Pub Date : 2024-08-29DOI: 10.1007/s10971-024-06525-3
Fouad El Aychaoui, Abdelhalim El Basset, Mohamed Naji, Mohammed Bouzid, Abdelilah Rjeb, Lahoucine Hajji, Yahya Ababou
In this paper, we studied the effect of lithium doping on the structural, microstructural, dielectric, and electrical properties of Ba1-xLixTiO3-δ (BTLx) ceramics prepared via the sol-gel method, with x = 0, 0.01, 0.03, 0.05, 0.07 and 0.09. The results obtained from Rietveld refinement of X-ray diffraction, infrared spectroscopy, and Raman spectroscopy show that all the samples crystallize in the tetragonal phase. Dielectric measurements show that increasing the lithium doping rate results in lower dielectric losses (from 0.04 for x = 0 to 0.008 for x = 0.09 at room temperature) and lower transition temperature Tm for compositions with x ≤ 0.07. The phase transition diffusivity parameter γ varies between 1 and 1.39, showing that our samples exhibit a diffuse phase transition but far from relaxor behavior. Complex impedance spectroscopy indicates that the grain boundary resistance of the materials is predominant in the electrical behavior of the materials. The activation energy Ea was calculated at 10 kHz by linear fitting of the temperature dependence of conductivity using the Arrhenius formula. The obtained values indicate that conduction for compositions with 0 ≤ x ≤ 0.05 occurs through free electrons originating from the ionization of oxygen vacancies, while for the compositions with x = 0.07 and 0.09, the predominant conduction mechanism is ionic conduction.
Graphical Abstract
本文研究了锂掺杂对溶胶-凝胶法制备的 Ba1-xLixTiO3-δ (BTLx) 陶瓷(x = 0、0.01、0.03、0.05、0.07 和 0.09)的结构、微观结构、介电和电气性能的影响。通过对 X 射线衍射、红外光谱和拉曼光谱进行里特维尔德细化得出的结果表明,所有样品均为四方晶相。介电测量结果表明,增加锂掺杂率可降低介电损耗(室温下,从 x = 0 时的 0.04 到 x = 0.09 时的 0.008),并降低 x ≤ 0.07 时的转变温度 Tm。相变扩散参数 γ 在 1 到 1.39 之间变化,表明我们的样品表现出扩散相变,但远非弛豫行为。复阻抗光谱表明,材料的晶界电阻在材料的电学行为中占主导地位。活化能 Ea 是在 10 kHz 频率下通过使用阿伦尼乌斯公式对导电率的温度依赖性进行线性拟合计算得出的。所得数值表明,在 0 ≤ x ≤ 0.05 的成分中,传导是通过氧空位电离产生的自由电子进行的,而在 x = 0.07 和 0.09 的成分中,主要的传导机制是离子传导。
{"title":"Structural and enhanced dielectric properties of Li-doped BT elaborated by the sol-gel method","authors":"Fouad El Aychaoui, Abdelhalim El Basset, Mohamed Naji, Mohammed Bouzid, Abdelilah Rjeb, Lahoucine Hajji, Yahya Ababou","doi":"10.1007/s10971-024-06525-3","DOIUrl":"10.1007/s10971-024-06525-3","url":null,"abstract":"<div><p>In this paper, we studied the effect of lithium doping on the structural, microstructural, dielectric, and electrical properties of Ba<sub>1-x</sub>Li<sub>x</sub>TiO<sub>3-δ</sub> (BTLx) ceramics prepared via the sol-gel method, with x = 0, 0.01, 0.03, 0.05, 0.07 and 0.09. The results obtained from Rietveld refinement of X-ray diffraction, infrared spectroscopy, and Raman spectroscopy show that all the samples crystallize in the tetragonal phase. Dielectric measurements show that increasing the lithium doping rate results in lower dielectric losses (from 0.04 for x = 0 to 0.008 for x = 0.09 at room temperature) and lower transition temperature Tm for compositions with x ≤ 0.07. The phase transition diffusivity parameter γ varies between 1 and 1.39, showing that our samples exhibit a diffuse phase transition but far from relaxor behavior. Complex impedance spectroscopy indicates that the grain boundary resistance of the materials is predominant in the electrical behavior of the materials. The activation energy Ea was calculated at 10 kHz by linear fitting of the temperature dependence of conductivity using the Arrhenius formula. The obtained values indicate that conduction for compositions with 0 ≤ x ≤ 0.05 occurs through free electrons originating from the ionization of oxygen vacancies, while for the compositions with x = 0.07 and 0.09, the predominant conduction mechanism is ionic conduction.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"182 - 201"},"PeriodicalIF":2.3,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195933","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}
