Pub Date : 2025-10-06DOI: 10.1007/s10971-025-06944-w
Minakshi Chaudhary, Rajesh K. Yadav, Rehana Shahin, Shaifali Mishra, Kanchan Sharma, Surendra K. Jaiswal, Arun Kumar Dubey, D. K. Dwivedi, Alok Kumar Singh, Jin-Ook Baeg
This work reports a novel method for enhancing solar energy applications by synthesizing high-performance nanostructured PPy@AF hydrogel as photocatalyst under controlled conditions. The incorporation of acid fuchsin (AF) as a dopant into polypyrrole (PPy) imparts unique supramolecular properties to the hydrogels, enabling efficient chemical transformations, including C-H bond activation. The incorporation of AF as a dopant into PPy imparts unique supramolecular properties to the hydrogels, enabling efficient chemical transformations, including C-H bond activation. These dopant-enhanced hydrogel frameworks exhibit superior catalytic efficiency, offering a sustainable and eco-friendly solution for energy conversion processes. The study highlights the synergistic impact of dopant inclusion in enhancing the stability, selectivity, and reaction kinetics of the hydrogels. This innovation has the potential to contribute to the development of advanced materials in solar energy systems, where efficient catalytic reactions are essential. Overall, the findings support the advancement of high-performance, dopant-modified nanostructured hydrogels with promising applications in renewable energy and green chemistry.
{"title":"Empowering solar energy: controlled synthesis of high-performance nanostructured hydrogel through dopant-enabled supramolecule innovation for organic transformations","authors":"Minakshi Chaudhary, Rajesh K. Yadav, Rehana Shahin, Shaifali Mishra, Kanchan Sharma, Surendra K. Jaiswal, Arun Kumar Dubey, D. K. Dwivedi, Alok Kumar Singh, Jin-Ook Baeg","doi":"10.1007/s10971-025-06944-w","DOIUrl":"10.1007/s10971-025-06944-w","url":null,"abstract":"<div><p>This work reports a novel method for enhancing solar energy applications by synthesizing high-performance nanostructured PPy@AF hydrogel as photocatalyst under controlled conditions. The incorporation of acid fuchsin (AF) as a dopant into polypyrrole (PPy) imparts unique supramolecular properties to the hydrogels, enabling efficient chemical transformations, including C-H bond activation. The incorporation of AF as a dopant into PPy imparts unique supramolecular properties to the hydrogels, enabling efficient chemical transformations, including C-H bond activation. These dopant-enhanced hydrogel frameworks exhibit superior catalytic efficiency, offering a sustainable and eco-friendly solution for energy conversion processes. The study highlights the synergistic impact of dopant inclusion in enhancing the stability, selectivity, and reaction kinetics of the hydrogels. This innovation has the potential to contribute to the development of advanced materials in solar energy systems, where efficient catalytic reactions are essential. Overall, the findings support the advancement of high-performance, dopant-modified nanostructured hydrogels with promising applications in renewable energy and green chemistry.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 3","pages":"2225 - 2237"},"PeriodicalIF":3.2,"publicationDate":"2025-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145675589","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-06DOI: 10.1007/s10971-025-06969-1
Huda J. Abdulhussein, Ali M. Mohammad
Over the past few decades, the issue of toxic and reactive gases has been of concern for environmental safety and human health, which in turn has led to ongoing developments in gas detection technology. Spinel ferrites are well known as suitable candidates for gas sensing. This study examines ZnxCu0.2-xMn0.8Fe2O4 (x = 0.0 to 0.2) nanoparticles, including their synthesis by sol-gel processing, characterization, and gas-sensing properties, as a sensor for nitrogen dioxide (NO2). The formation of a cubic spinel structure was confirmed by X-ray diffraction analysis, with the crystallite size decreasing from 73 nm to 67 nm with increasing zinc content. Field emission scanning electron microscopy revealed a decrease in particle size with increasing Zn content, which contributed to increased surface area and porosity. The presence of distinct absorption bands in the Fourier transform infrared spectra at 597–613 cm−1 and 389–401 cm−1 was attributed to metal-oxygen vibrations in the spinel configuration. The gas response of ZnxCu0.2-xMn0.8Fe2O4 nanoparticles exhibited improved sensitivity due to increased surface area as the crystallite size decreased, and the sensors exhibited a strong response towards NO2 in gas sensing tests. The best performance was observed with Zn0.2Mn0.8Fe2O4, exhibiting higher sensitivity and shorter response time. These results suggest that ZnxCu0.2-xMn0.8Fe2O4 ferrites are viable candidates for high-performance NO2 gas sensors, with implications for understanding gas-sensing behavior associated with tuning composition and structural properties.
