafuluoroethylene at a weight ratio of 60/30/10 . Mg alloy (AZ31) was used for an anode. Galvanostatic charge/discharge profiles were obtained by using a coin cell with a 0.3 M Mg[B(HFIP)4]2/triglyme electrolyte at 25 ºC, 10 mA/g.【Results and discussion】According to X-ray diffraction(XRD) patterns, MgMn2-xAlxO4 (x = 0, 0.1, 0.2, 0.5) spinel were obtained and their crystallinity become lower by Al substitution. In MgMn1.5Al0.5O4, the crystal structure changed from tetragonal to cubic phase, suggesting that the Jahn-Teller effect is suppressed by the formation of the solid solution of tetragonal MgMn2O4 and cubic MgAl2O4. The Al-substituted MgMn2O4 exhibited higher discharge capacities compared with MgMn2O4 (64.0 mAh/g), and especially MgMn1.9Al0.1O4 showed the highest discharge capacity of 92.3 mAh/g. In the poster session, X-ray absorption spectroscopy (XAS) and cycle characteristics will be reported.【Acknowledgment】This work was supported by JST ALCA-SPRING Grant Number JPMJAL1301, Japan.【References】[1] S. Okamoto, T. Ichitsubo, T. Kawaguchi, Y. Kumagai, F. Oba, S. Yagi, K. Shimokawa, N. Goto, T. Doi and E. Matsubara, Adv. Sci., 2015, 2, 1500072[2] H. Kobayashi, K. Yamaguchi and I. Honma, RSC Adv., 2019, 9, 36434-36439.[3] J. Yin, A. B. Brady, E. S. Takeuchi, A. C. Marschilok and K. J. Takeuchi, Chem. Commun., 2017, 53, 3665-3668.

Study of Critical Magnetic Behaviour in Nanocrystalline La0.65Ce0.05Sr0.3Mn1−xCuxO3 (x = 0, x = 0.05 and x = 0.15) Prepared by Pechini Method

The critical bahaviour of La0.65Ce0.05Sr0.3Mn1xCuxO3 (x = 0, x = 0.05 and x = 0.15) manganite prepared by the sol–gel-based Pechini method has been investigated by measuring the magnetization around the Curie temperature, TC. The obtained critical exponents (beta, gamma and delta) have been calculated using the modified Arrott plot and Kouvel–Fisher techniques, scaling hypothesis and critical isotherm analysis. The estimated results for the parent compound and x = 0.05 are in between mean-field and the 3D Heisenberg models. The values of β, γ and δ will shift gradually toward those of the 3D Heisenberg theory when x = 0.15, suggesting that the short-range FM order and magnetic inhomogeneity are favoured in Cu-doped samples. The non-monotonous temperature variation in effective exponents (βeff(ɛ) and γeff(ɛ)) proves the existence of a magnetic disorder in the studied compounds.

Synergistic Effect on Photocatalytic Activity of Co-Doped NiTiO3/g-C3N4 Composites under Visible Light Irradiation

Co-doped NiTiO3/g-C3N4 composite photocatalysts were prepared by a modified Pechini method to improve their photocatalytic activity toward methylene blue photodegradation under visible light irradiation. The combination of Co-doped NiTiO3 and g-C3N4 and Co-doping into the NiTiO3 lattice synergistically enhanced the photocatalytic performance of the composite photocatalysts. X-ray photoelectron spectroscopy results for the Co-doped NiTiO3/g-C3N4 composite photocatalysts confirmed Ti-N linkages between the Co-doped NiTiO3 and g-C3N4. In addition, characteristic X-ray diffraction peaks for the NiTiO3 lattice structure clearly indicated substitution of Co into the NiTiO3 lattice structure. The composite structure and Co-doping of the C-x composite photocatalysts (x wt % Co-doped NiTiO3/g-C3N4) not only decreased the emission intensity of the photoluminescence spectra but also the semicircle radius of the Nyquist plot in electrochemical impedance spectroscopy, giving the highest kapp value (7.15 × 10−3 min−1) for the C-1 composite photocatalyst.