Practical aspects of the successful preparation of monolithic poly(methylsilsesquioxane) (PMSQ) aerogels with glasslike transparency via ambient pressure drying (APD) are discussed in detail. Two-step acid-base process starting from methyltrimethoxysilane (MTMS) in the presence of nonionic poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) surfactant and the use of strong base as polycondensation catalyst resulted in fine mesoporous structure, showing low bulk density (0.148 g cm−3) and glasslike transparency (95% at 10 mm thickness). Cracking and irreversible shrinkage during APD have been prevented by optimized aging and drying processes. In particular, aging in an aqueous alcohol solution containing a low concentration of MTMS under controlled temperature has been found to be crucial in obtaining PMSQ aerogels with crack-free, low-density, glasslike transparency, and monolithic nature. A large-area APD aerogel in 93 × 93 × 6 mm3, with thermal conductivity of 15.6 mW m−1 K−1, has successfully been obtained due to optimizations of aging and drying conditions. Similar APD aerogels have also been obtained when alkali metal hydroxides, especially lithium hydroxide, are employed as base catalysts. These findings are expected to play important roles in designing industrial productions of monolithic aerogels for thermal superinsulation and other applications.
{"title":"Monolithic poly(methylsilsesquioxane) aerogels with glasslike transparency: from sol-gel synthesis to ambient pressure drying","authors":"Riichi Miyamoto, Ryota Ueoka, Koichiro Tachibana, Ayaka Maeno, Hironori Kaji, Kazuyoshi Kanamori","doi":"10.1007/s10971-024-06528-0","DOIUrl":"10.1007/s10971-024-06528-0","url":null,"abstract":"<div><p>Practical aspects of the successful preparation of monolithic poly(methylsilsesquioxane) (PMSQ) aerogels with glasslike transparency via ambient pressure drying (APD) are discussed in detail. Two-step acid-base process starting from methyltrimethoxysilane (MTMS) in the presence of nonionic poly(ethylene oxide)-<i>block</i>-poly(propylene oxide)-<i>block</i>-poly(ethylene oxide) surfactant and the use of strong base as polycondensation catalyst resulted in fine mesoporous structure, showing low bulk density (0.148 g cm<sup>−3</sup>) and glasslike transparency (95% at 10 mm thickness). Cracking and irreversible shrinkage during APD have been prevented by optimized aging and drying processes. In particular, aging in an aqueous alcohol solution containing a low concentration of MTMS under controlled temperature has been found to be crucial in obtaining PMSQ aerogels with crack-free, low-density, glasslike transparency, and monolithic nature. A large-area APD aerogel in 93 × 93 × 6 mm<sup>3</sup>, with thermal conductivity of 15.6 mW m<sup>−1</sup> K<sup>−1</sup>, has successfully been obtained due to optimizations of aging and drying conditions. Similar APD aerogels have also been obtained when alkali metal hydroxides, especially lithium hydroxide, are employed as base catalysts. These findings are expected to play important roles in designing industrial productions of monolithic aerogels for thermal superinsulation and other applications.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"202 - 215"},"PeriodicalIF":2.3,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142196037","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}
Smart devices, such as soft robots, artificial organs, and soft actuators, require materials that adapt their morphologies and properties in response to their environment. These materials can be obtained through the composition of different types of materials that exhibit different responses to environmental stimuli, arranged in a rational spatial configuration. We achieved unique responsive materials by forming interfaces and surfaces of appropriate materials using the sol–gel method. In recent decades, we have proposed the use of wrinkles and nano-brushes on sol–gel-derived materials for various sophisticated applications, such as micropattern fabrication, wettability control, and linear actuators for size-selective transportation. This account introduces environment-responsive materials with rational interfaces via the sol–gel method, particularly those characterized by surface morphology.