{"title":"Zn-substituted CuMn ferrite nanoparticles for enhanced NO2 gas sensing: synthesis, characterization, and high-performance","authors":"Huda J. Abdulhussein, Ali M. Mohammad","doi":"10.1007/s10971-025-06969-1","DOIUrl":"10.1007/s10971-025-06969-1","url":null,"abstract":"<div><p>Over the past few decades, the issue of toxic and reactive gases has been of concern for environmental safety and human health, which in turn has led to ongoing developments in gas detection technology. Spinel ferrites are well known as suitable candidates for gas sensing. This study examines Zn<sub><i>x</i></sub>Cu<sub>0.2-<i>x</i></sub>Mn<sub>0.8</sub>Fe<sub>2</sub>O<sub>4</sub> (<i>x</i> = 0.0 to 0.2) nanoparticles, including their synthesis by sol-gel processing, characterization, and gas-sensing properties, as a sensor for nitrogen dioxide (NO<sub>2</sub>). The formation of a cubic spinel structure was confirmed by X-ray diffraction analysis, with the crystallite size decreasing from 73 nm to 67 nm with increasing zinc content. Field emission scanning electron microscopy revealed a decrease in particle size with increasing Zn content, which contributed to increased surface area and porosity. The presence of distinct absorption bands in the Fourier transform infrared spectra at 597–613 cm<sup>−1</sup> and 389–401 cm<sup>−1</sup> was attributed to metal-oxygen vibrations in the spinel configuration. The gas response of Zn<sub><i>x</i></sub>Cu<sub>0.2-<i>x</i></sub>Mn<sub>0.8</sub>Fe<sub>2</sub>O<sub>4</sub> nanoparticles exhibited improved sensitivity due to increased surface area as the crystallite size decreased, and the sensors exhibited a strong response towards NO<sub>2</sub> in gas sensing tests. The best performance was observed with Zn<sub>0.2</sub>Mn<sub>0.8</sub>Fe<sub>2</sub>O<sub>4</sub>, exhibiting higher sensitivity and shorter response time. These results suggest that Zn<sub><i>x</i></sub>Cu<sub>0.2-<i>x</i></sub>Mn<sub>0.8</sub>Fe<sub>2</sub>O<sub>4</sub> ferrites are viable candidates for high-performance NO<sub>2</sub> gas sensors, with implications for understanding gas-sensing behavior associated with tuning composition and structural properties.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 3","pages":"1764 - 1774"},"PeriodicalIF":3.2,"publicationDate":"2025-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145675590","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-03DOI: 10.1007/s10971-025-06959-3
Wang Zhenzhen, Ouyang Chunming, Feng Zhihui, Ma Yongcun, Peng Shusen
Organic-inorganic hybrid sol-gel coatings are effective and environmentally friendly alternatives to chromium(VI) pretreatment for aluminum alloys. The advantage of preparing coatings via the sol-gel method is that it allows obtaining coatings with optimized properties by varying synthesis parameters. In this work, a γ-GPS-ZrO2 hybrid sol for surface pretreatment of AA2024-T3 was prepared by mixing pre-synthesized nano-zirconia (ZrO2) sol into hydrolyzed γ-glycidyl etheroxypropyltrimethoxysilane (γ-GPS). Sol-gels with Si-Zr molar ratios of 2, 3, and 4 were applied to the aluminum alloy surface by coating and cured in an oven at 70 °C to form films. Electrochemical impedance spectroscopy (EIS) was used to evaluate the corrosion behavior of the sol-gel coatings on the aluminum alloy surface in 0.5 M NaCl solution. The morphology and chemical structure of the prepared hybrid coatings were analyzed by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Results show that increasing the Zr-Si molar ratio enhances the crosslinked inorganic network in the sols, leading to increased initial coating resistance and corrosion resistance. However, this also reduces the connectivity of the organic network, enhancing coating hydrophilicity and promoting water-induced degradation, which negatively impacts corrosion resistance. In this study, balancing these opposing trends (corrosion resistance vs. hydrophilicity) was achieved at a Si-Zr molar ratio of 3, yielding coatings with optimal comprehensive performance.
有机-无机复合溶胶-凝胶涂层是替代铬(VI)对铝合金进行预处理的有效环保涂料。溶胶-凝胶法制备涂料的优点是可以通过不同的合成参数得到性能最优的涂料。本文将预合成的纳米氧化锆(ZrO2)溶胶与水解的γ-缩水甘油酯醚氧丙基三甲氧基硅烷(γ-GPS)混合,制备了用于AA2024-T3表面预处理的γ-GPS-ZrO2杂化溶胶。将Si-Zr摩尔比分别为2、3和4的溶胶-凝胶涂覆在铝合金表面,在70℃的烘箱中固化成膜。采用电化学阻抗谱(EIS)评价了溶胶-凝胶涂层在0.5 M NaCl溶液中对铝合金表面的腐蚀行为。采用扫描电镜(SEM)、能谱(EDS)、傅里叶变换红外光谱(FTIR)和x射线光电子能谱(XPS)分析了复合涂层的形貌和化学结构。结果表明,Zr-Si摩尔比的增加增强了溶胶中的交联无机网络,从而提高了初始涂层耐蚀性和耐腐蚀性。然而,这也降低了有机网络的连通性,增强了涂层的亲水性,促进了水致降解,这对耐腐蚀性产生了负面影响。在这项研究中,在Si-Zr摩尔比为3的情况下,平衡了这两种相反的趋势(耐腐蚀性和亲水性),得到了综合性能最佳的涂层。
{"title":"Preparation of γ-GPS-ZrO2 hybrid coating by sol-gel method and its synergistic enhancement effect on corrosion resistance and adhesion of AA2024 aluminum alloy","authors":"Wang Zhenzhen, Ouyang Chunming, Feng Zhihui, Ma Yongcun, Peng Shusen","doi":"10.1007/s10971-025-06959-3","DOIUrl":"10.1007/s10971-025-06959-3","url":null,"abstract":"<div><p>Organic-inorganic hybrid sol-gel coatings are effective and environmentally friendly alternatives to chromium(VI) pretreatment for aluminum alloys. The advantage of preparing coatings via the sol-gel method is that it allows obtaining coatings with optimized properties by varying synthesis parameters. In this work, a γ-GPS-ZrO<sub>2</sub> hybrid sol for surface pretreatment of AA2024-T3 was prepared by mixing pre-synthesized nano-zirconia (ZrO<sub>2</sub>) sol into hydrolyzed γ-glycidyl etheroxypropyltrimethoxysilane (γ-GPS). Sol-gels with Si-Zr molar ratios of 2, 3, and 4 were applied to the aluminum alloy surface by coating and cured in an oven at 70 °C to form films. Electrochemical impedance spectroscopy (EIS) was used to evaluate the corrosion behavior of the sol-gel coatings on the aluminum alloy surface in 0.5 M NaCl solution. The morphology and chemical structure of the prepared hybrid coatings were analyzed by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Results show that increasing the Zr-Si molar ratio enhances the crosslinked inorganic network in the sols, leading to increased initial coating resistance and corrosion resistance. However, this also reduces the connectivity of the organic network, enhancing coating hydrophilicity and promoting water-induced degradation, which negatively impacts corrosion resistance. In this study, balancing these opposing trends (corrosion resistance vs. hydrophilicity) was achieved at a Si-Zr molar ratio of 3, yielding coatings with optimal comprehensive performance.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 2","pages":"1432 - 1450"},"PeriodicalIF":3.2,"publicationDate":"2025-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145612270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-02DOI: 10.1007/s10971-025-06960-w