An A- and B-Site Substitutional Study of SrFeO3-δ Perovskites for Solar Thermochemical Air Separation.

An A‑ and B‑site substitutional study of SrFeO3−δ perovskites (A’xA1−xB’yB1−yO3−δ, where A = Sr and B = Fe) was performed for a two‑step solar thermochemical air separation cycle. The cycle steps encompass (1) the thermal reduction of A’xSr1−xB’yFe1−yO3−δ driven by concentrated solar irradiation and (2) the oxidation of A’xSr1−xB’yFe1−yO3−δ in air to remove O2, leaving N2. The oxidized A’xSr1−xB’yFe1−yO3−δ is recycled back to the first step to complete the cycle, resulting in the separation of N2 from air and concentrated solar irradiation. A-site substitution fractions between 0 ≤ x ≤ 0.2 were examined for A’ = Ba, Ca, and La. B-site substitution fractions between 0 ≤ y ≤ 0.2 were examined for B’ = Cr, Cu, Co, and Mn. Samples were prepared with a modified Pechini method and characterized with X-ray diffractometry. The mass changes and deviations from stoichiometry were evaluated with thermogravimetry in three screenings with temperature- and O2 pressure-swings between 573 and 1473 K and 20% O2/Ar and 100% Ar at 1 bar, respectively. A’ = Ba or La and B’ = Co resulted in the most improved redox capacities amongst temperature- and O2 pressure-swing experiments.

Effect of pH on the Tribological Behavior of Eu-Doped WO3 Nanoparticle in Water-Based Fluid

Eu-doped WO3 (WO3:Eu3+) nanoparticles were prepared by Pechini method under different pH values (pH 1, 3, 5, and 7). The prepared nano-powders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The results showed that the average external diameter of the prepared nano-WO3:Eu3+ powders is the smallest and reaches 50 nm at pH 5. Structural transformation matrix contained different crystals of anorthic and orthorhombic structures. Eu3+ ions are located at the center of the non-inversion symmetry of WO3:Eu3+. The tribological properties of the WO3:Eu3+ as extreme pressure and wear resistance agents in water-based lubricant were investigated by a four-ball machine. The results showed that WO3:Eu3+ displays excellent load-carrying capacity, wear resistance, and friction-reducing properties in water-based lubricant, particularly in the best concentration of WO3:Eu3+ was 0.6 wt%. WSD was reduced from 0.62 to 0.35 mm and COF was decreased from 0.083 to 0.055. This was due to the formation of tribofilms with a few tens of nanometers thick, which prevented no actual metal-to-metal contact.

Applying a Novel Polymeric Precursor Derived by Capillary-Gravitational Coating in Fabrication of Nanostructured Tri- Metal Oxide-Based pH Sensing Electrode

In this study polymeric precursor (Pechini method) has been modified and utilized with purpose of fabricating tri-metal oxide pH sensing electrode. The method used in this research is unlike Pechini method, hence, propylene glycol used instead of ethylene glycol. pH sensing films were prepared using top candidates in the list of metal oxides that have been used in this field, such as IrO2, RuO2 and TiO2. New process called gravitational-capillary coating method applied to coat two different wire substrate (Ti and Steel). Synthesized electrodes characterized by SEM and X-ray diffraction, other related tests carried out. Suitable close Nernstian slope sensitivity −58.69 and −58.89 mV/pH have been observed, for titanium and steel electrodes respectively, acceptable stability, low hysteresis, insignificant rate of drift, short response time 3-3.5 sec with perfect selectivity have been estimated for both electrode.