{"title":"Formation of interfaces responsive and adaptive to environment via the sol-gel method","authors":"Masahide Takahashi, Kenji Okada, Luca Malfatti, Plinio Innocenzi","doi":"10.1007/s10971-024-06522-6","DOIUrl":"10.1007/s10971-024-06522-6","url":null,"abstract":"<p>Smart devices, such as soft robots, artificial organs, and soft actuators, require materials that adapt their morphologies and properties in response to their environment. These materials can be obtained through the composition of different types of materials that exhibit different responses to environmental stimuli, arranged in a rational spatial configuration. We achieved unique responsive materials by forming interfaces and surfaces of appropriate materials using the sol–gel method. In recent decades, we have proposed the use of wrinkles and nano-brushes on sol–gel-derived materials for various sophisticated applications, such as micropattern fabrication, wettability control, and linear actuators for size-selective transportation. This account introduces environment-responsive materials with rational interfaces via the sol–gel method, particularly those characterized by surface morphology.</p>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"112 1","pages":"174 - 181"},"PeriodicalIF":2.3,"publicationDate":"2024-08-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10971-024-06522-6.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195972","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 : 2024-08-25DOI: 10.1007/s10971-024-06519-1
N. Khima, A. Chelouche, F. Challali, D. Djouadi, A. Djermoune, M. Luce, A. Cricenti, D. Becerril, S. Bellucci, T. Touam
The present study examines the impact of acidic and basic pH on the optical, morphological, and structural characteristics of TiO2 sol–gel thin films that are deposited using the dip-coating technique on glass substrates. All of the samples are polycrystalline and have anatase structures with preference orientation along the (101) direction, according to X-ray diffraction (XRD) and Raman spectroscopy (RS). It is observed that, for both basic and acidic pH values, crystallite size decreases as sol pH rises. All of the films’ surfaces were smooth and had a uniform grain distribution, according to atomic force microscopy (AFM). The pH of the sol has an impact on the surface roughness. All films had a higher degree of transparency, according to UV-visible spectroscopy. The refractive index and the direct and indirect band gaps are two essential optical properties of thin films that are significantly influenced by the pH of the deposition medium. Measurements of photoluminescence (PL) showed a strong violet-blue emission band, the intensity of which is highly dependent on the sol’s pH. In acidic media, PL decreases with increasing pH. However, in a basic environment, the PL rises sharply as the pH increases from 10 to 11 and then decreases for higher pH values. In particular, compared to the other samples, the emission intensity from the film deposited at a pH value of 10 is noticeably lower and displays unique spectral signatures.
