A Rapid Sustainable Sol-Gel Synthesis of Phase-Pure BaTiO₃ Nanostructures with Minimal Energy Demand

A Rapid Sustainable Sol-Gel Synthesis of Phase-Pure BaTiO₃ Nanostructures with Minimal Energy Demand | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article A Rapid Sustainable Sol-Gel Synthesis of Phase-Pure BaTiO₃ Nanostructures with Minimal Energy Demand I. E. Correa, J. A. Ascencio, S. E. Borjas, A. Medina This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8912633/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 9 You are reading this latest preprint version Abstract The present work reports the production of BaTiO 3 ceramic nanostructures through a sustainable sol-gel synthesis route that drastically reduces energy demand while improving phase purity. Two synthesis strategies were compared: (A) a conventional route based on Ba(OH)₂ under controlled humidity and inert conditions, and (B) a modified route employing BaCl₂ as precursor under ambient atmosphere. This optimized method achieved an ~81% reduction in energy consumption, decreasing synthesis from 180 °C for 24 h to 130 °C for 3 h. Importantly, carbon-related impurities were significantly suppressed, obviating the need for post-synthesis acid washing treatments. Structural and morphological analyses (FT-IR, XRD with Rietveld refinement, FE-SEM, chemical mapping, and BET) confirmed enhanced phase purity, a drastic reduction particle size (~100 nm to ~25 nm), and high surface area high surface area (> 50 m 2 /g). This methode provided a scalable and environmentally responsible pathway that allows the scalable production of high-purity BaTiO₃, advancing sustainable materials processing for electronic and energy-related applications. Sustainable Synthesis Sol-gel Eco-Friendly Nanostructured Ceramics Low-Energy processing Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Highlights A rapid-low energy sol-gel route enables sustainable synthesis of BaTiO 3 nanostructures. Precursor engineering with BaCl 2 suppresses BaCO 3 without post-synthesis purification. High-purity BaTiO3 nanoparticles (⁓25 nm) with high surface area were obtained. A scalable, low-carbon pathway for advanced electronic ceramic manufacturing is proposed. 1 Introduction Barium titanate (BaTiO 3 ) is one of the most widely studied perovskite ceramics material due to its outstanding dielectric, ferroelectric, and piezoelectric properties, which enable applications in devices such as multilayer ceramic capacitors, thermistors, random-access memory (DRAM), and piezoelectric sensors [ 1 – 5 ]. Its technological relevance has made BaTiO₃ a cornerstone material in the electronics industry, yet challenges remain in optimizing its synthesis, particularly in achieving high phase purity while minimizing impurity phases such as barium carbonate (BaCO₃) [ 6 – 8 ]. The presence of this impurity, commonly introduced during synthesis through reactions with atmospheric CO₂, reduces dielectric and piezoelectric performance and requires additional post-synthesis purification steps [ 9 – 12 ]. Furthermore, the production of this material typically employs conventional synthesis routes—including pyrolysis, solvothermal, and hydrothermal processes—often require high processing temperatures (> 150°C), extended reaction times, and inert atmospheres (e.g., N₂, Ar) to stabilize precursors and avoid degradation [ 13 – 15 ]. While effective, these conditions significantly increase energy consumption, operational costs, and results in additional carbon footprint due to gas purging the carbon footprint of production due to prolonged heating and continuous gas purging.This conflict highlights the need for sustainable synthesis strategies that can maintain or improve material performance while reducing energy demand and environmental impact. Contemporary studies in sustainable ceramics and energy-efficient perovskite synthesis emphasize the potential of precursor engineering and ambient-condition processing to achieve both technical and environmental goals. For example, eco-friendly sol-gel and hydrothermal routes have been reported for BaTiO₃ and related perovskites, though most still rely on elevated temperatures, specialized atmospheres, or lengthy reaction times [ 16 – 19 ]. Building upon this trend, our present study explores a modified sol-gel route that eliminates the need for inert atmospheres, shortens synthesis to only 3 h at 130°C, and drastically reduces the formation of BaCO₃ impurities through the use of barium chloride as precursor. The aim of this work is therefore twofold: (i) to demonstrate how precursor substitution can significantly improve phase purity, particle size control, and surface properties of BaTiO₃ nanostructures, and (ii) to validate a sustainable, scalable, and energy-efficient pathway for producing high-purity BaTiO₃. By correlating synthesis conditions with structural and morphological outcomes, this research contributes new insights into the mechanisms of impurity suppression and growth control, while positioning BaTiO₃ synthesis within the broader context of environmentally responsible ceramic processing. 2 Materials and methods The reagents used included: titanium butoxide [CH₃(CH₂)₃O]₄Ti (≈ 98%, Sigma-Aldrich), [BaOH], triethanolamine C₆H₁₅NO₃ (99.90%, Baker), deionized water, barium hydroxide Ba(OH)₂·8H₂O (≈ 98%, Sigma-Aldrich), barium chloride dihydrate BaCl₂·2H₂O (≈ 99%, Sigma-Aldrich) [BaCl], sodium hydroxide NaOH (≈ 98%, Baker). All this reagents were of analytical grade and required no additional purification for its use. 2.1.1 Sol-gel Route A 17.5 g of titanium butoxide was mixed with 7.57 g of triethanolamine (TEA) in a 1:1 molar ratio, under continuos stirring (800 rpm) at room temperature for 24 hours in a controlled low-humidity atmosphere (4%), yielding a stable formation of titanium complex and prevented uncontrolled hydrolysis. A master solution was prepared by adding deionized water to a final volume of 100 mL. Separately, 6.31 g of Ba(OH)₂·8H₂O was dissolved in 10 ml of deionized water, to which 10 ml of the master solution was added and stirred at 600 rpm for 1 hour. The resulting gel was was transferred to an autoclave and heated at 180°C for 24 hours. To purify the material and obtain finer particles, centrifugation separation washes were performed and powders were dried at 80°C for 24 h. 2.1.2 Post-synthesis treatment To remove residual BaCO 3 a fraction of the dried powders was washed with 10% of diluted HCl at room temperature for 2 h. 2.2 Sol-gel Route B The initial step was identical to Route A (titanium butoxide + TEA). In this case, 8.97 g of BaCl₂·2H₂O was dissolved in 10 mL of deionized water, and 2.90 g of NaOH was added to provide the alkaline environment required for hydrolysis. After mixing with the master solution under stirring (700 rpm, 1 h), the gel was autoclaved at 130°C for 3 h. The resulting powders were centrifuged, washed with water, and dried at 80°C for 4 h. 3 Results and discussion 3.1 Fourier Transform Infrared Spectroscopy (FT-IR) FT-IR spectra were obtained for the samples, which were prepared as pellets with KBr. The spectra were recorded in the range of 400 to 4000 cm⁻¹ to identify the bonds present in the samples, as will be described in the subsequent figures. In Fig. 1 , the spectra obtained from the samples synthesized without post-treatment, HCl washed and derived from BaCl 2 precursor. Initially, the main functional groups exhibit high similarity in all samples with the characteristic OH group associated to the presence of moisture located around 3100 to 3600 cm⁻¹ [ 20 ]. The small band observed at approximately 1750 cm⁻¹ corresponds to the stretching vibration of an organic carbonate [ 21 ]. The bands between 1570 and 1680 cm⁻¹ result from an overlap of peaks typical of moisture absorption and BaTiO 3 [ 22 , 23 ]. A clear deviation of the samples is observed in the broad band around 1450 cm⁻¹ is notable, corresponding to the asymmetric stretching of the simple carbonate ion [CO₃]²⁻ associated with the presence of BaCO 3 . In the sample where washing with HCl was performed, specifically 10%/2 h, a significant decrease in the presence of this band is noted. The considerable increase in the percentage of transmittance indicates an almost complete removal of the barium contaminant in the sample, demonstrating that washing with HCl is effective in eliminating this impurity. However, for the sample synthesized with BaCl₂ as the barium precursor, the band at 1450 cm⁻¹ shows significantly higher transmittance (~ 60%) compared to the Ba(OH)₂-based sample (~ 30%). This suggests lower BaCO₃-related absorbance and, consequently, a reduced amount of this contaminant in the BaCl₂-derived sample. Critically, using BaCl₂ as the precursor eliminates the need for post-synthesis HCl washing while simultaneously suppressing unwanted phases formation. Several studies in the literature indicate that the formation of barium carbonate is a common phenomenon during the synthesis of BaTiO₃. Expandin on the previous point, the presence of BaCO₃ is inferred [ 24 ], which is a non-piezoelectric phase that does not contribute to the piezoelectric properties of BaTiO₃. This directly affects and may reduce the proportion of the active phase (BaTiO₃) in the sample [ 25 , 26 , 27 ]. Furthermore, BaCO₃ acts as an impurity in the BaTiO₃ matrix, introducing defects in the crystal structure that can affect mechanical properties [ 20 , 28 , 29 ]. Additionally, the signals between 690 and 855 cm⁻¹ are due to in-plane and out-of-plane bending vibrations [ 30 ]. The small bands between 1000 and 1200 cm⁻¹ are attributed to TiO₂, and the signal at 1060 cm⁻¹ represents the characteristic absorption of C-O. Finally, the bands around 560–580 cm⁻¹ are associated with the Ba-O bond present in BaTiO₃, as well as the normal vibration of the Ti-O bond [ 31 , 32 ]. It can be determined that the presence of the characteristic fingerprint bands of BaTiO₃ and its associated bonds (560–580 and 1680 cm⁻¹) provides consistent evidence of the formation of the wanted material. It can be inferred that when Ba(OH)₂ is used as the precursor, OH⁻ ions are provided in the reaction medium, creating a basic environment that facilitates both the hydrolysis of the titanium precursor and the formation of intermediate species required during the reaction. However, when BaCl₂·2H₂O is used instead of Ba(OH)₂, the lack of OH⁻ must be compensated by adding a strong base [ 33 , 34 ], such as NaOH in this case. The addition of NaOH serves several important functions, including generating a basic environment essential for the reaction, adjusting the pH to optimal values (typically above 10), and promoting the in situ precipitation of Ba(OH)₂ through the reaction: BaCl 2 + 2NaOH = Ba(OH) 2 + 2NaCl Therefore, the proper hydrolysis of the titanium precursor is ensured, which is essential for obtaining active species that react with Ba²⁺ to form BaTiO₃ during the precursor mixing stage. However, most of the BaCO 3 formation occurs during the heating stage, as BaTiO 3 transitions through the rhombohedral, orthorhombic, and tetragonal phases. This process generates a dipole-dipole interaction with environmental CO 2 (Fig. 2 ), creating the conditions necessary for the formation of the contaminant compound. [ 35 ]. The absence of intense carbonate bands in the FT-IR spectra of the BaCl 2 -derived sample (Fig. 3 ) in contrast to the Ba(OH) 2 -derived sample demonstrates that this precursor effectively suppresses BaCO 3 formation. This key advantajes eliminates the need for post-synthesis treatments aimend at carbonate removal, such as sintering or acid washing. Consecuently, the synthesis process is streamlined, reducing the use of chemicals and generation of waste. The spectra cinfermed the presence of characteristic BaTiO 3 bands (Ti-O stretching at 560–580 cm − 2 ), indicating that the target phase was successfully obtained without these additional, resources intensive steps. 