Structural and Magnetic Characterisations of Pb-Doped MgO Nanoparticles by a Modified Pechini Method

Doping magnesium oxide nanoparticles (MgO-NPs) forms a good material for magnetisation applications. The Room Temperature Ferromagnetic (RTFM) of Pb2+-doped ions MgO-NPs synthesised by a modified Pechini method are discussed in the present paper. The structural, morphological and magnetic properties of the samples were characterised by X-ray diffraction (XRD), Field Emission scanning electron microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS) and vibrating sample magnetometer (VSM).The XRD results showed that the synthesised materials have a single set of peaks in the XRD patterns, corresponding to the cubic phase of MgO-NPs. As the Pb content increased in the host MgO-NPs leading to an increase in the lattice parameter, the interplanar spacing and the crystallite size; however, the intensity decreased.Small spherical nanoparticles (22.87–29.05nm) were observed in the Pb2+-doped ions MgO samples by (FE-SEM). The purity of the samples was confirmed using EDS spectroscopy.The pure MgO and doped samples exhibiting RTFM may be attributed to vacancy defects, which caused local magnetisation. The saturation magnetism (Ms) was found to be varied as a function of doping concentration. The maximum (Ms) was found at x=0.015 of Mg0.985Pb0.015O sample. The obtained results suggest that both Pb doping and oxygen vacancies play an important role in the development of room-temperature ferromagnetism.

Electrochemical Degradation of Pharmaceuticals Using Ti/SnO2-Sb2O5-IrO2-RuO2 Anode: Electrode Properties, Performance and Contributions of Diverse Reactive Species

Non-biodegradable pharmaceuticals are a group of emerging contaminants that have gained much attention because of their potential risk of inducing adverse ecological and health effects. An efficient Ti/SnO2-Sb2O5-IrO2-RuO2 electrode was prepared by Pechini method and employed as the anode for electrochemical degradation of selected pharmaceuticals (i.e., ibuprofen, atenolol, and carbamazepine). Compared its counterparts, Ti/SnO2-Sb2O5-IrO2-RuO2 exhibited higher oxygen evolution potential, lower chlorine evolution potential, larger active area, and higher stability. Unlike the negligible effect of solution pH from 4.0 to 10.0, increasing current density favored the target pollutants and COD removal. The removal of IBU was mainly attributed to the reaction with •OH, the contribution of which to IBU removal was enhanced with increasing current density. In contrast to IBU, the removal of ATEN and CBZ was mainly ascribed to the reaction with selective radical chlorine species (RCS) mainly in the form of Cl•, which was produced from direct oxidation of Cl− or indirect oxidation by •OH. It was found that the removal of ATEN and CBZ was less affected by dissolved organic matter (DOM) than that of IBU in municipal effluent. This study demonstrates that Ti/SnO2-Sb-RuO2-IrO2 is an attractive electrode for the destruction of pharmaceutical contaminants.

Effect of annealing temperature on persistent luminescence of Y3Al2Ga3O12:Cr3+ co-doped with Ce3+ and Pr3+

Abstract Y3(Al,Ga)5O12 (YAGG) materials doped with Ce3+, Cr3+ and Pr3+ were synthesized by using a modified Pechini method and subsequently annealed in air at selected temperatures between 900 and 1500 °C. According to X-ray powder diffraction (XRPD) and transmission electron microscopy (TEM) analyses, the particles and size distributions become large and broad, respectively, due to sintering and agglomeration at high annealing temperatures. Based on infrared (FTIR) spectra and calculation of multi-phonon de-excitation probabilities, the high energy O–H vibrations are not causing significant multi-phonon de-excitation of the emitting 5d level of Ce3+ if the annealing temperature is above 900 °C. The analysis of the photoluminescence excitation (PLE), photoluminescence (PL) and persistent luminescence (PersL) spectra as well as the luminescence decay curves revealed that both the energy transfer efficiency and luminescence intensity increase with increasing annealing temperatures. The charge carrier trapping-detrapping model was applied to explain the PersL mechanism of the YAGG materials studied.