{"title":"TiO2 sol–gel thin films: effect of acidic and basic pH on physical characteristics","authors":"N. Khima, A. Chelouche, F. Challali, D. Djouadi, A. Djermoune, M. Luce, A. Cricenti, D. Becerril, S. Bellucci, T. Touam","doi":"10.1007/s10971-024-06519-1","DOIUrl":"10.1007/s10971-024-06519-1","url":null,"abstract":"<div><p>The present study examines the impact of acidic and basic pH on the optical, morphological, and structural characteristics of TiO<sub>2</sub> sol–gel thin films that are deposited using the dip-coating technique on glass substrates. All of the samples are polycrystalline and have anatase structures with preference orientation along the (101) direction, according to X-ray diffraction (XRD) and Raman spectroscopy (RS). It is observed that, for both basic and acidic pH values, crystallite size decreases as sol pH rises. All of the films’ surfaces were smooth and had a uniform grain distribution, according to atomic force microscopy (AFM). The pH of the sol has an impact on the surface roughness. All films had a higher degree of transparency, according to UV-visible spectroscopy. The refractive index and the direct and indirect band gaps are two essential optical properties of thin films that are significantly influenced by the pH of the deposition medium. Measurements of photoluminescence (PL) showed a strong violet-blue emission band, the intensity of which is highly dependent on the sol’s pH. In acidic media, PL decreases with increasing pH. However, in a basic environment, the PL rises sharply as the pH increases from 10 to 11 and then decreases for higher pH values. In particular, compared to the other samples, the emission intensity from the film deposited at a pH value of 10 is noticeably lower and displays unique spectral signatures.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"277 - 288"},"PeriodicalIF":2.3,"publicationDate":"2024-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195973","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 : 2024-08-19DOI: 10.1007/s10971-024-06511-9
Mohamed Hsini, T. Raoufi, M. H. Ehsani, Manel Essid, Nuha Al-Harbi, B. M. Alotaibi, Hayfa A. Alyousef
This study investigates the critical behavior analysis and predicting magnetocaloric properties of La0.6-xGdxSr0.4MnO3 manganites, focusing on the impact of varying gadolinium (Gd) doping levels (x = 0, 0.0125, 0.05, and 0.10). Using modified Arrott plots (MAPs) and the Kouvel–Fisher method, the critical exponents γ and β were determined, yielding values that indicate how Gd content influences magnetic phase transitions. Additionally, the magnetocaloric effect (MCE) was analyzed to assess the magnetic entropy change (-Delta {{rm{S}}}_{{rm{M}}}({rm{T}})) and the Temperature-Averaged Entropy Change (({TEC})) across different magnetic field changes. The results show that increasing Gd doping enhances the magnetocaloric response, suggesting potential applications in magnetic refrigeration. Overall, the study provides insights into optimizing these manganites for applications in high-temperature sensors, spintronics, and magnetic cooling.
{"title":"Predicting the magnetocaloric properties in Gd ion substitution on La0.6-xGdxSr0.4MnO3 (x = 0, 0.0125, 0.05, and 0.10) manganites synthesized via the sol-gel method","authors":"Mohamed Hsini, T. Raoufi, M. H. Ehsani, Manel Essid, Nuha Al-Harbi, B. M. Alotaibi, Hayfa A. Alyousef","doi":"10.1007/s10971-024-06511-9","DOIUrl":"10.1007/s10971-024-06511-9","url":null,"abstract":"<div><p>This study investigates the critical behavior analysis and predicting magnetocaloric properties of La<sub>0.6-x</sub>Gd<sub>x</sub>Sr<sub>0.4</sub>MnO<sub>3</sub> manganites, focusing on the impact of varying gadolinium (Gd) doping levels (x = 0, 0.0125, 0.05, and 0.10). Using modified Arrott plots (MAPs) and the Kouvel–Fisher method, the critical exponents γ and β were determined, yielding values that indicate how Gd content influences magnetic phase transitions. Additionally, the magnetocaloric effect (MCE) was analyzed to assess the magnetic entropy change <span>(-Delta {{rm{S}}}_{{rm{M}}}({rm{T}}))</span> and the Temperature-Averaged Entropy Change <span>(({TEC}))</span> across different magnetic field changes. The results show that increasing Gd doping enhances the magnetocaloric response, suggesting potential applications in magnetic refrigeration. Overall, the study provides insights into optimizing these manganites for applications in high-temperature sensors, spintronics, and magnetic cooling.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Predicting of <span>(-Delta {{rm{S}}}_{{rm{M}}}({rm{T}}))</span> curves (solid lines) under various magnetic fields. The experimental results are presented with symbols for the La<sub>0.6-x</sub>Gd<sub>x</sub>Sr<sub>0.4</sub>MnO<sub>3</sub> manganites (x = 0, 0.0125, 0.05, 0.10) indicated by G0, G1, G2 and G3, respectively.</p></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"112 1","pages":"162 - 173"},"PeriodicalIF":2.3,"publicationDate":"2024-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195975","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}
Catalytic reduction of 4-nitrophenol (4-NP) into 4-aminophenol (4-AP) is an important method for treating toxic nitroaromatic pollutant. In this work, amorphous CoSn(OH)6 nanocubes were synthesized by coprecipitation and calcination methods for 4-NP photocatalytic reduction. The crystal structure, morphology and optical property of the samples were characterized by XRD, SEM, TEM, XPS, and UV–vis DRS. The amorphous CoSn(OH)6 nanocubes showed excellent photocatalytic performance in 4-NP reduction. The effects of catalyst dosage, 4-NP concentration, and sodium borohydride concentration on the conversion rate of 4-NP were investigated. The results showed that the conversion rate of 4-NP could reach 98.38% in 15 min at room temperature under visible light irradiation. After five cycles of experiments, the conversion rate of 4-NP remained above 90%, indicating the good catalytic stability of the amorphous CoSn(OH)6 nanocubes. Finally, the mechanisms of photocatalytic reduction on amorphous CoSn(OH)6 nanocubes are also discussed. The successful preparation of amorphous CoSn(OH)6 nanocubes may enable the widespread use of amorphous polymetallic oxides for the removal of nitrophenols from wastewater in the future.