Basem Al Alwan, Mohammad Ashraf Hossain, Atef EL Jery, Saba Firdous, Md Rezaul Karim, Ismail Hossain, Muhammad Jamshaid
Water pollution from industrial effluents remains a major global challenge and demands effective and eco-friendly treatment plans. In this work, we report for the first time the integration of micro–nanobubble (MNB) technology with a ternary PbFe12O19/g-C3N4/rGO (PGR) nanocomposite for photocatalytic dye degradation and antibacterial applications. The PGR nanocomposite was synthesized via a hydrothermal process and systematically characterized by XRD, SEM, Raman and FTIR analyses. The band gap of pristine PbFe₁₂O₁₉ (2.94 eV) was successfully tuned in the composite (2.40 eV). The PGR nanocomposite achieved rapid degradation of methyl orange (95%) and crystal violet (98%) following pseudo-first-order kinetics with rate constants of 0.024 and 0.022 min⁻¹ respectively. The unique synergy between rGO-mediated charge transfer, g-C₃N₄ sensitization and MNB-induced reactive oxygen species generation led to enhanced electron mobility, suppressed recombination and superior catalytic efficiency. Moreover, the composite exhibited strong antibacterial activity against Staphylococcus aureus and Pseudomonas aeruginosa. This study introduces a novel micro–nanobubble driven photocatalytic platform, offering a promising and sustainable route for wastewater purification coupled with antibacterial functionality.
{"title":"Micro–nanobubble-assisted photocatalytic and antibacterial performance of rGO- modified PbFe₁₂O₁₉/g-C₃N₄ nanocomposites","authors":"Basem Al Alwan, Mohammad Ashraf Hossain, Atef EL Jery, Saba Firdous, Md Rezaul Karim, Ismail Hossain, Muhammad Jamshaid","doi":"10.1007/s10971-025-06960-w","DOIUrl":"10.1007/s10971-025-06960-w","url":null,"abstract":"<div><p>Water pollution from industrial effluents remains a major global challenge and demands effective and eco-friendly treatment plans. In this work, we report for the first time the integration of micro–nanobubble (MNB) technology with a ternary PbFe<sub>12</sub>O<sub>19</sub>/g-C<sub>3</sub>N<sub>4</sub>/rGO (PGR) nanocomposite for photocatalytic dye degradation and antibacterial applications. The PGR nanocomposite was synthesized via a hydrothermal process and systematically characterized by XRD, SEM, Raman and FTIR analyses. The band gap of pristine PbFe₁₂O₁₉ (2.94 eV) was successfully tuned in the composite (2.40 eV). The PGR nanocomposite achieved rapid degradation of methyl orange (95%) and crystal violet (98%) following pseudo-first-order kinetics with rate constants of 0.024 and 0.022 min⁻¹ respectively. The unique synergy between rGO-mediated charge transfer, g-C₃N₄ sensitization and MNB-induced reactive oxygen species generation led to enhanced electron mobility, suppressed recombination and superior catalytic efficiency. Moreover, the composite exhibited strong antibacterial activity against <i>Staphylococcus aureus</i> and <i>Pseudomonas aeruginosa</i>. This study introduces a novel micro–nanobubble driven photocatalytic platform, offering a promising and sustainable route for wastewater purification coupled with antibacterial functionality.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 2","pages":"1419 - 1431"},"PeriodicalIF":3.2,"publicationDate":"2025-10-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145612246","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-01DOI: 10.1007/s10971-025-06961-9
Abdullah M. Aldukhayel
This work targets a clear structure–property link in BaMn0.5Ti0.5O3 (BMTO) by correlating sol–gel–derived crystal chemistry with temperature-dependent dielectric and electrical responses. Phase-pure rhombohedral perovskite (R3c) was confirmed by Rietveld refinement, with nanoscale crystallites (≈45–47 nm) and dense microstructure (≈124 nm grains) evidenced by XRD/SEM; EDS verified near-stoichiometric composition. Dielectric spectra (1 kHz–1 MHz, 200–320 K) show strong frequency dispersion, ε′ decreases with frequency but increase systematically with temperature, consistent with Maxwell–Wagner interfacial polarization and thermally activated hopping. AC conductivity follows Jonscher’s power law and rises with temperature, indicating small-polaron hopping and overall negative temperature coefficient of resistance behavior. Impedance and modulus analyses reveal non-Debye relaxation dominated by grain-boundary processes; Nyquist plots are well described by an Rs–(Rgb||CPE) equivalent circuit, with grain-boundary resistance falling from ~255 Ω (200 K) to ~55 Ω (320 K) and the relaxation frequency shifting from ~3 kHz to ~30 kHz as temperature increases, while the CPE exponent approaches unity (0.86 → 0.93), indicating more ideal capacitive behavior at higher temperatures. These results show that B-site Mn/Ti substitution and associated defect chemistry (octahedral tilts, oxygen-vacancy assisted hopping) govern polarization and transport. BMTO therefore offers thermally tunable dielectric response and semiconducting conduction desirable for capacitors, sensors, and other multifunctional electronic components.