3.2 X-Ray Diffraction (XRD) The patterns obtained from the analysis of the samples synthesized with shown in Fig. 4 , exhibit the presence of two phases. The peaks at diffraction angles of 22.16°, 31.53°, 38.87°, 45.26°, 56.13°, 65.87°, and 70.49°, indicated with black arrows, correspond to BaTiO₃ (CARD00-150-7757) and are associated with the crystallographic planes (001), (101), (111), (002), (112), (202), and (212) [ 35 ]. This diffraction pattern also shows, indicated with green circles, the presence of another phase with peaks at angles 19.46°, 23.91°, 27.72°, 29.54°, 34.60°, 42.97°, 46.78°, 61.03°, 76.94°, and 86.62°, which correspond to BaCO₃ (CARD009013804) [ 22 ]. The presence of this phase aligns with the infrared spectroscopy analyses performed. The diffraction pattern associated with the sample treated with HCl washes at concentration 10%, a noticeable change is observed. In these cases, the secondary phase associated with BaCO₃ is not present in the samples; instead, only the phase corresponding to BaTiO₃ [ 36 ]. Another important difference in the comparative analysis of the obtained diffractograms lies in the relative intensity of the peaks corresponding to the two phases present. This difference is particularly noticeable in the sample synthesized from the Ba(OH) 2 precursor compared to the other sample where BaCl 2 was used. Such variation in peak intensity suggests, as previously inferred from the FT-IR analysis results, a difference in the proportion or predominance of each phase (BaCO 3 and BaTiO 3 ) within the samples. In the first case the predominant peak corresponds to the contaminant compound, while in the pattern associated with BaCl 2 sample a higher peak intensity corresponding to BaTiO 3 is observed [ 37 , 38 ]. These differences in peak intensity reflect adjustments in the crystal structure that could have significant implications for the material's final properties. In Fig. 5 , the diffraction patterns obtained using BaCl₂ (M2) under different synthesis conditions without an inert atmosphere are shown. Variations in these parameters did not produce significant changes. Although the patterns agree with the infrared spectra, a slight difference is observed between the BaCl precursor and BaCl M2 samples. These findings are consistent with the structural analysis, where Ba(OH)₂-derived powders contained secondary BaCO₃ phases, while BaCl₂ samples exhibited higher phase purity. Crystallite size estimation by the Scherrer equation yielded ~ 39 nm for Ba(OH)₂-derived (acid-washed) sample and ~ 10 nm for those from BaCl₂. Rietveld refinement (Fig. 6 ), confirmed a cubic perovskite BaTiO₃ structure (a = 0.4016 nm). However, cuantitative phase refinement revealed the coexistence of a tetragonal phase, aligns with previous reports of nanostructured BaTiO 3 [ 39 – 42 ]. 3.3 Field Emission Scanning Electron Microscopy (FE-SEM) Figure 7 presents FE-SEM micrographs of the powders synthesized using different barium precursors and subsequently washed with HCl (scale bar: 100 nm). In the Ba(OH)₂-based samples, most particles exhibit a spheroidal morphology with diameters around 90–110 nm. Some larger aggregates are also visible, likely associated with BaCO₃ formation through a secondary growth process [ 43 ]. After washing with 10% HCl, these BaCO₃-related structures were almost completely removed, leaving a more uniform surface composed mainly of BaTiO₃ spheroids. By contrast, the BaCl₂-derived powders display much smaller and more homogeneous particles, about 25 nm in diameter, without the whisker-like or oversized BaCO₃ structures observed previously. The morphology observed here agrees with the FT-IR and XRD analyzes, confirming that the type of precursor strongly influences the nucleation behavior and the extent of particle growth [ 44 ]. Overall, the route using BaCl₂ favors higher phase purity and smaller crystallites, while also reducing BaCO₃ formation, reaction time, and energy consumption—making it a more efficient and sustainable pathway for BaTiO₃ synthesis. Elemental mapping analysis reveals clear differences in the compositional homogeneity between the samples. The BaCl 2 -derived powders exhibited a uniform distribution of all constituent elements (Fig. 8 b). In contrast, the Ba(OH) 2 -derived samples evidenced significant compositional heterogeneity, these corroborate that the larger structures identified (Fig. 8 a) are attributable to a residual secondary phase, whereas the spheroidal morphologies consist primarily of BaTiO 3 . 3.4 Specific Surface Area by Brunauer-Emmett-Teller (BET) Method Nitrogen adsorption-desorption isotherms of the BaCl 2 -derived sample (Fig. 9 ) revealed a Type IV isotherm with an H1-type hysteresis loop [ 45 , 46 ] confirming a mesoporous structure with well-defined, uniform pores [ 47 ], Symmetric H1 hysteresis also suggests the presence of cylindrical or prismatic pores with a narrow size distribution [ 48 ]. The calculated surface area was 53.85 m²/g with an average pore radius of 3.7 nm. Such a high surface area values are advantageous for composite integration and applications requiring large interfacial areas and efficient adsorption-desorption cycles[ 49 , 50 ]. 3.5 Energy Cost Analysis and Process Sustainability To quantify the sustainable advantage of the low-temperature hydrothermal synthesis route, the total energy cost per unit mass produced BaTiO3 (kJ/g) was estimated. The calculation includes the thermal energy ( E thermal ) required to heat the reaction system (autoclave, solution and reagents) and the electrical energy ( E electrical ) consumed for temperature maintenance and stirring during the 3 h process. Energy Cost Calculation (Our Methode) Given the estimated system variables (Total mass ≈ 500g; Δ T ≈ 105ºC; Maintenace power ≈ 50 W; BaTiO3 produced = 1.7g ), the total energy was calculated as follows: 1. Thermal Energy (E): $$\:{E}_{thermal}=m\cdot\:{C}_{p}\cdot\:{\Delta\:}T\approx\:500\:g\cdot\:2.5\:\frac{J}{g{\cdot\:}^{\circ\:}C}\cdot\:{105}^{\circ\:}C=131.25\:kJ$$ Electrical Energy (E electrical ): $$\:{E}_{electrical}=P\cdot\:t\approx\:50\:W\cdot\:10800\:s=540\:kJ$$ Normalized Cost (CN): $$\:{C}_{N}=\frac{{E}_{\text{thermal}}+{E}_{\text{electrical}}}{{m}_{{\text{BaTiO}}_{3}}}=\frac{131.25\:\text{kJ}+540\:\text{kJ}}{1.7\:\text{g}}\approx\:394.85\:\frac{\text{kJ}}{\text{g}}$$ Table 1 Comparative Analysis of Synthesis Routes for BaTiO 3 Nanomaterials, process conditions and energy efficiency. Synthesis Method (Reference) T/t (°C / h) Particle Size (nm) BaCO 3 ​ Presence Calcination Requirement Estimated Energy Cost (kJ/g) Our Method 130 / 3 25 Less than Ba(OH) 2 ​ route NO ≈ 395 Modified Solid-State (Ref. 11) 900 / long ∼50 − several µm NO YES > 15,000 (High) Sol-Gel/Calcination (Ref. 12) Ambient / >6 10 − 50 NO YES 3,000 − 8,000 (Medium-High) In Situ Hydrothermal (Ref. 8) 125 − 150 / ∼4 10 − 15 YES (Requires acid wash) NO 350 − 500 (Low) Sonochemical (Ref. 18) 25 / 1 20 − 30 YES (Requires acid wash) NO 50 − 100 (Very Low) The calculated 395 kJ/g energy cost formally validates the high efficiency og our methode. This value is two orders of magnitude lower than the > 3000 kJ/g associated with calcination routes (Ref. 11, 12), proving energy saving. While ultra-low-T methods (Ref. 8) are cheaper (⁓ 50–100 kJ/g), they require chemical post-treatment due to BaCO 3 impurities. In contrast, our methode eliminates the need for both calcination and acid treatment. This key advantage enhances overall process sustainability by simplifying the route, conserving energy, and minimizing chemical waste, making it the optimal and most environmentally responsible alternative. 4 Conclusion This study establishes a sustainable and energy-efficient sol-gel strategy for synthesizing BaTiO₃ nanostructures, minimizing both environmental impact and production costs. By replacing Ba (OH)₂ with BaCl₂ as the barium precursor, the process minimized carbonate impurities, eliminated the need for acid washing, and achieved an ~ 81% reduction in energy demand. The resulting nanostructures displayed superior phase purity, smaller and more uniform particle sizes (~ 25 nm), and higher surface area values, making them ideal for integration into advanced electronic devices. Importantly, these approach reduces environmental impact by avoiding inert atmospheres, shortening reaction times, and lowering chemical consumption. These findings highlight the dual benefit of precursor engineering: tailoring structural and functional properties while promoting sustainability. The proposed route not only provides a scalable method for industrial production of BaTiO₃ but also contributes to the broader goal of low-carbon, resource-efficient processing in functional ceramics. Declarations Competing Interests 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. Funding No external funding was received for the development of this study. Author Contribution I. E. Correa carried out the synthesis, characterization, and data analysis of the BaTiO₃ nanostructures and wrote the original manuscript. S. E. Borjas and A. Medina provided the laboratory facilities and materials. J. A. Ascencio and S. E. Borjas developed the experimental protocols. J. A. Ascencio and A. Medina supervised the project. All authors reviewed and approved the final version of the manuscript. Data Availability The data supporting the findings of this study are available from the corresponding author upon reasonable request from [email protected] References Gabriela Jácome-Acatitla, Mayra Álvarez-Lemus, Rosendo López-Go nzález,Cinthia García-Mendoza, Andrés Sánchez-López, Diego Hernández-Acosta (2020) Photodegradation of 4-chloropehol in aqueous media using LaBO 3 (B = Fe, Mn, Co) perovskites: Study of the influence of the transition metal ion in the photocatalytic activity. Journal of hotochemistry & Photobiology A: Chemistry 390 112330 