{"title":"Synthesis of amorphous CoSn(OH)6 nanocubes for photocatalytic reduction of 4-nitrophenol","authors":"Enlei Zhang, Jiaojiao Chen, Rui Xu, Xiaowen Song, Bengui Zhang, Guosheng Wang","doi":"10.1007/s10971-024-06508-4","DOIUrl":"10.1007/s10971-024-06508-4","url":null,"abstract":"<div><p>Catalytic reduction of 4-nitrophenol (4-NP) into 4-aminophenol (4-AP) is an important method for treating toxic nitroaromatic pollutant. In this work, amorphous CoSn(OH)<sub>6</sub> nanocubes were synthesized by coprecipitation and calcination methods for 4-NP photocatalytic reduction. The crystal structure, morphology and optical property of the samples were characterized by XRD, SEM, TEM, XPS, and UV–vis DRS. The amorphous CoSn(OH)<sub>6</sub> nanocubes showed excellent photocatalytic performance in 4-NP reduction. The effects of catalyst dosage, 4-NP concentration, and sodium borohydride concentration on the conversion rate of 4-NP were investigated. The results showed that the conversion rate of 4-NP could reach 98.38% in 15 min at room temperature under visible light irradiation. After five cycles of experiments, the conversion rate of 4-NP remained above 90%, indicating the good catalytic stability of the amorphous CoSn(OH)<sub>6</sub> nanocubes. Finally, the mechanisms of photocatalytic reduction on amorphous CoSn(OH)<sub>6</sub> nanocubes are also discussed. The successful preparation of amorphous CoSn(OH)<sub>6</sub> nanocubes may enable the widespread use of amorphous polymetallic oxides for the removal of nitrophenols from wastewater in the future.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Amorphous CoSn(OH)<sub>6</sub> nanocubes exhibit superior photocatalytic reduction 4-NP to 4-AP performance.</p></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"112 1","pages":"152 - 161"},"PeriodicalIF":2.3,"publicationDate":"2024-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195979","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 : 2024-08-18DOI: 10.1007/s10971-024-06515-5
C. Jayakrishnan, S. R. Sheeja, G. Suresh Kumar, K. Lalithambigai, J. Duraimurugan, Mohammed Mujahid Alam
In this study, we have investigated the effects of EDTA, citric acid, and urea on the morphology-controlled synthesis of ZnO nanostructures by a hydrothermal method. XRD, FTIR, FESEM, TEM, BET, and UV-DRS studies revealed that the addition of different complexing agents not only controls the size and morphology but also alters the crystallinity, particle size, energy bandgap, specific surface area, and pore characteristics of ZnO. We achieved diverse morphologies, including spherical nanoparticles (80–100 nm), nanorods (1 µm length, 100 nm diameter), and nanoflakes (100–200 nm lateral dimension with 10–20 nm thickness) utilizing citric acid, urea, and EDTA as morphology controllers. The resulting nanoparticles had surface areas of 11.8 m2/g, 29.6 m2/g, and 4.6 m2/g, respectively. ZnO nanostructures developed with citric acid, urea, and EDTA were found to have a band gap of 3.273 eV, 3.209 eV, and 3.380 eV, respectively. The photodegradation efficiency of ZnO spherical nanoparticles, nanorods, and nanoflakes was found to be 90%, 97%, and 81%, respectively, demonstrating the shape-dependent photodegradation of MB dye. The prepared ZnO photocatalyst exhibits pseudo-first-order kinetics with good recyclability (five cycles) and stability. The enhanced photocatalytic performance of ZnO nanorods was attributed to their morphology, which facilitates efficient charge separation and increased surface area, leading to more active sites for pollutant degradation. This study offers a potential approach for developing morphology-driven photocatalysts for environmental remediation and water purification.