{"title":"Sol–gel synthesized BaMn0.5Ti0.5O3 perovskite: structural, dielectric, and electrical properties with temperature-dependent analysis","authors":"Abdullah M. Aldukhayel","doi":"10.1007/s10971-025-06961-9","DOIUrl":"10.1007/s10971-025-06961-9","url":null,"abstract":"<div><p>This work targets a clear structure–property link in BaMn<sub>0.5</sub>Ti<sub>0.5</sub>O<sub>3</sub> (BMTO) by correlating sol–gel–derived crystal chemistry with temperature-dependent dielectric and electrical responses. Phase-pure rhombohedral perovskite (R3c) was confirmed by Rietveld refinement, with nanoscale crystallites (≈45–47 nm) and dense microstructure (≈124 nm grains) evidenced by XRD/SEM; EDS verified near-stoichiometric composition. Dielectric spectra (1 kHz–1 MHz, 200–320 K) show strong frequency dispersion, ε′ decreases with frequency but increase systematically with temperature, consistent with Maxwell–Wagner interfacial polarization and thermally activated hopping. AC conductivity follows Jonscher’s power law and rises with temperature, indicating small-polaron hopping and overall negative temperature coefficient of resistance behavior. Impedance and modulus analyses reveal non-Debye relaxation dominated by grain-boundary processes; Nyquist plots are well described by an R<sub>s</sub>–(R<sub>gb</sub>||CPE) equivalent circuit, with grain-boundary resistance falling from ~255 Ω (200 K) to ~55 Ω (320 K) and the relaxation frequency shifting from ~3 kHz to ~30 kHz as temperature increases, while the CPE exponent approaches unity (0.86 → 0.93), indicating more ideal capacitive behavior at higher temperatures. These results show that B-site Mn/Ti substitution and associated defect chemistry (octahedral tilts, oxygen-vacancy assisted hopping) govern polarization and transport. BMTO therefore offers thermally tunable dielectric response and semiconducting conduction desirable for capacitors, sensors, and other multifunctional electronic components.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 2","pages":"1401 - 1418"},"PeriodicalIF":3.2,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145612237","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-09-30DOI: 10.1007/s10971-025-06957-5
P. Alastuey, E. G. Gioria, J. P. Monteza Basaldúa, A. V. Bordoni, A. Wolosiuk
In the last decades, alkoxide sol-gel chemistry provided an exceptional tool for the synthesis of nanostructured building blocks and designing application of novel materials. To keep up with the latest advancements in this field, a group of Argentine researchers established the Buenos Aires School of Materials Synthesis and Sol-Gel Processes, which has been held every 2 years at Buenos Aires—Argentina, since 2003. The course, aimed at young graduate students, postdoctoral researchers, and industry professionals, focuses on both the fundamentals and the newest developments of sol-gel processes. Also, during 40 h of laboratory-based work, they become immersed in the typical techniques and skills in sol-gel synthesis and materials characterization. These “hands-on” experimental sessions are the defining feature of this school as they explore key sol-gel related processes: hydrolysis and condensation kinetics, wet-lab synthetic approaches, and materials characterization techniques. In the work presented here, the students employ the well-known Stöber´s method for obtaining SiO2 colloidal particles. Tetraethoxysilane hydrolysis and condensation kinetics are followed using a conductometer, and the time-dependent data obtained are interpreted using a simple consecutive reaction kinetics mechanism. Later, the students explore simple one-pot post-grafting colloidal surface chemical modifications, which are confirmed through infrared spectrometry and zeta-potential measurements. Carefully controlled additions of the alkoxide precursor allow for experimentation on increasing particle diameter, which can be readily confirmed using scanning electron microscopy. Moreover, encapsulation within the SiO2 framework with cationic luminescent dyes as [Ru(bpy)3]2+ results in photochemical hybrid platforms. In essence, this laboratory activity encompasses several sol-gel and colloidal chemistry concepts suited for an advanced chemical course on materials synthesis.