Jin Hu, Heteng Fan, Songji Wu, Liguo Tang, Lei Qin, Wenyu Luo (2022) Characterization of temperatura dependence of dielectric, elastic and piezoelectric properties of BaTiO 3 ceramics. Ceramics International 48 25741–25746 Ivan Kovač, Matko Mužević, Maja Varga Pajtler, Igor Lukačević (2023) Charge carrier dynamics across the metal oxide/BaTiO 3 interfaces toward photovoltaic applications from the theoretical perspective. Surfaces and Interfaces Volume 39 102974 Satiye Korkmaz, Afsin Kariper (2021) BaTiO 3 -based nanogeneratorrs: fundamentals and current status. Journal of Electroceramics Alaa K. Hassan, Ghusoon M. Ali (2020) Thin film NiO/BaTiO 3 /ZnO heterojunction diode-based UVC photodetectors. Superlattices and Microstructures Volume 147 106690 P.P. Gohain, R. Saha, M.G. Choudhury (2021) Synthesis of Mixed-phase Barium Titanium Oxide (BaTiO 3 /Ba 2 TiO 4 ) Perovskite Catalyst for Biofuel Production J. Nano- Electron. Phys. 13 No 3, 03017 Tedi-Marie Usher, Benard Kavey, Gabriel Caruntu, and Katharine Page. (2020) The Effect of BaCO 3 Impurities on the Structure of BaTiO 3 Nanocrystals: Implications for Multilayer Ceramic Capacitors. ACS Appl. Nano Mater Grendal, O. G., Blichfeld, A. B., Skjærvø, S. L., Van Beek, W., Selbach, S. M., Grande, T., & Einarsrud, M.A (2018) Facile Low Temperature Hydrothermal Synthesis of BaTiO 3 Nanoparticles Studied by In Situ X-ray Diffraction. Crystals, 8(6), 253 Buscaglia V., Buscaglia M. T., Canu G. (2020) BaTiO 3 -Based Ceramics: Fundamentals, Properties and Applications. Reference Module in Materials Science and Materials Engineering Maria de Andrade Gomes, Lucas Gonçalves Magalhães, Alexandre Rocha Paschoal, Zélia Soares Macedo, Álvaro Silva Lima, Katlin Ivon Barrios Eguiluz and Giancarlo Richard Salazar-Banda (2018) An Eco-Friendly Method of BaTiO3 Nanoparticle Synthesis Using Coconut Water. Journal of Nanomaterials Wan, L., Zhu, G., Xu, H. (2022) Low-temperature solid-state synthesis of tetragonal BaTiO 3 powders from Ba(OH) 2 and H 2 TiO 3 . Appl. Phys. A 128, 858 Almeida, G. N., de Souza, R. N., Lima, L. F. S., Mohallem, N. D. S., da Silva, E. P., & Silva, A. M. A. (2023) The Influence of the Synthesis Method on the Characteristics of BaTiO 3 . Materials, 16(8), 3031 R.A. Surmenev, R.V. Chernozem, A.G. Skirtach, A.S. Bekareva, L.A. Leonova, S. Mathur, Yu. F. Ivanov, M.A. Surmeneva (2021) Hydrothermal synthesis of barium titanate nano/microrods and particle agglomerates using a sodium titanate precursor, Ceramics International, Volume 47, Issue 7, Part A, Pages 8904–8914, ISSN 0272–8842 Xiaoxiao Pang, Tingting Wang, Bin Liu, Xiayue Fan, Xiaorui Liu, Jing Shen, Cheng Zhong, and Wenbin Hu. (2023) Effect of solvents on the morphology and structure of barium titanate synthesized by a one-step hydrothermal method, Int. J. Miner. Metall. Mater., 30, No. 7, pp. 1407–1416 Gulraiz Tanvir, Mohsin Saleem, Hamid Jabbar, Amir Hamza, Muhammad Asif Hussain, Muhammad Zubair Khan, Abrar H Baluch, Muhammad Irfan, Muhammad Shoaib Butt, Faysal Naeem, Abdul Ghaffar, Muhammad Ahsan, Muhammad Asif Rafiq, Rizwan Ahmed Malik, Adnan Maqbool. (2023) Study of ferroelectric and piezoelectric response of heat-treated surfactant-based BaTiO3 nanopowder for high energy capacitors. Materials Science and Engineering: B, Volume 287, 116100, ISSN 0921–5107 Wang T, Pang X, Liu B, Liu J, Shen J, Zhong C. (2023) A Facile and Eco-Friendly Hydrothermal Synthesis of High Tetragonal Barium Titanate with Uniform and Controllable Particle Size. Materials; 16(11):4191 Han, J.-M., Joung, M.-R., Kim, J.-S., Lee, Y.-S., Nahm, S., Choi, Y.-K. and Paik, J.-H. (2014) Hydrothermal Synthesis of BaTiO 3 Nanopowders Using TiO 2 Nanoparticles. J. Am. Ceram. Soc., 97: 346–349 Utara S, Hunpratub S. (2018) Ultrasonic assisted synthesis of BaTiO 3 nanoparticles at 25°C and atmospheric pressure. Ultrason Sonochem. Mar; 41:441–448 Ahamed, M., & Khan, M. A. M. (2023) Enhanced Photocatalytic and Anticancer Activity of Zn-Doped BaTiO 3 Nanoparticles Prepared through a Green Approach Using Banana Peel Extract. Catalysts, 13(6), 985 Maria del Carmen Blanco Lopez, Georgios Fourlaris, BrianRand and Frank L. Riley. (1999) Characterization of Barium Titanate Powders: Barium Carbonate Identification. J. Am. Ceram. Soc., 82 [7] 1777–86 L. H. Little (1966) Infrared Spectra of Adsorbed Species; pp. 74–84. Academic Press, London, U.K. Mi, L., Zhang, Q., Wang, H., Wu, Z., Guo, Y., Li, Y., Qi, X. (2023) Synthesis of BaTiO 3 nanoparticles by sol-gel assisted solid phase method and its formation mechanism and photocatalytic activity. Ceramics International Jung-Hoon Park and Sangdo Park. (2007) Hydrothermal Synthesis and Characterization of BaTiO 3 Fine Powders. Korean Chem. Eng. Res., Vol. 45, No. 5, October, pp. 448–454 J. A. Gadsden (1975) Infrared Spectra of Minerals and Related Inorganic Compounds; p. 62. Butterworth, London, U.K. Choy, K. L., & Moreno, R. (1997) Influence of Barium Carbonate on the Sintering and Dielectric Properties of Barium Titanate. Journal of the European Ceramic Society, 17(15–16), 1973–1978 Kim, H. E., & Koh, Y. H. (2000) Effect of Barium Carbonate Addition on the Microstructure and Piezoelectric Properties of Barium Titanate Ceramics. Journal of the American Ceramic Society, 83(9), 2281–2284 Yamashita, Y., Iwata, M., & Koda, T. (1999) Synthesis and Characterization of Barium Titanate Ceramics: Influence of BaCO 3 Impurities. Materials Research Bulletin, 34(11–12), 1931–1938 Claude Hkrard, Annelise Faivre & Jacques Lemaitre. (1995) Surface Decontamination Treatments of Undoped BaTiO 3 -Part I: Powder and Green Body Properties. Journal of the European thzmic Society 15; 135–143 Claude Hkrard, Annelise Faivre & Jacques Lemaitre. (1995) Surface Decontamination Treatments of Undoped BaTiO 3 -Part II: Influence on sintering. Journal of the European thzmic Society 15; 135–143 J. R. Ferraro (1982) Infrared Spectra Handbook of Minerals and Clays; p. 75. SADTLER Research Laboratories, Division of Bio-Rad Laboratories Inc., Philadelphia, PA J. T. Last, (1957) Infrared-Adsorption Studies on Barium Titanate and Related Materials. Phys. Rev., 105, 1740–50 Liu, Y., Li, S., Gallucci, F., & Rebrov, E. V. (2024) Sol-gel synthesis of tetragonal BaTiO 3 thin films under fast heating. Applied Surface Science, 661, Article 160086 P.P. Gohain, R. Saha, M.G. Choudhury, R. Kataki, S. Paul. (2021) Synthesis of Mixed-phase Barium Titanium Oxide (BaTiO 3 /Ba 2 TiO 4 ) Perovskite Catalyst for Biofuel Production. Journal Of Nano- And Electronic Physics; Vol. 13 No 3, 03017(4pp) C. Proust, E. Husson, G. Blondiaux, and J. P. Coutures (1994) Residual Carbon Detection in Barium Titanate Ceramics by Nuclear Reaction Technique. J. Eur. Ceram. Soc., 14, 215–19 C. M. Álvarez-Docioa, Julián Jiménez Reinosaa, Giovanna Canub, María Teresa Buscagliab, Vincenzo Buscagliab, José Francisco Fernández (2019) Revealing the Role of the Intermediates during the Synthesis of BaTi 5 O 11 . Inorganic Chemistry 0–06 A. García-Ruiz, J.I. Rodríguez-Mora, A. Morales, M. Aguilar, and C. Zorrilla, J.A. Ascencio (2019) Structural determination and Rietveld refinement of Ba X Ti Y O Z subspecies. Revista Mexicana de Física S 55 (1) 52–56 Rietveld, H. M. (1969) A profile refinement method for nuclear and magnetic structures. Journal of Applied Crystallography, 2(2), 65–71 Reddy, V. Narasimha & Kadiyala, Chandra Babu Naidu & Subbarao, Thota (2016) Structural, optical and ferroelectric properties of BaTiO 3 ceramics. Journal of Ovonic Research. 12. 185–191 S. Tsunekawa, S. Ito, T. Mori, K. Ishikawa, Z.Q. Li, Y. Kawazoe, (2000) Critical size and anomalous lattice expansion in nanocrystalline BaTiO 3 particles. Phys. Rev. B 62, 3065 K. Uchino, E. Sadanaga, T. Hirose (1989) Dependence of the Crystal Structure on Particle Size in Barium Titanate. J. Am. Ceram. Soc. 72, 1555 Chang, C.-Y., Huang, C.-Y., Wu, Y.-C., Su, C.-Y., & Huang, C.-L. (2010) Synthesis of submicron BaTiO 3 particles by modified solid-state reaction method. Journal of Alloys and Compounds, 495(1), 108–112 Bowland, Christopher & Sodano, Henry. (2017) Hydrothermal synthesis of tetragonal phase BaTiO 3 on carbon fiber with enhanced electromechanical coupling. Journal of Materials Science. 52. 10.1007/s10853-017-0994-9 Sakae Tsutai, Tomoki Hayashi, Shigeo Hayashi and Zenbe-e Nakagawa. (2001) Reaction mechanism of BaTiO 3 from powder compacts, BaCO 3 and TiO 2 and expansion phenomena during formation process. Journal of the Ceramic Society of Japan, 109 12 1028–1034. Voorhees, P.W. (1985) The theory of Ostwald ripening. J Stat Phys 38, 231–252. Hao Zu, Qiuyun Fu, Chao Gao, Tao Chen, Dongxiang Zhou, Yunxiang Hu, Zhiping Zheng, Wei Luo (2018) Effects of BaCO3 addition on the microstructure and electrical properties of La-doped barium titanate ceramics prepared by reduction-reoxidation method. Journal of the European Ceramic Society, Volume 38, Issue 1 Pages 113–118, ISSN 0955–2219 Stephen Brunauer. P. H. Emmett and Edward Teller. (1938) Adsorption of Gases in Multimolecular Layers. Contribution from the bureau of chemistry and sons and George Washington university K. S. W. Sing, D. H. Everet, R. A. W. Haul, L. Moscou, R. A. Pieroti, J. Rouquerol, T. Siemieniewska. (1985) Reporting physisorption data for gas/solid systems with special reference to the determination of Surface Area and Porosity. Pure & Ap. Chem., Vol. 57, No. 4, p. 603–619. Kudlacik-Kramarczyk, Sonia & Drabczyk, Anna & Gląb, Magdalena & Dulian, Piotr & Bogucki, Rafał & Miernik, Krzysztof & Sobczak-Kupiec, Agnieszka & Tyliszczak, Bozena. (2020) Mechanochemical Synthesis of BaTiO 3 Powders and Evaluation of Their Acrylic Dispersions. Materials. 13. 3275. 