{"title":"Hydrothermal assisted synthesis of shape-controlled zinc oxide nanostructures for tuneable photodegradation of methylene blue pollutant","authors":"C. Jayakrishnan, S. R. Sheeja, G. Suresh Kumar, K. Lalithambigai, J. Duraimurugan, Mohammed Mujahid Alam","doi":"10.1007/s10971-024-06515-5","DOIUrl":"10.1007/s10971-024-06515-5","url":null,"abstract":"<div><p>In this study, we have investigated the effects of EDTA, citric acid, and urea on the morphology-controlled synthesis of ZnO nanostructures by a hydrothermal method. XRD, FTIR, FESEM, TEM, BET, and UV-DRS studies revealed that the addition of different complexing agents not only controls the size and morphology but also alters the crystallinity, particle size, energy bandgap, specific surface area, and pore characteristics of ZnO. We achieved diverse morphologies, including spherical nanoparticles (80–100 nm), nanorods (1 µm length, 100 nm diameter), and nanoflakes (100–200 nm lateral dimension with 10–20 nm thickness) utilizing citric acid, urea, and EDTA as morphology controllers. The resulting nanoparticles had surface areas of 11.8 m<sup>2</sup>/g, 29.6 m<sup>2</sup>/g, and 4.6 m<sup>2</sup>/g, respectively. ZnO nanostructures developed with citric acid, urea, and EDTA were found to have a band gap of 3.273 eV, 3.209 eV, and 3.380 eV, respectively. The photodegradation efficiency of ZnO spherical nanoparticles, nanorods, and nanoflakes was found to be 90%, 97%, and 81%, respectively, demonstrating the shape-dependent photodegradation of MB dye. The prepared ZnO photocatalyst exhibits pseudo-first-order kinetics with good recyclability (five cycles) and stability. The enhanced photocatalytic performance of ZnO nanorods was attributed to their morphology, which facilitates efficient charge separation and increased surface area, leading to more active sites for pollutant degradation. This study offers a potential approach for developing morphology-driven photocatalysts for environmental remediation and water purification.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"262 - 276"},"PeriodicalIF":2.3,"publicationDate":"2024-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195977","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 : 2024-08-17DOI: 10.1007/s10971-024-06473-y
Udhaya Kumar Aruchamy, Emilia Merino, Alicia Durán, Helena Pálková, Dušan Galusek, Yolanda Castro
Relative humidity (RH) is one of the key parameters that significantly affect the curing kinetics and final properties of polysilazane-based coatings. Thus, the paper discusses the effect of relative humidity during the curing process and the anti-corrosion properties of (3-glycidyloxypropyl) trimethoxysilane (GPTMS)-modified polyorganosilazane (OPSZ) functionalized silica coatings on AA2024-T3. Modified polyorganosilazane sol was prepared and then deposited on AA2024-T3 substrates varying the curing conditions. After the deposition, the coated aluminum substrates were exposed to different RH levels; 15%, 40% and 80%, and then cured at 120 °C for 2 h. Transparent and crack-free GPTMS-modified polyorganosilazane coatings with a thickness of around 15–17 μm were obtained. The exposure to the relative humidity increased the crosslinking and hydrolysis-condensation reactions of the OPSZ and GPTMS molecules, showing more Si-O-Si bonds. The incorporation of GPTMS affected the crosslinking structure, enhancing the corrosion protection properties of the coating. GPTMS-modified polyorganosilazane coatings cured at 40%RH had the best anti-corrosive properties after immersion in 3.5 wt% NaCl solution. The impedance modulus of ∼109 Ω.cm2 at a low frequency was obtained, which was five orders of magnitude higher than that for the AA2024-T3 alloy.