{"title":"Synthesis, characterization, and sol-gel kinetic studies of colloidal silica particles using Stöber’s method: a teaching laboratory activity","authors":"P. Alastuey, E. G. Gioria, J. P. Monteza Basaldúa, A. V. Bordoni, A. Wolosiuk","doi":"10.1007/s10971-025-06957-5","DOIUrl":"10.1007/s10971-025-06957-5","url":null,"abstract":"<div><p>In the last decades, alkoxide sol-gel chemistry provided an exceptional tool for the synthesis of nanostructured building blocks and designing application of novel materials. To keep up with the latest advancements in this field, a group of Argentine researchers established the Buenos Aires School of Materials Synthesis and Sol-Gel Processes, which has been held every 2 years at Buenos Aires—Argentina, since 2003. The course, aimed at young graduate students, postdoctoral researchers, and industry professionals, focuses on both the fundamentals and the newest developments of sol-gel processes. Also, during 40 h of laboratory-based work, they become immersed in the typical techniques and skills in sol-gel synthesis and materials characterization. These “hands-on” experimental sessions are the defining feature of this school as they explore key sol-gel related processes: hydrolysis and condensation kinetics, wet-lab synthetic approaches, and materials characterization techniques. In the work presented here, the students employ the well-known Stöber´s method for obtaining SiO<sub>2</sub> colloidal particles. Tetraethoxysilane hydrolysis and condensation kinetics are followed using a conductometer, and the time-dependent data obtained are interpreted using a simple consecutive reaction kinetics mechanism. Later, the students explore simple one-pot post-grafting colloidal surface chemical modifications, which are confirmed through infrared spectrometry and zeta-potential measurements. Carefully controlled additions of the alkoxide precursor allow for experimentation on increasing particle diameter, which can be readily confirmed using scanning electron microscopy. Moreover, encapsulation within the SiO<sub>2</sub> framework with cationic luminescent dyes as [Ru(bpy)<sub>3</sub>]<sup>2+</sup> results in photochemical hybrid platforms. In essence, this laboratory activity encompasses several sol-gel and colloidal chemistry concepts suited for an advanced chemical course on materials synthesis.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 3","pages":"2494 - 2504"},"PeriodicalIF":3.2,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145675601","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In the face of surging global energy demands and increasing environmental pollution, the development of efficient energy storage and conversion technologies has become critically important. In this study, a series of three-dimensional transition metal-doped Ni9S8/Co9S8 nanowire electrode materials were synthesized via a hydrothermal method, and their performance as supercapacitor electrodes and bifunctional electrocatalysts for water splitting was systematically investigated. The electronic structure and morphology of the materials were effectively modulated through doping with Cr, Ce, Fe, Mo, and W, leading to significantly enhanced electrochemical performance. Among them, the Cr–Ni9S8/Co9S8–0.04 electrode, with a Cr doping concentration of 0.04 mM, exhibited an areal specific capacitance of 1128 C cm-2 at 1 mA cm-2 and a gravimetric specific capacitance of 485 C g-1 at 1 A g-1. As an electrocatalyst, it delivered overpotentials of 227.6 mV for the oxygen evolution reaction (OER) and 117.4 mV for the hydrogen evolution reaction (HER) at 10 mA cm-2. Further comparative analysis of the effects of different transition metal dopants revealed that Mo-Ni9S8/Co9S8-0.04 exhibited the best overall performance, with OER and HER overpotentials reaching 161.6 mV and 125.4 mV, respectively. Additionally, its gravimetric and areal specific capacitances reached 674.5 C g-1 at 1 A g-1 and 1834 C cm-2 at 1 mA cm-2. Moreover, the Cr-Ni9S8/Co9S8-0.04 electrocatalyst required only 1.42 V to drive a current density of 10 mA cm-2 in overall water splitting, demonstrating excellent bifunctional catalytic activity. This study provides a novel strategy for synergistically modulating the electrochemical properties of sulfide composite materials through multi-element doping.
Graphical abstract
This paper reports the preparation of a series of three-dimensional transition metal-doped Ni9S8/Co9S8 nanowire electrode materials via a hydrothermal synthesis method, and systematically investigates their performance as bifunctional materials for supercapacitor electrodes and electrocatalytic water splitting.