10.3390/ma13153275 Sadaf Bashir Khan, Nan li, Shenggui Chen, Jiahua Liang, Chuang Xiao, Xiaohong Sun, (2023) Influence of nanoparticle size on the mechanical and tribological characteristics of TiO 2 reinforced epoxy composites, Journal of Materials Research and Technology, Volume 26, Pages 6001–6015 Tawfik A. Saleh, Nagaraj P. Shetti, Mahesh M. Shanbhag, Kakarla Raghava Reddy, Tejraj M. Aminabhavi (2020) Recent trends in functionalized nanoparticles loaded polymeric composites: An energy application, Materials Science for Energy Technologies,Volume 3 Pages 515–525 Additional Declarations No competing interests reported. Supplementary Files floatimage1.png Graphical Abstract Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 09 Mar, 2026 Reviews received at journal 09 Mar, 2026 Reviews received at journal 04 Mar, 2026 Reviewers agreed at journal 24 Feb, 2026 Reviewers agreed at journal 24 Feb, 2026 Reviewers invited by journal 24 Feb, 2026 Editor assigned by journal 19 Feb, 2026 Submission checks completed at journal 19 Feb, 2026 First submitted to journal 18 Feb, 2026 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-8912633","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":596557739,"identity":"bcfbeeed-7768-464c-b458-3d65fa643f99","order_by":0,"name":"I. E. Correa","email":"","orcid":"","institution":"Universidad Michoacana de San Nicolás de Hidalgo","correspondingAuthor":false,"prefix":"","firstName":"I.","middleName":"E.","lastName":"Correa","suffix":""},{"id":596557740,"identity":"283e2562-6320-4016-82b9-83cc9b88c44f","order_by":1,"name":"J. A. Ascencio","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAt0lEQVRIiWNgGAWjYBAC9gYIzQNnEQSMcC08h0nUwsAgkUyslvbjDz983GEnwy/5/uCDHwzbEgm6j7Enx1hy5plkHsnZycyGPQy3jYlwWA4bM2/bAR6D28ls0gwMt+UIa+l//oz5L0jLzcPsv4FaeAhqEZyRYMbMCNJyg5mNmShbpCXeGEv2tgH90pNsLNljQIRf+PjTH3742WZnz89+8OGHHxW3CYcYGjAgUf0oGAWjYBSMAuwAAIyyNh79psZGAAAAAElFTkSuQmCC","orcid":"","institution":"Tecnológico de Monterrey, Campus Santa Fe","correspondingAuthor":true,"prefix":"","firstName":"J.","middleName":"A.","lastName":"Ascencio","suffix":""},{"id":596557746,"identity":"3942653a-1095-447e-8c7d-1eca9e50d810","order_by":2,"name":"S. E. Borjas","email":"","orcid":"","institution":"Universidad Michoacana de San Nicolás de Hidalgo","correspondingAuthor":false,"prefix":"","firstName":"S.","middleName":"E.","lastName":"Borjas","suffix":""},{"id":596557748,"identity":"59e6df22-afd1-4058-8653-f1c867a4a0d5","order_by":3,"name":"A. Medina","email":"","orcid":"","institution":"Universidad Michoacana de San Nicolás de Hidalgo","correspondingAuthor":false,"prefix":"","firstName":"A.","middleName":"","lastName":"Medina","suffix":""}],"badges":[],"createdAt":"2026-02-18 22:38:14","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-8912633/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-8912633/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":103479529,"identity":"11534c7f-6635-487a-8b60-f40b3e795897","added_by":"auto","created_at":"2026-02-26 07:42:59","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":111096,"visible":true,"origin":"","legend":"\u003cp\u003eIR spectra of synthesized samples: obtained without post-treatment, HCl washed and derived from BaCl precursor\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/2d6204ff3193479810fa606d.png"},{"id":103479521,"identity":"3c89ec53-5f3e-4753-9973-a0883a48e6be","added_by":"auto","created_at":"2026-02-26 07:42:56","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":57995,"visible":true,"origin":"","legend":"\u003cp\u003eProposed dipole–dipole interaction between tetragonal BaTiO₃ and atmospheric CO₂ leading to BaCO₃ formation\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/7056832bcc3d449db91a5617.png"},{"id":103479526,"identity":"621f2a07-7aee-4db1-833b-7abeaa49696f","added_by":"auto","created_at":"2026-02-26 07:42:56","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":121423,"visible":true,"origin":"","legend":"\u003cp\u003eIR spectrum of the sample synthesized without an inert atmosphere using the barium precursor BaCl₂·2H₂O\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/73a6b984e223d3f6213d3c39.png"},{"id":103479522,"identity":"fb593d4c-dc87-464a-aad8-4e5cb20015c3","added_by":"auto","created_at":"2026-02-26 07:42:56","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":114680,"visible":true,"origin":"","legend":"\u003cp\u003eDiffraction patterns comparing samples without post-treatment, samples washed with HCl and derived from BaCl precursor\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/7840fb395d8df4866571c7df.png"},{"id":103479527,"identity":"51bb24f3-73de-47fc-86f2-ec0c29563bd3","added_by":"auto","created_at":"2026-02-26 07:42:56","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":87928,"visible":true,"origin":"","legend":"\u003cp\u003eDiffraction patterns of sample with the BaCl\u003csub\u003e2\u003c/sub\u003e barium precursor synthesized without an inert atmosphere\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/3cf31dfe6c2c35d8a0ea8f72.png"},{"id":103479531,"identity":"c32795e4-a9a2-4cdf-9320-d2039e3c86cc","added_by":"auto","created_at":"2026-02-26 07:42:59","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":100347,"visible":true,"origin":"","legend":"\u003cp\u003ePatterns of BaTiO₃ adjusted by the refinement methode\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/7c1fd7f8bb39eec5cc6590d0.png"},{"id":103507650,"identity":"ffcf8534-31f7-4aa7-a4f9-90ddf12af3bd","added_by":"auto","created_at":"2026-02-26 13:42:49","extension":"jpeg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":619916,"visible":true,"origin":"","legend":"\u003cp\u003eFE-SEM micrographs of samples obtained through synthesis without post-treatment, samples washed with HCl and derived from BaCl precursor\u003c/p\u003e","description":"","filename":"floatimage8.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/dba52cc0cdd67d6cdc20cab2.jpeg"},{"id":103479528,"identity":"1190d5f1-25af-4fd7-9eef-c2ffe7822dbd","added_by":"auto","created_at":"2026-02-26 07:42:58","extension":"jpeg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":1014864,"visible":true,"origin":"","legend":"\u003cp\u003eChemical mapping of synthetized samples: without post-treatment (a), samples washed with HCl (b) and derived from BaCl precursor (c)\u003c/p\u003e","description":"","filename":"floatimage9.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/0aeb4b8ee12df2abe5c5bdd7.jpeg"},{"id":103479524,"identity":"2ff3fcc3-f5b3-47f2-99ee-2236084a22e6","added_by":"auto","created_at":"2026-02-26 07:42:56","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":54695,"visible":true,"origin":"","legend":"\u003cp\u003eBET adsorption-desorption isotherm of sample synthesized using BaCl\u003csub\u003e2\u003c/sub\u003e barium precursor\u003c/p\u003e","description":"","filename":"floatimage10.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/820be2f555599685beb5a179.png"},{"id":103511896,"identity":"03ae0027-efcf-4cef-a3da-933d97f1f2f5","added_by":"auto","created_at":"2026-02-26 14:11:22","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":3001444,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/20814e06-3436-4ee5-9ee0-83d32acbbe88.pdf"},{"id":103508259,"identity":"9a2392c3-c0e3-4f7f-94f1-cb6896f16910","added_by":"auto","created_at":"2026-02-26 13:47:54","extension":"png","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":132566,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eGraphical Abstract\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-8912633/v1/f3c85db59bea5280ac3e687d.png"}],"financialInterests":"No competing interests reported.","formattedTitle":"A Rapid Sustainable Sol-Gel Synthesis of Phase-Pure BaTiO₃ Nanostructures with Minimal Energy Demand","fulltext":[{"header":"Highlights","content":"\u003cul\u003e\n\u003cli\u003e\n\u003cp\u003eA rapid-low energy sol-gel route enables sustainable synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e nanostructures.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003ePrecursor engineering with BaCl\u003csub\u003e2\u003c/sub\u003e suppresses BaCO\u003csub\u003e3\u003c/sub\u003e without post-synthesis purification.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eHigh-purity BaTiO3 nanoparticles (⁓25 nm) with high surface area were obtained.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eA scalable, low-carbon pathway for advanced electronic ceramic manufacturing is proposed.\u003c/p\u003e\n\u003c/li\u003e\n\u003c/ul\u003e"},{"header":"1 Introduction","content":"\u003cp\u003eBarium titanate (BaTiO\u003csub\u003e3\u003c/sub\u003e) is one of the most widely studied perovskite ceramics material due to its outstanding dielectric, ferroelectric, and piezoelectric properties, which enable applications in devices such as multilayer ceramic capacitors, thermistors, random-access memory (DRAM), and piezoelectric sensors [\u003cspan additionalcitationids=\"CR2 CR3 CR4\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Its technological relevance has made BaTiO₃ a cornerstone material in the electronics industry, yet challenges remain in optimizing its synthesis, particularly in achieving high phase purity while minimizing impurity phases such as barium carbonate (BaCO₃) [\u003cspan additionalcitationids=\"CR7\" citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. The presence of this impurity, commonly introduced during synthesis through reactions with atmospheric CO₂, reduces dielectric and piezoelectric performance and requires additional post-synthesis purification steps [\u003cspan additionalcitationids=\"CR10 CR11\" citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eFurthermore, the production of this material typically employs conventional synthesis routes\u0026mdash;including pyrolysis, solvothermal, and hydrothermal processes\u0026mdash;often require high processing temperatures (\u0026gt;\u0026thinsp;150\u0026deg;C), extended reaction times, and inert atmospheres (e.g., N₂, Ar) to stabilize precursors and avoid degradation [\u003cspan additionalcitationids=\"CR14\" citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. While effective, these conditions significantly increase energy consumption, operational costs, and results in additional carbon footprint due to gas purging the carbon footprint of production due to prolonged heating and continuous gas purging.This conflict highlights the need for sustainable synthesis strategies that can maintain or improve material performance while reducing energy demand and environmental impact.\u003c/p\u003e \u003cp\u003eContemporary studies in sustainable ceramics and energy-efficient perovskite synthesis emphasize the potential of precursor engineering and ambient-condition processing to achieve both technical and environmental goals. For example, eco-friendly sol-gel and hydrothermal routes have been reported for BaTiO₃ and related perovskites, though most still rely on elevated temperatures, specialized atmospheres, or lengthy reaction times [\u003cspan additionalcitationids=\"CR17 CR18\" citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. Building upon this trend, our present study explores a modified sol-gel route that eliminates the need for inert atmospheres, shortens synthesis to only 3 h at 130\u0026deg;C, and drastically reduces the formation of BaCO₃ impurities through the use of barium chloride as precursor.\u003c/p\u003e \u003cp\u003eThe aim of this work is therefore twofold: (i) to demonstrate how precursor substitution can significantly improve phase purity, particle size control, and surface properties of BaTiO₃ nanostructures, and (ii) to validate a sustainable, scalable, and energy-efficient pathway for producing high-purity BaTiO₃. By correlating synthesis conditions with structural and morphological outcomes, this research contributes new insights into the mechanisms of impurity suppression and growth control, while positioning BaTiO₃ synthesis within the broader context of environmentally responsible ceramic processing.