Barium cobaltite nanoparticles: Sol-gel synthesis and characterization and their electrochemical hydrogen storage properties

The study of the effect of different chelating agents in the Pechini method on the morphology has been a promising strategy that can be used for practical tuning of the nanoparticle's morphology and hence the electrochemical hydrogen storage capacity. In the current study, the conventional Pechini sol-gel approach was used to prepare the Ba2Co9O14 nanoparticles as a novel hydrogen storage material. The X-ray diffraction investigation approved the formation of Ba2Co9O14 with a Hexagonal crystal structure for all of the synthesized samples. The scanning electron microscopy (SEM) revealed when citric acid was used as a chelating agent, nanoparticles with finer and more uniform morphology were obtained rather than other chelating sources. The transmission electron microscopy (TEM) showed in the presence of citric acid; the size of the synthesized nanoparticles was between 14 and 24 nm. According to the Diffuse Reflectance Spectroscopy (DRS) analysis, the calculated bandgap of synthesized nanoparticles was approximately 3.2 eV, which indicates that synthesized nanoparticles were semiconductors in essence. The electrochemical hydrogen adsorption/desorption results showed that the sample synthesized by the citric acid has an enhancement in electrochemical hydrogen storage of approximately 800 mAh/g after 15 cycles.

Magnetization Dynamics Behavior in Y3Fe5O12 Particles

YIG particles were obtained by Pechini method with a thermal annealing between 800 and 1200 °C. The formation of the cubic YIG phase was corroborated by means of X-ray diffraction (XRD), where YIG particles have crystallite size range between 107 and 303 nm. Magnetization dynamics were studied by means of magnetization hysteresis cycles, ferromagnetic resonance, and micromagnetic simulations. Different magnetic processes were determined as particle size function, and the magnetization dynamics can be explained by different contributions, such as single domain state, magnetic vortex state, and superparamagnetic behavior, besides considering their interactions. Graphical Abstract

Effects of temperature and heating method on the performance of Ti/Ru0.25Ir0.25Ti0.50O2 anodes applied toward Bisphenol S removal

One of the challenges faced by environmentally-related electrochemical techniques and which limit their industrial application is the lack of efficient and economically viable electrodes. This paper reports the development and application of a microwave-assisted hybrid heating method for the production of mixed metal oxide (MMO) anodes aiming at obtaining low-cost, highly catalytic, and durable anodes with reduced production time. The Ti/Ru0.25Ir0.25Ti0.50O2 electrodes were prepared by the Pechini method using two calcination temperatures (350 and 400 °C) and two heating mechanisms (conventional in an electric furnace and hybrid heating using microwaves). The electrodes developed were applied toward the electrochemical degradation of Bisphenol S (BPS); this is the first report involving the application of MMO electrodes for BPS removal in the literature. The calcination temperature and type of heating influence the electrodes physical and electrochemical characteristics, as well as the film compositions and catalytic activities. With the exception of the anode produced in the furnace at 400 °C (CM-400), which exhibited a crack-free compact surface, the oxide film layers covered the Ti substrates entirely, displaying a typical “cracked mud” morphology. The morphological characteristics of CM-400 contributed toward obtaining low voltammetric charge (88 mC) and high resistivity (194 Ω) for the film. In contrast, the electrode developed by microwave-assisted hybrid heating at 350 °C was produced in a relatively shorter time (4.6-fold), presented the lowest charge transfer resistance (24 Ω), the highest voltammetric charge (240 mC), and the highest stability (with 51 h – accelerated life test). Overall, the electrodes produced in furnace were slightly more efficient when applied toward the electrochemical removal of BPS; to be precise, the electrode calcined at 400 °C showed total BPS removal in 10 min at 100 mA cm–2. About 20% of TOC removal was obtained in 60 min of electrolysis; this is the highest TOC rate reported for BPS under such short treatment time. Thus, the anodes developed are found to be suitable and highly promising for the electrochemical removal of BPS from water.