面对日益增长的全球能源需求和日益严重的环境污染,开发高效的能源存储和转换技术变得至关重要。本研究通过水热法制备了一系列三维过渡金属掺杂Ni9S8/Co9S8纳米线电极材料,并对其作为超级电容器电极和双功能电催化剂的水裂解性能进行了系统研究。通过Cr、Ce、Fe、Mo和W的掺杂,有效地调控了材料的电子结构和形貌,从而显著提高了材料的电化学性能。其中,Cr掺杂浓度为0.04 mM的Cr - ni9s8 / Co9S8-0.04电极在1 mA cm-2时的面积比电容为1128 C cm-2,在1 a g-1时的重量比电容为485 C g-1。作为电催化剂,在10 mA cm-2下析氧反应(OER)和析氢反应(HER)的过电位分别为227.6 mV和117.4 mV。进一步对比分析不同过渡金属掺杂剂的影响,Mo-Ni9S8/Co9S8-0.04表现出最佳的综合性能,OER和HER过电位分别达到161.6 mV和125.4 mV。此外,在1 A g-1和1 mA cm-2下,其重量和面积比电容分别达到674.5 C g-1和1834 C cm-2。此外,Cr-Ni9S8/Co9S8-0.04电催化剂仅需要1.42 V就能驱动10 mA cm-2的电流密度,表现出优异的双功能催化活性。本研究为通过多元素掺杂协同调节硫化物复合材料的电化学性能提供了一种新的策略。摘要本文采用水热合成方法制备了一系列三维过渡金属掺杂Ni9S8/Co9S8纳米线电极材料,并系统研究了其作为超级电容器电极和电催化水分解双功能材料的性能。
{"title":"Dual-functional Ni9S8/Co9S8 nanowires for high-energy storage and efficient water splitting","authors":"Xin Li, Kai Jia, Zhekai Zhang, Bo-yao Zhang, Song-lin Xu, Zihan Lv, Shuang-shuang Zhang, Rong-da Zhao, Depeng Zhao, Menggang Li, Fu-fa Wu","doi":"10.1007/s10971-025-06951-x","DOIUrl":"10.1007/s10971-025-06951-x","url":null,"abstract":"<div><p>In the face of surging global energy demands and increasing environmental pollution, the development of efficient energy storage and conversion technologies has become critically important. In this study, a series of three-dimensional transition metal-doped Ni<sub>9</sub>S<sub>8</sub>/Co<sub>9</sub>S<sub>8</sub> nanowire electrode materials were synthesized via a hydrothermal method, and their performance as supercapacitor electrodes and bifunctional electrocatalysts for water splitting was systematically investigated. The electronic structure and morphology of the materials were effectively modulated through doping with Cr, Ce, Fe, Mo, and W, leading to significantly enhanced electrochemical performance. Among them, the Cr–Ni<sub>9</sub>S<sub>8</sub>/Co<sub>9</sub>S<sub>8</sub>–0.04 electrode, with a Cr doping concentration of 0.04 mM, exhibited an areal specific capacitance of 1128 C cm<sup>-2</sup> at 1 mA cm<sup>-2</sup> and a gravimetric specific capacitance of 485 C g<sup>-1</sup> at 1 A g<sup>-1</sup>. As an electrocatalyst, it delivered overpotentials of 227.6 mV for the oxygen evolution reaction (OER) and 117.4 mV for the hydrogen evolution reaction (HER) at 10 mA cm<sup>-2</sup>. Further comparative analysis of the effects of different transition metal dopants revealed that Mo-Ni<sub>9</sub>S<sub>8</sub>/Co<sub>9</sub>S<sub>8</sub>-0.04 exhibited the best overall performance, with OER and HER overpotentials reaching 161.6 mV and 125.4 mV, respectively. Additionally, its gravimetric and areal specific capacitances reached 674.5 C g<sup>-1</sup> at 1 A g<sup>-1</sup> and 1834 C cm<sup>-2</sup> at 1 mA cm<sup>-2</sup>. Moreover, the Cr-Ni<sub>9</sub>S<sub>8</sub>/Co<sub>9</sub>S<sub>8</sub>-0.04 electrocatalyst required only 1.42 V to drive a current density of 10 mA cm<sup>-2</sup> in overall water splitting, demonstrating excellent bifunctional catalytic activity. This study provides a novel strategy for synergistically modulating the electrochemical properties of sulfide composite materials through multi-element doping.</p><h3>Graphical abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>This paper reports the preparation of a series of three-dimensional transition metal-doped Ni<sub>9</sub>S<sub>8</sub>/Co<sub>9</sub>S<sub>8</sub> nanowire electrode materials via a hydrothermal synthesis method, and systematically investigates their performance as bifunctional materials for supercapacitor electrodes and electrocatalytic water splitting.</p></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 2","pages":"1041 - 1057"},"PeriodicalIF":3.2,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145612993","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-09-30DOI: 10.1007/s10971-025-06946-8
Redha A. Alkhadry, Ibrahim S. Yahia, Souad A. Elfeky, Walid Tawfik, M. I. Mohammed, Diaa A. Rayan, Mostafa Zedan
The synergistic effects of population growth, industrialization, and urbanization drive an increase in environmental crises, such as water pollution. Polymeric nanocomposites (PNCs) offer a promising trend for large-scale applications in environmental remediation including photocatalytic water pollutants. In this work, V2O5 nanoparticles were synthesized using the sol-gel method and successfully incorporated into PMMA using the casting method. A series of V2O5/PMMA photocatalyst films have been fabricated with various loading content of V2O5 NPs. The morphological, crystal structure, and optical properties of the prepared V2O5/PMMA photocatalysts were characterized using SEM, XRD, FTIR, and UV-Vis spectrophotometry, respectively. The SEM images indicate that there are mainly physical interactions between PMMA and V2O5 NPs. Moreover, the prepared V2O5/PMMA films before and after treatment with H2O2 + UV were evaluated toward MB photodegradation under UV irradiation. The results obtained showed that doping V2O5 NPs into PMMA could inhibit the recombination rate of the photogenerated charge carriers. Among all prepared catalysts, the highest photocatalytic performance toward MB degradation under UV irradiation was obtained using the treated P-VPO1 nanocomposite film (0.033% V2O5/PMMA) compared to other formulations. Approximately 80% of MB was degraded after 60 min of UV irradiation in the presence of the treated P-VPO1. The enhanced photocatalytic activity was ascribed to the promoting effect of the H2O2 + UV treatment for the prepared V2O5 doped PMMA films and with an appropriate loading amount of V2O5 NPs. Moreover, the P-VPO1 shows good reusability and stability for MB dye photodegradation after five consecutive runs under UV irradiation. This study reported a straightforward, and rapid approach to fabricate an improved V2O5/PMMA nanocomposite films with excellent reusability and attractive photocatalytic properties for diverse environmental applications, including water treatment.