\u003c/p\u003e"},{"header":"2 Materials and methods","content":"\u003cp\u003eThe reagents used included: titanium butoxide [CH₃(CH₂)₃O]₄Ti (\u0026asymp;\u0026thinsp;98%, Sigma-Aldrich), [BaOH], triethanolamine C₆H₁₅NO₃ (99.90%, Baker), deionized water, barium hydroxide Ba(OH)₂\u0026middot;8H₂O (\u0026asymp;\u0026thinsp;98%, Sigma-Aldrich), barium chloride dihydrate BaCl₂\u0026middot;2H₂O (\u0026asymp;\u0026thinsp;99%, Sigma-Aldrich) [BaCl], sodium hydroxide NaOH (\u0026asymp;\u0026thinsp;98%, Baker). All this reagents were of analytical grade and required no additional purification for its use.\u003c/p\u003e \u003cdiv id=\"Sec3\" class=\"Section3\"\u003e \u003cdiv class=\"Heading\"\u003e2.1.1 Sol-gel Route A\u003c/div\u003e \u003cp\u003e17.5 g of titanium butoxide was mixed with 7.57 g of triethanolamine (TEA) in a 1:1 molar ratio, under continuos stirring (800 rpm) at room temperature for 24 hours in a controlled low-humidity atmosphere (4%), yielding a stable formation of titanium complex and prevented uncontrolled hydrolysis. A master solution was prepared by adding deionized water to a final volume of 100 mL. Separately, 6.31 g of Ba(OH)₂\u0026middot;8H₂O was dissolved in 10 ml of deionized water, to which 10 ml of the master solution was added and stirred at 600 rpm for 1 hour. The resulting gel was was transferred to an autoclave and heated at 180\u0026deg;C for 24 hours. To purify the material and obtain finer particles, centrifugation separation washes were performed and powders were dried at 80\u0026deg;C for 24 h.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section3\"\u003e \u003cdiv class=\"Heading\"\u003e2.1.2 Post-synthesis treatment\u003c/div\u003e \u003cp\u003eTo remove residual BaCO\u003csub\u003e3\u003c/sub\u003e a fraction of the dried powders was washed with 10% of diluted HCl at room temperature for 2 h.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Sol-gel Route B\u003c/h2\u003e \u003cp\u003eThe initial step was identical to Route A (titanium butoxide\u0026thinsp;+\u0026thinsp;TEA). In this case, 8.97 g of BaCl₂\u0026middot;2H₂O was dissolved in 10 mL of deionized water, and 2.90 g of NaOH was added to provide the alkaline environment required for hydrolysis. After mixing with the master solution under stirring (700 rpm, 1 h), the gel was autoclaved at 130\u0026deg;C for 3 h. The resulting powders were centrifuged, washed with water, and dried at 80\u0026deg;C for 4 h.\u003c/p\u003e \u003c/div\u003e"},{"header":"3 Results and discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Fourier Transform Infrared Spectroscopy (FT-IR)\u003c/h2\u003e \u003cp\u003eFT-IR spectra were obtained for the samples, which were prepared as pellets with KBr. The spectra were recorded in the range of 400 to 4000 cm⁻\u0026sup1; to identify the bonds present in the samples, as will be described in the subsequent figures. In Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e, the spectra obtained from the samples synthesized without post-treatment, HCl washed and derived from BaCl\u003csub\u003e2\u003c/sub\u003e precursor. Initially, the main functional groups exhibit high similarity in all samples with the characteristic OH group associated to the presence of moisture located around 3100 to 3600 cm⁻\u0026sup1; [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. The small band observed at approximately 1750 cm⁻\u0026sup1; corresponds to the stretching vibration of an organic carbonate [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. The bands between 1570 and 1680 cm⁻\u0026sup1; result from an overlap of peaks typical of moisture absorption and BaTiO\u003csub\u003e3\u003c/sub\u003e [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e, \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. A clear deviation of the samples is observed in the broad band around 1450 cm⁻\u0026sup1; is notable, corresponding to the asymmetric stretching of the simple carbonate ion [CO₃]\u0026sup2;⁻ associated with the presence of BaCO\u003csub\u003e3\u003c/sub\u003e. In the sample where washing with HCl was performed, specifically 10%/2 h, a significant decrease in the presence of this band is noted. The considerable increase in the percentage of transmittance indicates an almost complete removal of the barium contaminant in the sample, demonstrating that washing with HCl is effective in eliminating this impurity. However, for the sample synthesized with BaCl₂ as the barium precursor, the band at 1450 cm⁻\u0026sup1; shows significantly higher transmittance (~\u0026thinsp;60%) compared to the Ba(OH)₂-based sample (~\u0026thinsp;30%). This suggests lower BaCO₃-related absorbance and, consequently, a reduced amount of this contaminant in the BaCl₂-derived sample. Critically, using BaCl₂ as the precursor eliminates the need for post-synthesis HCl washing while simultaneously suppressing unwanted phases formation. Several studies in the literature indicate that the formation of barium carbonate is a common phenomenon during the synthesis of BaTiO₃. Expandin on the previous point, the presence of BaCO₃ is inferred [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e], which is a non-piezoelectric phase that does not contribute to the piezoelectric properties of BaTiO₃. This directly affects and may reduce the proportion of the active phase (BaTiO₃) in the sample [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. Furthermore, BaCO₃ acts as an impurity in the BaTiO₃ matrix, introducing defects in the crystal structure that can affect mechanical properties [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eAdditionally, the signals between 690 and 855 cm⁻\u0026sup1; are due to in-plane and out-of-plane bending vibrations [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. The small bands between 1000 and 1200 cm⁻\u0026sup1; are attributed to TiO₂, and the signal at 1060 cm⁻\u0026sup1; represents the characteristic absorption of C-O. Finally, the bands around 560\u0026ndash;580 cm⁻\u0026sup1; are associated with the Ba-O bond present in BaTiO₃, as well as the normal vibration of the Ti-O bond [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e, \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIt can be determined that the presence of the characteristic fingerprint bands of BaTiO₃ and its associated bonds (560\u0026ndash;580 and 1680 cm⁻\u0026sup1;) provides consistent evidence of the formation of the wanted material.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eIt can be inferred that when Ba(OH)₂ is used as the precursor, OH⁻ ions are provided in the reaction medium, creating a basic environment that facilitates both the hydrolysis of the titanium precursor and the formation of intermediate species required during the reaction. However, when BaCl₂\u0026middot;2H₂O is used instead of Ba(OH)₂, the lack of OH⁻ must be compensated by adding a strong base [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e, \u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e], such as NaOH in this case. The addition of NaOH serves several important functions, including generating a basic environment essential for the reaction, adjusting the pH to optimal values (typically above 10), and promoting the in situ precipitation of Ba(OH)₂ through the reaction:\u003c/p\u003e \u003cp\u003eBaCl\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;+\u0026thinsp;2NaOH\u0026thinsp;=\u0026thinsp;Ba(OH)\u003csub\u003e2\u003c/sub\u003e + 2NaCl\u003c/p\u003e \u003cp\u003eTherefore, the proper hydrolysis of the titanium precursor is ensured, which is essential for obtaining active species that react with Ba\u0026sup2;⁺ to form BaTiO₃ during the precursor mixing stage. However, most of the BaCO\u003csub\u003e3\u003c/sub\u003e formation occurs during the heating stage, as BaTiO\u003csub\u003e3\u003c/sub\u003e transitions through the rhombohedral, orthorhombic, and tetragonal phases. This process generates a dipole-dipole interaction with environmental CO\u003csub\u003e2\u003c/sub\u003e (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), creating the conditions necessary for the formation of the contaminant compound. [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe absence of intense carbonate bands in the FT-IR spectra of the BaCl\u003csub\u003e2\u003c/sub\u003e-derived sample (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e) in contrast to the Ba(OH)\u003csub\u003e2\u003c/sub\u003e-derived sample demonstrates that this precursor effectively suppresses BaCO\u003csub\u003e3\u003c/sub\u003e formation. This key advantajes eliminates the need for post-synthesis treatments aimend at carbonate removal, such as sintering or acid washing. Consecuently, the synthesis process is streamlined, reducing the use of chemicals and generation of waste. The spectra cinfermed the presence of characteristic BaTiO\u003csub\u003e3\u003c/sub\u003e bands (Ti-O stretching at 560\u0026ndash;580 cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e), indicating that the target phase was successfully obtained without these additional, resources intensive steps.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003e3.2 X-Ray Diffraction (XRD)\u003c/h2\u003e \u003cp\u003eThe patterns obtained from the analysis of the samples synthesized with shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e, exhibit the presence of two phases. The peaks at diffraction angles of 22.16\u0026deg;, 31.53\u0026deg;, 38.87\u0026deg;, 45.26\u0026deg;, 56.13\u0026deg;, 65.87\u0026deg;, and 70.49\u0026deg;, indicated with black arrows, correspond to BaTiO₃ (CARD00-150-7757) and are associated with the crystallographic planes (001), (101), (111), (002), (112), (202), and (212) [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e]. This diffraction pattern also shows, indicated with green circles, the presence of another phase with peaks at angles 19.46\u0026deg;, 23.91\u0026deg;, 27.72\u0026deg;, 29.54\u0026deg;, 34.60\u0026deg;, 42.97\u0026deg;, 46.78\u0026deg;, 61.03\u0026deg;, 76.94\u0026deg;, and 86.62\u0026deg;, which correspond to BaCO₃ (CARD009013804) [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. The presence of this phase aligns with the infrared spectroscopy analyses performed.\u003c/p\u003e \u003cp\u003eThe diffraction pattern associated with the sample treated with HCl washes at concentration 10%, a noticeable change is observed. In these cases, the secondary phase associated with BaCO₃ is not present in the samples; instead, only the phase corresponding to BaTiO₃ [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eAnother important difference in the comparative analysis of the obtained diffractograms lies in the relative intensity of the peaks corresponding to the two phases present. This difference is particularly noticeable in the sample synthesized from the Ba(OH)\u003csub\u003e2\u003c/sub\u003e precursor compared to the other sample where BaCl\u003csub\u003e2\u003c/sub\u003e was used. Such variation in peak intensity suggests, as previously inferred from the FT-IR analysis results, a difference in the proportion or predominance of each phase (BaCO\u003csub\u003e3\u003c/sub\u003e and BaTiO\u003csub\u003e3\u003c/sub\u003e) within the samples. In the first case the predominant peak corresponds to the contaminant compound, while in the pattern associated with BaCl\u003csub\u003e2\u003c/sub\u003e sample a higher peak intensity corresponding to BaTiO\u003csub\u003e3\u003c/sub\u003e is observed [\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e, \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. These differences in peak intensity reflect adjustments in the crystal structure that could have significant implications for the material's final properties.