Luminescence behaviour of the synthesized erbium and thulium co-doped potassium, sodium, lithium or rubidium yttrium double tungstate nanopowders

Nanocrystalline M I Y(WO 4 ) 2 double tungstates (M I = Li, Na, K and Rb) co-doped with Er 3+ and Tm 3+ ions were synthesized by hydrothermal and Pechini techniques and characterised by means of X-ray diffraction, infrared absorption and electron absorption spectra. Their emission spectra and luminescence decay kinetics were recorded at ambient temperature. These investigations were focused on impact of structural changes and morphology inducing by the alkaline ion on the Er ↔ Tm energy transfer efficiency in the studied nanocrystalline oxide systems. The effect of the thermal treatment on morphology and spectroscopic properties of the synthesized nano-materials was studied. Furthermore, emission spectra attained under different excitation as well as study on luminescence decay curves made it possible to determine the differences and dynamics of feeding and relaxation of excited states involved in luminescence phenomena. The energy transfer mechanism between Er 3+ and Tm 3+ ions was proposed and analysed in terms its usefulness in the phosphors and optical amplifiers operating at 1.8 μm. • Li/Na/K/RbY(WO 4 ) 2 :Er 3+ ,Tm 3+ were synthesized by the Pechini and hydrothermal method in the nanocrystalline form. • Structural properties were characterised by the X-ray diffraction (XRD) and infrared spectroscopy. • Strong green emission of Er 3+ ions located at 525 and 550 nm is observed for all compounds. • The lowest intensity of this emission is observed for lithium compounds. • The efficient energy transfer from erbium to thulium takes place in KY(WO 4 ) 2 :Er 3+ ,Tm 3+ sample.

Sol-gel synthesis and characterization of Co3O4/CeO2 nanocomposites and its application for photocatalytic discoloration of organic dye from aqueous solutions.

Herein, Co3O4/CeO2 nanocomposite was synthesized by the modified Pechini method. Citric, maleic, succinic, and trimsic acids were used as a stabilizer, and the variation affected the morphology and size of the synthesized nanocomposites. Subsequently, the formation of Co3O4/CeO2 nanocomposites was confirmed by various analyses. Furthermore, the particles were considered for size and morphology by SEM and HRTEM analyses, and the sample that used trimsic acid as the stabilizer was designated as the goal sample to continue the route. The optimum sample was used to investigate the photocatalytic properties of the synthesized nanocomposite. The UV-light photocatalyst test was performed in neutral, alkaline, and acidic states against two aqueous solutions containing color contamination of methylene blue and erythrosine B dyes. The results showed decolorization at 85% for methylene blue and 90% for erythrosine B over 120 min test time.

Estudio de la actividad catalítica de la ferrita de cobalto en la degradación de diclofenac sódico

Los contaminantes emergentes y dentro de ellos los compuestos farmacéuticos suelen encontrarse en aguas superficiales y residuales a lo largo del planeta. En este trabajo se presenta el estudio de la degradación de diclofenac sódico mediante un proceso tipo foto-Fenton heterogéneo empleando ferritas de cobalto. Los materiales fueron sintetizados con el método de Pechini y caracterizados mediante difracción de rayos X, espectroscopía Mössbauer, espectroscopía fotoelectrónica de rayos X, espectroscopía Uv-visible, reducción a temperatura programada y área superficial. Se obtuvieron fases puras con estructura de espinela. Ambos materiales presentaron buenos resultados catalíticos en la degradación del contaminate. Se propone un mecanismo de reacción radicalario basado en la formación de radicales *OH. Se logró una degradación completa del compuesto, con un 86% de mineralización del carbono orgánico total empleando el material calcinado a 800°C. El catalizador presentó excelentes resultados en tres ciclos consecutivos de uso.