{"title":"Novel synthesized V2O5-doped PMMA nanocomposite films for effective photocatalytic removal of methylene blue from water","authors":"Redha A. Alkhadry, Ibrahim S. Yahia, Souad A. Elfeky, Walid Tawfik, M. I. Mohammed, Diaa A. Rayan, Mostafa Zedan","doi":"10.1007/s10971-025-06946-8","DOIUrl":"10.1007/s10971-025-06946-8","url":null,"abstract":"<p>The synergistic effects of population growth, industrialization, and urbanization drive an increase in environmental crises, such as water pollution. Polymeric nanocomposites (PNCs) offer a promising trend for large-scale applications in environmental remediation including photocatalytic water pollutants. In this work, V<sub>2</sub>O<sub>5</sub> nanoparticles were synthesized using the sol-gel method and successfully incorporated into PMMA using the casting method. A series of V<sub>2</sub>O<sub>5</sub>/PMMA photocatalyst films have been fabricated with various loading content of V<sub>2</sub>O<sub>5</sub> NPs. The morphological, crystal structure, and optical properties of the prepared V<sub>2</sub>O<sub>5</sub>/PMMA photocatalysts were characterized using SEM, XRD, FTIR, and UV-Vis spectrophotometry, respectively. The SEM images indicate that there are mainly physical interactions between PMMA and V<sub>2</sub>O<sub>5</sub> NPs. Moreover, the prepared V<sub>2</sub>O<sub>5</sub>/PMMA films before and after treatment with H<sub>2</sub>O<sub>2</sub> + UV were evaluated toward MB photodegradation under UV irradiation. The results obtained showed that doping V<sub>2</sub>O<sub>5</sub> NPs into PMMA could inhibit the recombination rate of the photogenerated charge carriers. Among all prepared catalysts, the highest photocatalytic performance toward MB degradation under UV irradiation was obtained using the treated P-VPO1 nanocomposite film (0.033% V<sub>2</sub>O<sub>5</sub>/PMMA) compared to other formulations. Approximately 80% of MB was degraded after 60 min of UV irradiation in the presence of the treated P-VPO1. The enhanced photocatalytic activity was ascribed to the promoting effect of the H<sub>2</sub>O<sub>2</sub> + UV treatment for the prepared V<sub>2</sub>O<sub>5</sub> doped PMMA films and with an appropriate loading amount of V<sub>2</sub>O<sub>5</sub> NPs. Moreover, the P-VPO1 shows good reusability and stability for MB dye photodegradation after five consecutive runs under UV irradiation. This study reported a straightforward, and rapid approach to fabricate an improved V<sub>2</sub>O<sub>5</sub>/PMMA nanocomposite films with excellent reusability and attractive photocatalytic properties for diverse environmental applications, including water treatment.</p>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 3","pages":"2025 - 2041"},"PeriodicalIF":3.2,"publicationDate":"2025-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10971-025-06946-8.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145675602","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-09-29DOI: 10.1007/s10971-025-06943-x
Hakan Kızıltaş
In this study, AgFe2O4/ZnO composites were synthesized, characterized, and evaluated for their photocatalytic performance. XRD analysis confirmed the formation of crystalline ZnO, AgFe2O4, and AgFe2O4/ZnO composites, with calculated crystallite sizes of 7, 8, and 10 nm, respectively. SEM and TEM analyses showed a uniform particle distribution with minimal agglomeration and well-defined interfaces, indicating stable morphology and effective particle integration. EDS and XPS confirmed the homogeneous distribution of Zn, Fe, Ag, and O elements, supporting efficient charge transfer. PL analysis showed reduced emission intensity in the composite, suggesting suppressed electron-hole recombination and enhanced charge separation due to the heterojunction between AgFe2O4 and ZnO. Photocatalytic tests demonstrated that the AgFe2O4/ZnO composite achieved over 80% degradation efficiency for organic pollutants within 120 minutes, outperforming pure ZnO. Recyclability tests indicated that the composite retained over 97% of its efficiency after ten cycles, demonstrating long-term stability. The scavenger experiments identified •OH and •O2- radicals as the principal reactive oxygen species, confirming their central role in the photocatalytic degradation pathway. VSM analysis revealed weak ferromagnetism, enabling efficient magnetic separation and enhancing the material’s reusability in photocatalytic applications. The novelty of this work lies in the synthesis of AgFe2O4/ZnO heterojunction nanocomposites, which have not been previously reported in the literature. These materials exhibit enhanced charge separation and excellent stability for repeated photocatalytic applications. These findings suggest that AgFe2O4/ZnO composites are promising materials for sustainable wastewater treatment through photocatalytic degradation of organic pollutants.