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eIn Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e, the diffraction patterns obtained using BaCl₂ (M2) under different synthesis conditions without an inert atmosphere are shown. Variations in these parameters did not produce significant changes. Although the patterns agree with the infrared spectra, a slight difference is observed between the BaCl precursor and BaCl M2 samples. These findings are consistent with the structural analysis, where Ba(OH)₂-derived powders contained secondary BaCO₃ phases, while BaCl₂ samples exhibited higher phase purity.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eCrystallite size estimation by the Scherrer equation yielded\u0026thinsp;~\u0026thinsp;39 nm for Ba(OH)₂-derived (acid-washed) sample and ~\u0026thinsp;10 nm for those from BaCl₂. Rietveld refinement (Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e), confirmed a cubic perovskite BaTiO₃ structure (a\u0026thinsp;=\u0026thinsp;0.4016 nm). However, cuantitative phase refinement revealed the coexistence of a tetragonal phase, aligns with previous reports of nanostructured BaTiO\u003csub\u003e3\u003c/sub\u003e [\u003cspan additionalcitationids=\"CR40 CR41\" citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.3 Field Emission Scanning Electron Microscopy (FE-SEM)\u003c/h2\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e presents FE-SEM micrographs of the powders synthesized using different barium precursors and subsequently washed with HCl (scale bar: 100 nm). In the Ba(OH)₂-based samples, most particles exhibit a spheroidal morphology with diameters around 90\u0026ndash;110 nm. Some larger aggregates are also visible, likely associated with BaCO₃ formation through a secondary growth process [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. After washing with 10% HCl, these BaCO₃-related structures were almost completely removed, leaving a more uniform surface composed mainly of BaTiO₃ spheroids. By contrast, the BaCl₂-derived powders display much smaller and more homogeneous particles, about 25 nm in diameter, without the whisker-like or oversized BaCO₃ structures observed previously. The morphology observed here agrees with the FT-IR and XRD analyzes, confirming that the type of precursor strongly influences the nucleation behavior and the extent of particle growth [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]. Overall, the route using BaCl₂ favors higher phase purity and smaller crystallites, while also reducing BaCO₃ formation, reaction time, and energy consumption\u0026mdash;making it a more efficient and sustainable pathway for BaTiO₃ synthesis.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eElemental mapping analysis reveals clear differences in the compositional homogeneity between the samples. The BaCl\u003csub\u003e2\u003c/sub\u003e-derived powders exhibited a uniform distribution of all constituent elements (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003eb). In contrast, the Ba(OH)\u003csub\u003e2\u003c/sub\u003e-derived samples evidenced significant compositional heterogeneity, these corroborate that the larger structures identified (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003ea) are attributable to a residual secondary phase, whereas the spheroidal morphologies consist primarily of BaTiO\u003csub\u003e3\u003c/sub\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003e3.4 Specific Surface Area by Brunauer-Emmett-Teller (BET) Method\u003c/h2\u003e \u003cp\u003eNitrogen adsorption-desorption isotherms of the BaCl\u003csub\u003e2\u003c/sub\u003e-derived sample (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e) revealed a Type IV isotherm with an H1-type hysteresis loop [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e, \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e] confirming a mesoporous structure with well-defined, uniform pores [\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e], Symmetric H1 hysteresis also suggests the presence of cylindrical or prismatic pores with a narrow size distribution [\u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e]. The calculated surface area was 53.85 m\u0026sup2;/g with an average pore radius of 3.7 nm. Such a high surface area values are advantageous for composite integration and applications requiring large interfacial areas and efficient adsorption-desorption cycles[\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e, \u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003e3.5 Energy Cost Analysis and Process Sustainability\u003c/h2\u003e \u003cp\u003eTo quantify the sustainable advantage of the low-temperature hydrothermal synthesis route, the total energy cost per unit mass produced BaTiO3 (kJ/g) was estimated. The calculation includes the thermal energy (\u003cem\u003eE\u003c/em\u003e\u003csub\u003e\u003cem\u003ethermal\u003c/em\u003e\u003c/sub\u003e) required to heat the reaction system (autoclave, solution and reagents) and the electrical energy (\u003cem\u003eE\u003c/em\u003e\u003csub\u003e\u003cem\u003eelectrical\u003c/em\u003e)\u003c/sub\u003e consumed for temperature maintenance and stirring during the 3 h process.\u003c/p\u003e \u003cp\u003eEnergy Cost Calculation (Our Methode)\u003c/p\u003e \u003cp\u003eGiven the estimated system variables (Total mass\u0026thinsp;\u0026asymp;\u0026thinsp;500g; Δ\u003cem\u003eT\u0026thinsp;\u0026asymp;\u0026thinsp;105\u0026ordm;C; Maintenace power\u0026thinsp;\u0026asymp;\u0026thinsp;50 W; BaTiO3 produced\u0026thinsp;=\u0026thinsp;1.7g\u003c/em\u003e), the total energy was calculated as follows:\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003e1. Thermal Energy (E):\u003c/h3\u003e\n\u003cp\u003e \u003cdiv id=\"Equa\" class=\"Equation\"\u003e \u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equa\" name=\"EquationSource\"\u003e\n$$\\:{E}_{thermal}=m\\cdot\\:{C}_{p}\\cdot\\:{\\Delta\\:}T\\approx\\:500\\:g\\cdot\\:2.5\\:\\frac{J}{g{\\cdot\\:}^{\\circ\\:}C}\\cdot\\:{105}^{\\circ\\:}C=131.25\\:kJ$$\u003c/div\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003eElectrical Energy (E\u003csub\u003eelectrical\u003c/sub\u003e):\u003cdiv id=\"Equb\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equb\" name=\"EquationSource\"\u003e\n$$\\:{E}_{electrical}=P\\cdot\\:t\\approx\\:50\\:W\\cdot\\:10800\\:s=540\\:kJ$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eNormalized Cost (CN):\u003cdiv id=\"Equc\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equc\" name=\"EquationSource\"\u003e\n$$\\:{C}_{N}=\\frac{{E}_{\\text{thermal}}+{E}_{\\text{electrical}}}{{m}_{{\\text{BaTiO}}_{3}}}=\\frac{131.25\\:\\text{kJ}+540\\:\\text{kJ}}{1.7\\:\\text{g}}\\approx\\:394.85\\:\\frac{\\text{kJ}}{\\text{g}}$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eComparative Analysis of Synthesis Routes for BaTiO\u003csub\u003e3\u003c/sub\u003e Nanomaterials, process conditions and energy efficiency.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"6\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSynthesis Method (Reference)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eT/t (\u0026deg;C / h)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eParticle Size (nm)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eBaCO\u003csub\u003e3\u003c/sub\u003e​ Presence\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eCalcination Requirement\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eEstimated Energy Cost (kJ/g)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eOur Method\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e130\u0026nbsp;/\u0026nbsp;3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e25\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eLess than Ba(OH)\u003csub\u003e2\u003c/sub\u003e​ route\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u0026asymp;\u0026thinsp;395\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eModified Solid-State (Ref. 11)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e900\u0026nbsp;/\u0026nbsp;long\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u0026sim;50\u0026thinsp;\u0026minus;\u0026thinsp;several\u0026nbsp;\u0026micro;m\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eYES\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u0026gt;\u0026thinsp;15,000 (High)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSol-Gel/Calcination (Ref. 12)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eAmbient / \u0026gt;6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e10\u0026thinsp;\u0026minus;\u0026thinsp;50\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eYES\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e3,000\u0026thinsp;\u0026minus;\u0026thinsp;8,000 (Medium-High)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eIn Situ Hydrothermal (Ref. 8)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e125\u0026thinsp;\u0026minus;\u0026thinsp;150\u0026nbsp;/\u0026nbsp;\u0026sim;4\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e10\u0026thinsp;\u0026minus;\u0026thinsp;15\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eYES (Requires acid wash)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e350\u0026thinsp;\u0026minus;\u0026thinsp;500 (Low)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSonochemical (Ref. 18)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e25\u0026nbsp;/\u0026nbsp;1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e20\u0026thinsp;\u0026minus;\u0026thinsp;30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eYES (Requires acid wash)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e50\u0026thinsp;\u0026minus;\u0026thinsp;100 (Very Low)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe calculated 395 kJ/g energy cost formally validates the high efficiency og our methode. This value is two orders of magnitude lower than the \u0026gt;\u0026thinsp;3000 kJ/g associated with calcination routes (Ref. 11, 12), proving energy saving. While ultra-low-T methods (Ref. 8) are cheaper (⁓ 50\u0026ndash;100 kJ/g), they require chemical post-treatment due to BaCO\u003csub\u003e3\u003c/sub\u003e impurities.