Modeling and optimization of synthesis condition of CuCr2O4 Spinel for CO oxidation

In this paper, the CuCr2O4 spinel catalyst was synthesized by the Pechini method, and its activity was evaluated in catalytic oxidation of CO. CuCr2O4 spinel catalyst was characterized by XRD, BET, H2-TPR, and SEM. This catalyst has a good ability in CO oxidation. The effects of three synthesis variables (EG/citrate, citrate/nitrate ratio, and calcination temperature) and reaction temperature as an operational variable on CO conversion were investigated. Based on the results, the optimum neural network architecture succeeded to predict CO conversion data with an acceptable level of accuracy. The model predicted that the relative importance of variables is as follows: calcination temperature > citrate/nitrate ratio > EG/citrate ratio. The optimum neural network architecture was used as a fitness function for the genetic algorithm to find the optimum catalyst. Under the optimum condition (EG/citrate: 3.24, citrate/nitrate ratio: 0.62 and calcination temperature: 620 °C), the predicted optimum value of CO conversion was found to be in a good agreement with the corresponding actual value.

Study of the Corrosion of Carbon Steel (SAE 1020) Coated with Niobium Oxides

Carbon steel is widely used in the industry due to its mechanical properties and low cost, but in contrast it resists poorly to corrosion, leading to economic losses and mechanical issues. The use of surface treatment is essential to extend the life of the metallic material. In this context, niobium is being studied for its great corrosion resistance properties. The aim of this paper was to produce and evaluate the corrosion protection of a niobium-based coating produced by the Pechini Method. The resin was applied in the metallic surface by dip-coating and then calcinated at 450 oC for 1 hour. The coated material was analyzed electrochemically by open circuit potential and potentiodynamic polarization, and morphologically by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. The electrochemical analyses showed that the deposition of the coating increased the corrosion resistance and the morphological analyses indicated a homogenous coating with the presence of phases of NbO and NbO2.

Synthesis and Characterization of Barium Titanate Nanopowders by Pechini Process

Barium titanate nanoparticles have been synthesized via Pechini method, using barium acetate and an aqueous solution of titanium(IV) triethanolaminato isopropoxide. Structural properties of barium titanate (BaTiO3) are characterized by X-ray diffraction (XRD), Rietveld refinement, scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX), thermogravimetric analysis (TGA) and Fourier-transform infrared spectroscopy (FT-IR). XRD and Rietveld refinement studies revealed that BaTiO3 possesses a cubic structure with a space group of Pm-3m (#221). As estimated by the Scherrer formula, the average crystallite size was accurately determined to be properly 51.9 nm for the calcined temperature at 800ºC.

A Comparison of the Role of the Chelating Agent on the Structure of Lithium Conducting Solid Electrolyte Li1.4Al0.4Ti1.6(PO4)3: Pechini vs. Modified Pechini-Type Methods

In recent years, solid lithium-ion conductors have been widely studied because of their applications as electrodes and solid electrolytes in rechargeable lithium-ion batteries. Citric acid (CA) and ethylenediaminetetraacetic acid (EDTA) were employed to synthesize the nanostructured NASICON-type Li1.4Al0.4Ti1.6(PO4)3 ceramic. The chelating agent, together with an ethylene glycol (EG) and the esterification agent were employed to form a network decorated with uniform dispersed metal ions under specific conditions: molar ratio [complexing agent/metal ions] = 1 and the molar ratio [EG/EDTA] = 6, whereas the solution pH was kept below 1. A well crystalline NASICON structure was formed following the heat treatment of the produced gel at 630 °C. Simultaneous thermal analysis (STA) revealed lower required temperature for pyrolysis and crystallization using EDTA. Powder X-ray diffraction (PXRD) showed the formation of larger crystallite size when citric acid was employed. The data from scanning electron microscopy (SEM) and electrochemical impedance spectroscopy (EIS) have confirmed the higher apparent porosity and a larger proportion of grain boundaries in the case of EDTA-assisted synthesis.