{"title":"AgFe2O4/ZnO-based nanocomposites: synthesis, characterization, and photocatalytic performance","authors":"Hakan Kızıltaş","doi":"10.1007/s10971-025-06943-x","DOIUrl":"10.1007/s10971-025-06943-x","url":null,"abstract":"<div><p>In this study, AgFe<sub>2</sub>O<sub>4</sub>/ZnO composites were synthesized, characterized, and evaluated for their photocatalytic performance. XRD analysis confirmed the formation of crystalline ZnO, AgFe<sub>2</sub>O<sub>4,</sub> and AgFe<sub>2</sub>O<sub>4</sub>/ZnO composites, with calculated crystallite sizes of 7, 8, and 10 nm, respectively. SEM and TEM analyses showed a uniform particle distribution with minimal agglomeration and well-defined interfaces, indicating stable morphology and effective particle integration. EDS and XPS confirmed the homogeneous distribution of Zn, Fe, Ag, and O elements, supporting efficient charge transfer. PL analysis showed reduced emission intensity in the composite, suggesting suppressed electron-hole recombination and enhanced charge separation due to the heterojunction between AgFe<sub>2</sub>O<sub>4</sub> and ZnO. Photocatalytic tests demonstrated that the AgFe<sub>2</sub>O<sub>4</sub>/ZnO composite achieved over 80% degradation efficiency for organic pollutants within 120 minutes, outperforming pure ZnO. Recyclability tests indicated that the composite retained over 97% of its efficiency after ten cycles, demonstrating long-term stability. The scavenger experiments identified •OH and •O<sub>2</sub><sup>-</sup> radicals as the principal reactive oxygen species, confirming their central role in the photocatalytic degradation pathway. VSM analysis revealed weak ferromagnetism, enabling efficient magnetic separation and enhancing the material’s reusability in photocatalytic applications. The novelty of this work lies in the synthesis of AgFe<sub>2</sub>O<sub>4</sub>/ZnO heterojunction nanocomposites, which have not been previously reported in the literature. These materials exhibit enhanced charge separation and excellent stability for repeated photocatalytic applications. These findings suggest that AgFe<sub>2</sub>O<sub>4</sub>/ZnO composites are promising materials for sustainable wastewater treatment through photocatalytic degradation of organic pollutants.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 3","pages":"2010 - 2024"},"PeriodicalIF":3.2,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145675629","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
As dangerous vectors, mosquitoes pose a serious risk to both human and animal populations worldwide by transmitting dangerous viruses into uninhabitable areas. Because of the emergence of insecticide resistance, controlling the use of synthetic pesticides is essential. S. diastaticus was used in this investigation for the actinobacterial-mediated biosynthesis of Se-NPs. The biosynthesized Se-NPs were characterized using a variety of techniques, including UV, XRD, FT-IR, SEM with EDX, TEM, DLS, and zeta potential. The biosynthesized Se-NPs were effective against C. quinquefasciatus, A. stephensi, and A. aegypti, with LC50 values of 8.13 µg/mL, 9.36 µg/mL, and 13.71 µg/mL, respectively. The highest concentration of Se-NPs revealed high pupicidal activity and increased larval pupal duration against all three mosquito species. The effect of Se-NPs considerably increased the SOD and GPx levels but drastically decreased the AChE and GST level after 24 h of treatment. Histopathological analyses of the treated larvae revealed damaged epithelial cells, peritrophic membranes, and gut cells as compared to the control group. Additionally, A. salina showed low mortality. Conclusively, the biosynthesized Se-NPs using S. diastaticus were used as a potential biopesticide for controlling C. quinquefasciatus, A. stephensi, and A. aegypti.
{"title":"Evaluation of the larvicidal potential of selenium nanoparticles synthesized using Streptomyces diastaticus (KA-21) (OM758168) and their toxicity against the larvae of Culex quinquefasciatus, Aedes aegypti and Anopheles stephensi","authors":"Manickam Kalpana, Krishnan Raguvaran, Thulasiraman Manimegalai, Suresh Kalaivani, Palanisamy Devapriya, Rajan Maheswaran","doi":"10.1007/s10971-025-06953-9","DOIUrl":"10.1007/s10971-025-06953-9","url":null,"abstract":"<div><p>As dangerous vectors, mosquitoes pose a serious risk to both human and animal populations worldwide by transmitting dangerous viruses into uninhabitable areas. Because of the emergence of insecticide resistance, controlling the use of synthetic pesticides is essential. <i>S. diastaticus</i> was used in this investigation for the actinobacterial-mediated biosynthesis of Se-NPs. The biosynthesized Se-NPs were characterized using a variety of techniques, including UV, XRD, FT-IR, SEM with EDX, TEM, DLS, and zeta potential. The biosynthesized Se-NPs were effective against <i>C. quinquefasciatus</i>, <i>A. stephensi</i>, and <i>A. aegypti</i>, with LC<sub>50</sub> values of 8.13 µg/mL, 9.36 µg/mL, and 13.71 µg/mL, respectively. The highest concentration of Se-NPs revealed high pupicidal activity and increased larval pupal duration against all three mosquito species. The effect of Se-NPs considerably increased the SOD and GPx levels but drastically decreased the AChE and GST level after 24 h of treatment. Histopathological analyses of the treated larvae revealed damaged epithelial cells, peritrophic membranes, and gut cells as compared to the control group. Additionally, <i>A. salina</i> showed low mortality. Conclusively, the biosynthesized Se-NPs using <i>S. diastaticus</i> were used as a potential biopesticide for controlling <i>C. quinquefasciatus</i>, <i>A. stephensi</i>, and <i>A. aegypti</i>.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"116 2","pages":"1024 - 1040"},"PeriodicalIF":3.2,"publicationDate":"2025-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145613061","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}