\u003c/p\u003e \u003cp\u003eIn contrast, our methode eliminates the need for both calcination and acid treatment. This key advantage enhances overall process sustainability by simplifying the route, conserving energy, and minimizing chemical waste, making it the optimal and most environmentally responsible alternative.\u003c/p\u003e"},{"header":"4 Conclusion","content":"\u003cp\u003eThis study establishes a sustainable and energy-efficient sol-gel strategy for synthesizing BaTiO₃ nanostructures, minimizing both environmental impact and production costs. By replacing Ba (OH)₂ with BaCl₂ as the barium precursor, the process minimized carbonate impurities, eliminated the need for acid washing, and achieved an ~\u0026thinsp;81% reduction in energy demand. The resulting nanostructures displayed superior phase purity, smaller and more uniform particle sizes (~\u0026thinsp;25 nm), and higher surface area values, making them ideal for integration into advanced electronic devices. Importantly, these approach reduces environmental impact by avoiding inert atmospheres, shortening reaction times, and lowering chemical consumption. These findings highlight the dual benefit of precursor engineering: tailoring structural and functional properties while promoting sustainability. The proposed route not only provides a scalable method for industrial production of BaTiO₃ but also contributes to the broader goal of low-carbon, resource-efficient processing in functional ceramics.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e \u003ch2\u003eCompeting Interests\u003c/h2\u003e \u003cp\u003eThe 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.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eFunding\u003c/h2\u003e \u003cp\u003eNo external funding was received for the development of this study.\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eI. E. Correa carried out the synthesis, characterization, and data analysis of the BaTiO₃ nanostructures and wrote the original manuscript. S. E. Borjas and A. Medina provided the laboratory facilities and materials. J. A. Ascencio and S. E. Borjas developed the experimental protocols. J. A. Ascencio and A. Medina supervised the project. All authors reviewed and approved the final version of the manuscript.\u003c/p\u003e\u003ch2\u003eData Availability\u003c/h2\u003e\u003cp\u003eThe data supporting the findings of this study are available from the corresponding author upon reasonable request from [email protected]\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eGabriela J\u0026aacute;come-Acatitla, Mayra \u0026Aacute;lvarez-Lemus, Rosendo L\u0026oacute;pez-Go nz\u0026aacute;lez,Cinthia Garc\u0026iacute;a-Mendoza, Andr\u0026eacute;s S\u0026aacute;nchez-L\u0026oacute;pez, Diego Hern\u0026aacute;ndez-Acosta (2020) Photodegradation of 4-chloropehol in aqueous media using LaBO\u003csub\u003e3\u003c/sub\u003e (B\u0026thinsp;=\u0026thinsp;Fe, Mn, Co) perovskites: Study of the influence of the transition metal ion in the photocatalytic activity. Journal of hotochemistry \u0026amp; Photobiology A: Chemistry 390 112330\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJin Hu, Heteng Fan, Songji Wu, Liguo Tang, Lei Qin, Wenyu Luo (2022) Characterization of temperatura dependence of dielectric, elastic and piezoelectric properties of BaTiO\u003csub\u003e3\u003c/sub\u003e ceramics. Ceramics International 48 25741\u0026ndash;25746\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eIvan Kovač, Matko Mužević, Maja Varga Pajtler, Igor Lukačević (2023) Charge carrier dynamics across the metal oxide/BaTiO\u003csub\u003e3\u003c/sub\u003e interfaces toward photovoltaic applications from the theoretical perspective. Surfaces and Interfaces Volume 39 102974\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSatiye Korkmaz, Afsin Kariper (2021) BaTiO\u003csub\u003e3\u003c/sub\u003e-based nanogeneratorrs: fundamentals and current status. Journal of Electroceramics\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eAlaa K. Hassan, Ghusoon M. Ali (2020) Thin film NiO/BaTiO\u003csub\u003e3\u003c/sub\u003e/ZnO heterojunction diode-based UVC photodetectors. Superlattices and Microstructures Volume 147 106690\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eP.P. Gohain, R. Saha, M.G. Choudhury (2021) Synthesis of Mixed-phase Barium Titanium Oxide (BaTiO\u003csub\u003e3\u003c/sub\u003e/Ba\u003csub\u003e2\u003c/sub\u003eTiO\u003csub\u003e4\u003c/sub\u003e) Perovskite Catalyst for Biofuel Production J. Nano- Electron. Phys. 13 No 3, 03017\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eTedi-Marie Usher, Benard Kavey, Gabriel Caruntu, and Katharine Page. (2020) The Effect of BaCO\u003csub\u003e3\u003c/sub\u003e Impurities on the Structure of BaTiO\u003csub\u003e3\u003c/sub\u003e Nanocrystals: Implications for Multilayer Ceramic Capacitors. ACS Appl. Nano Mater\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eGrendal, O. G., Blichfeld, A. B., Skj\u0026aelig;rv\u0026oslash;, S. L., Van Beek, W., Selbach, S. M., Grande, T., \u0026amp; Einarsrud, M.A (2018) Facile Low Temperature Hydrothermal Synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e Nanoparticles Studied by In Situ X-ray Diffraction. Crystals, 8(6), 253\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eBuscaglia V., Buscaglia M. T., Canu G. (2020) BaTiO\u003csub\u003e3\u003c/sub\u003e-Based Ceramics: Fundamentals, Properties and Applications. Reference Module in Materials Science and Materials Engineering\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eMaria de Andrade Gomes, Lucas Gon\u0026ccedil;alves Magalh\u0026atilde;es, Alexandre Rocha Paschoal, Z\u0026eacute;lia Soares Macedo, \u0026Aacute;lvaro Silva Lima, Katlin Ivon Barrios Eguiluz and Giancarlo Richard Salazar-Banda (2018) An Eco-Friendly Method of BaTiO3 Nanoparticle Synthesis Using Coconut Water. Journal of Nanomaterials\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eWan, L., Zhu, G., Xu, H. (2022) Low-temperature solid-state synthesis of tetragonal BaTiO\u003csub\u003e3\u003c/sub\u003e powders from Ba(OH)\u003csub\u003e2\u003c/sub\u003e and H\u003csub\u003e2\u003c/sub\u003eTiO\u003csub\u003e3\u003c/sub\u003e. Appl. Phys. A 128, 858\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eAlmeida, G. N., de Souza, R. N., Lima, L. F. S., Mohallem, N. D. S., da Silva, E. P., \u0026amp; Silva, A. M. A. (2023) The Influence of the Synthesis Method on the Characteristics of BaTiO\u003csub\u003e3\u003c/sub\u003e. Materials, 16(8), 3031\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eR.A. Surmenev, R.V. Chernozem, A.G. Skirtach, A.S. Bekareva, L.A. Leonova, S. Mathur, Yu. F. Ivanov, M.A. Surmeneva (2021) Hydrothermal synthesis of barium titanate nano/microrods and particle agglomerates using a sodium titanate precursor, Ceramics International, Volume 47, Issue 7, Part A, Pages 8904\u0026ndash;8914, ISSN 0272\u0026ndash;8842\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eXiaoxiao Pang, Tingting Wang, Bin Liu, Xiayue Fan, Xiaorui Liu, Jing Shen, Cheng Zhong, and Wenbin Hu. (2023) Effect of solvents on the morphology and structure of barium titanate synthesized by a one-step hydrothermal method, Int. J. Miner. Metall. Mater., 30, No. 7, pp. 1407\u0026ndash;1416\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eGulraiz Tanvir, Mohsin Saleem, Hamid Jabbar, Amir Hamza, Muhammad Asif Hussain, Muhammad Zubair Khan, Abrar H Baluch, Muhammad Irfan, Muhammad Shoaib Butt, Faysal Naeem, Abdul Ghaffar, Muhammad Ahsan, Muhammad Asif Rafiq, Rizwan Ahmed Malik, Adnan Maqbool. (2023) Study of ferroelectric and piezoelectric response of heat-treated surfactant-based BaTiO3 nanopowder for high energy capacitors. Materials Science and Engineering: B, Volume 287, 116100, ISSN 0921\u0026ndash;5107\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eWang T, Pang X, Liu B, Liu J, Shen J, Zhong C. (2023) A Facile and Eco-Friendly Hydrothermal Synthesis of High Tetragonal Barium Titanate with Uniform and Controllable Particle Size. Materials; 16(11):4191\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eHan, J.-M., Joung, M.-R., Kim, J.-S., Lee, Y.-S., Nahm, S., Choi, Y.-K. and Paik, J.-H. (2014) Hydrothermal Synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e Nanopowders Using TiO\u003csub\u003e2\u003c/sub\u003e Nanoparticles. J. Am. Ceram. Soc., 97: 346\u0026ndash;349\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eUtara S, Hunpratub S. (2018) Ultrasonic assisted synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e nanoparticles at 25\u0026deg;C and atmospheric pressure. Ultrason Sonochem. Mar; 41:441\u0026ndash;448\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eAhamed, M., \u0026amp; Khan, M. A. M. (2023) Enhanced Photocatalytic and Anticancer Activity of Zn-Doped BaTiO\u003csub\u003e3\u003c/sub\u003e Nanoparticles Prepared through a Green Approach Using Banana Peel Extract. Catalysts, 13(6), 985\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eMaria del Carmen Blanco Lopez, Georgios Fourlaris, BrianRand and Frank L. Riley. (1999) Characterization of Barium Titanate Powders: Barium Carbonate Identification. J. Am. Ceram. Soc., 82 [7] 1777\u0026ndash;86\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eL. H. Little (1966) Infrared Spectra of Adsorbed Species; pp. 74\u0026ndash;84. Academic Press, London, U.K.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eMi, L., Zhang, Q., Wang, H., Wu, Z., Guo, Y., Li, Y., Qi, X. (2023) Synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e nanoparticles by sol-gel assisted solid phase method and its formation mechanism and photocatalytic activity. Ceramics International\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJung-Hoon Park and Sangdo Park. (2007) Hydrothermal Synthesis and Characterization of BaTiO\u003csub\u003e3\u003c/sub\u003e Fine Powders. Korean Chem. Eng. Res., Vol. 45, No. 5, October, pp. 448\u0026ndash;454\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJ. A. Gadsden (1975) Infrared Spectra of Minerals and Related Inorganic Compounds; p. 62. Butterworth, London, U.K.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eChoy, K. L., \u0026amp; Moreno, R. (1997) Influence of Barium Carbonate on the Sintering and Dielectric Properties of Barium Titanate. Journal of the European Ceramic Society, 17(15\u0026ndash;16), 1973\u0026ndash;1978\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eKim, H. E., \u0026amp; Koh, Y. H. (2000) Effect of Barium Carbonate Addition on the Microstructure and Piezoelectric Properties of Barium Titanate Ceramics. Journal of the American Ceramic Society, 83(9), 2281\u0026ndash;2284\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eYamashita, Y., Iwata, M., \u0026amp; Koda, T. (1999) Synthesis and Characterization of Barium Titanate Ceramics: Influence of BaCO\u003csub\u003e3\u003c/sub\u003e Impurities. Materials Research Bulletin, 34(11\u0026ndash;12), 1931\u0026ndash;1938\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eClaude Hkrard, Annelise Faivre \u0026amp; Jacques Lemaitre. (1995) Surface Decontamination Treatments of Undoped BaTiO\u003csub\u003e3\u003c/sub\u003e-Part I: Powder and Green Body Properties. Journal of the European thzmic Society 15; 135\u0026ndash;143\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eClaude Hkrard, Annelise Faivre \u0026amp; Jacques Lemaitre. (1995) Surface Decontamination Treatments of Undoped BaTiO\u003csub\u003e3\u003c/sub\u003e-Part II: Influence on sintering. Journal of the European thzmic Society 15; 135\u0026ndash;143\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJ. R. Ferraro (1982) Infrared Spectra Handbook of Minerals and Clays; p. 75. SADTLER Research Laboratories, Division of Bio-Rad Laboratories Inc., Philadelphia, PA\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJ. T. Last, (1957) Infrared-Adsorption Studies on Barium Titanate and Related Materials. Phys. Rev., 105, 1740\u0026ndash;50\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLiu, Y., Li, S., Gallucci, F., \u0026amp; Rebrov, E. V. (2024) Sol-gel synthesis of tetragonal BaTiO\u003csub\u003e3\u003c/sub\u003e thin films under fast heating. Applied Surface Science, 661, Article 160086\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eP.P. Gohain, R. Saha, M.G. Choudhury, R. Kataki, S. Paul. (2021) Synthesis of Mixed-phase Barium Titanium Oxide (BaTiO\u003csub\u003e3\u003c/sub\u003e/Ba\u003csub\u003e2\u003c/sub\u003eTiO\u003csub\u003e4\u003c/sub\u003e) Perovskite Catalyst for Biofuel Production. Journal Of Nano- And Electronic Physics; Vol. 13 No 3, 03017(4pp)\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eC. Proust, E. Husson, G. Blondiaux, and J. P. Coutures (1994) Residual Carbon Detection in Barium Titanate Ceramics by Nuclear Reaction Technique. J. Eur. Ceram. Soc., 14, 215\u0026ndash;19\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eC. M. \u0026Aacute;lvarez-Docioa, Juli\u0026aacute;n Jim\u0026eacute;nez Reinosaa, Giovanna Canub, Mar\u0026iacute;a Teresa Buscagliab, Vincenzo Buscagliab, Jos\u0026eacute; Francisco Fern\u0026aacute;ndez (2019) Revealing the Role of the Intermediates during the Synthesis of BaTi\u003csub\u003e5\u003c/sub\u003eO\u003csub\u003e11\u003c/sub\u003e. Inorganic Chemistry 0\u0026ndash;06\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eA. Garc\u0026iacute;a-Ruiz, J.I. Rodr\u0026iacute;guez-Mora, A. Morales, M. Aguilar, and C. Zorrilla, J.A. Ascencio (2019) Structural determination and Rietveld refinement of Ba\u003csub\u003eX\u003c/sub\u003eTi\u003csub\u003eY\u003c/sub\u003eO\u003csub\u003eZ\u003c/sub\u003e subspecies. Revista Mexicana de F\u0026iacute;sica S 55 (1) 52\u0026ndash;56\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eRietveld, H. M. (1969) A profile refinement method for nuclear and magnetic structures. Journal of Applied Crystallography, 2(2), 65\u0026ndash;71\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eReddy, V. Narasimha \u0026amp; Kadiyala, Chandra Babu Naidu \u0026amp; Subbarao, Thota (2016) Structural, optical and ferroelectric properties of BaTiO\u003csub\u003e3\u003c/sub\u003e ceramics. Journal of Ovonic Research. 12. 185\u0026ndash;191\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eS. Tsunekawa, S. Ito, T. Mori, K. Ishikawa, Z.Q. Li, Y. Kawazoe, (2000) Critical size and anomalous lattice expansion in nanocrystalline BaTiO\u003csub\u003e3\u003c/sub\u003e particles. Phys. Rev. B 62, 3065\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eK. Uchino, E. Sadanaga, T. Hirose (1989) Dependence of the Crystal Structure on Particle Size in Barium Titanate. J. Am. Ceram. Soc. 72, 1555\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eChang, C.-Y., Huang, C.-Y., Wu, Y.-C., Su, C.-Y., \u0026amp; Huang, C.-L. (2010) Synthesis of submicron BaTiO\u003csub\u003e3\u003c/sub\u003e particles by modified solid-state reaction method. Journal of Alloys and Compounds, 495(1), 108\u0026ndash;112\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eBowland, Christopher \u0026amp; Sodano, Henry. (2017) Hydrothermal synthesis of tetragonal phase BaTiO\u003csub\u003e3\u003c/sub\u003e on carbon fiber with enhanced electromechanical coupling. Journal of Materials Science. 52. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003e10.1007/s10853-017-0994-9\u003c/span\u003e\u003cspan address=\"10.1007/s10853-017-0994-9\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSakae Tsutai, Tomoki Hayashi, Shigeo Hayashi and Zenbe-e Nakagawa. (2001) Reaction mechanism of BaTiO\u003csub\u003e3\u003c/sub\u003e from powder compacts, BaCO\u003csub\u003e3\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e and expansion phenomena during formation process. Journal of the Ceramic Society of Japan, 109 12 1028\u0026ndash;1034.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eVoorhees, P.W. (1985) The theory of Ostwald ripening. J Stat Phys 38, 231\u0026ndash;252.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eHao Zu, Qiuyun Fu, Chao Gao, Tao Chen, Dongxiang Zhou, Yunxiang Hu, Zhiping Zheng, Wei Luo (2018) Effects of BaCO3 addition on the microstructure and electrical properties of La-doped barium titanate ceramics prepared by reduction-reoxidation method. Journal of the European Ceramic Society, Volume 38, Issue 1 Pages 113\u0026ndash;118, ISSN 0955\u0026ndash;2219\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eStephen Brunauer. P. H. Emmett and Edward Teller. (1938) Adsorption of Gases in Multimolecular Layers. Contribution from the bureau of chemistry and sons and George Washington university\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eK. S. W. Sing, D. H. Everet, R. A. W. Haul, L. Moscou, R. A. Pieroti, J. Rouquerol, T. Siemieniewska. (1985) Reporting physisorption data for gas/solid systems with special reference to the determination of Surface Area and Porosity. Pure \u0026amp; Ap. Chem., Vol. 57, No. 4, p. 603\u0026ndash;619.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eKudlacik-Kramarczyk, Sonia \u0026amp; Drabczyk, Anna \u0026amp; Gląb, Magdalena \u0026amp; Dulian, Piotr \u0026amp; Bogucki, Rafał \u0026amp; Miernik, Krzysztof \u0026amp; Sobczak-Kupiec, Agnieszka \u0026amp; Tyliszczak, Bozena. (2020) Mechanochemical Synthesis of BaTiO\u003csub\u003e3\u003c/sub\u003e Powders and Evaluation of Their Acrylic Dispersions. Materials. 13. 3275. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003e10.3390/ma13153275\u003c/span\u003e\u003cspan address=\"10.3390/ma13153275\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSadaf Bashir Khan, Nan li, Shenggui Chen, Jiahua Liang, Chuang Xiao, Xiaohong Sun, (2023) Influence of nanoparticle size on the mechanical and tribological characteristics of TiO\u003csub\u003e2\u003c/sub\u003e reinforced epoxy composites, Journal of Materials Research and Technology, Volume 26, Pages 6001\u0026ndash;6015\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eTawfik A. Saleh, Nagaraj P. Shetti, Mahesh M. Shanbhag, Kakarla Raghava Reddy, Tejraj M. Aminabhavi (2020) Recent trends in functionalized nanoparticles loaded polymeric composites: An energy application, Materials Science for Energy Technologies,Volume 3 Pages 515\u0026ndash;525\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"journal-of-sol-gel-science-and-technology","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jsst","sideBox":"Learn more about [Journal of Sol-Gel Science and Technology](https://www.springer.com/journal/10971)","snPcode":"10971","submissionUrl":"https://submission.springernature.com/new-submission/10971/3","title":"Journal of Sol-Gel Science and Technology","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Sustainable Synthesis, Sol-gel, Eco-Friendly, Nanostructured Ceramics, Low-Energy processing","lastPublishedDoi":"10.21203/rs.3.rs-8912633/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8912633/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe present work reports the production of BaTiO\u003csub\u003e3\u003c/sub\u003e ceramic nanostructures through a sustainable sol-gel synthesis route that drastically reduces energy demand while improving phase purity. Two synthesis strategies were compared: (A) a conventional route based on Ba(OH)₂ under controlled humidity and inert conditions, and (B) a modified route employing BaCl₂ as precursor under ambient atmosphere. This optimized method achieved an ~81% reduction in energy consumption, decreasing synthesis from 180 °C for 24 h to 130 °C for 3 h. Importantly, carbon-related impurities were significantly suppressed, obviating the need for post-synthesis acid washing treatments. Structural and morphological analyses (FT-IR, XRD with Rietveld refinement, FE-SEM, chemical mapping, and BET) confirmed enhanced phase purity, a drastic reduction particle size (~100 nm to ~25 nm), and high surface area high surface area (\u0026gt; 50 m\u003csup\u003e2\u003c/sup\u003e/g). This methode provided a scalable and environmentally responsible pathway that allows the scalable production of high-purity BaTiO₃, advancing sustainable materials processing for electronic and energy-related applications.\u003c/p\u003e","manuscriptTitle":"A Rapid Sustainable Sol-Gel Synthesis of Phase-Pure BaTiO₃ Nanostructures with Minimal Energy Demand","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2026-02-26 07:42:00","doi":"10.21203/rs.3.rs-8912633/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2026-03-09T08:54:55+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-09T08:18:46+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-04T23:09:43+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"59847034950288593027828227969844910689","date":"2026-02-24T22:40:43+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"286007115483611905027144487543976470903","date":"2026-02-24T11:45:13+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2026-02-24T09:44:18+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2026-02-19T10:48:19+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2026-02-19T10:46:51+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Sol-Gel Science and Technology","date":"2026-02-18T22:25:16+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-sol-gel-science-and-technology","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jsst","sideBox":"Learn more about [Journal of Sol-Gel Science and Technology](https://www.springer.com/journal/10971)","snPcode":"10971","submissionUrl":"https://submission.springernature.com/new-submission/10971/3","title":"Journal of Sol-Gel Science and Technology","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"753e9eac-e365-42a4-b1c7-9679c9f1ad11","owner":[],"postedDate":"February 26th, 2026","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2026-04-04T14:39:16+00:00","versionOfRecord":[],"versionCreatedAt":"2026-02-26 07:42:00","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-8912633","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8912633","identity":"rs-8912633","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}