{"title":"Humidity-induced curing and anti-corrosion properties of GPTMS-modified polyorganosilazane functionalized silica coating on AA2024-T3 aluminum alloy","authors":"Udhaya Kumar Aruchamy, Emilia Merino, Alicia Durán, Helena Pálková, Dušan Galusek, Yolanda Castro","doi":"10.1007/s10971-024-06473-y","DOIUrl":"10.1007/s10971-024-06473-y","url":null,"abstract":"<div><p>Relative humidity (RH) is one of the key parameters that significantly affect the curing kinetics and final properties of polysilazane-based coatings. Thus, the paper discusses the effect of relative humidity during the curing process and the anti-corrosion properties of (3-glycidyloxypropyl) trimethoxysilane (GPTMS)-modified polyorganosilazane (OPSZ) functionalized silica coatings on AA2024-T3. Modified polyorganosilazane sol was prepared and then deposited on AA2024-T3 substrates varying the curing conditions. After the deposition, the coated aluminum substrates were exposed to different RH levels; 15%, 40% and 80%, and then cured at 120 °C for 2 h. Transparent and crack-free GPTMS-modified polyorganosilazane coatings with a thickness of around 15–17 μm were obtained. The exposure to the relative humidity increased the crosslinking and hydrolysis-condensation reactions of the OPSZ and GPTMS molecules, showing more Si-O-Si bonds. The incorporation of GPTMS affected the crosslinking structure, enhancing the corrosion protection properties of the coating. GPTMS-modified polyorganosilazane coatings cured at 40%RH had the best anti-corrosive properties after immersion in 3.5 wt% NaCl solution. The impedance modulus of ∼10<sup>9</sup> Ω.cm<sup>2</sup> at a low frequency was obtained, which was five orders of magnitude higher than that for the AA2024-T3 alloy.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"140 - 151"},"PeriodicalIF":2.3,"publicationDate":"2024-08-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10971-024-06473-y.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142196016","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}
Aerogel possesses distinctive features rendering it widely applicable in thermal insulation. Nevertheless, supercritical fluid drying (SCFD) method and freeze-drying employed for aerogels necessitates the complex process, resulting in heightened energy consumption and more risk. To achieve the cost-effective preparation of silica aerogel, we introduce an in-situ acid catalysis strategy for rapidly crafting high-performance SiO2 aerogel materials under ambient conditions. The resultant SiO2 aerogels exhibit remarkable porosity (95%) and a substantial specific surface area (759 m²/g). Furthermore, SiO2 aerogel composites display low thermal conductivity (0.015 W·m−1 K−1), coupled with commendable mechanical property. More importantly, we reveal the mechanism of the in-situ acid catalysis (ISAC) strategy. The entire production cycle of SiO2 aerogel composites and powder is only 6 and 4 h respectively, which greatly reduces the preparation time while ensuring excellent performances. This study introduces a novel approach for the industrial, low-cost, and rapid preparation of SiO2 aerogel materials through ambient pressure drying.
{"title":"In-situ acid catalysis strategy to achieve rapid ambient pressure drying preparation of aerogels","authors":"Zun Zhao, Yuelei Pan, Mingyuan Yan, Yueyue Xiao, Hui Yang, Xudong Cheng","doi":"10.1007/s10971-024-06518-2","DOIUrl":"10.1007/s10971-024-06518-2","url":null,"abstract":"<div><p>Aerogel possesses distinctive features rendering it widely applicable in thermal insulation. Nevertheless, supercritical fluid drying (SCFD) method and freeze-drying employed for aerogels necessitates the complex process, resulting in heightened energy consumption and more risk. To achieve the cost-effective preparation of silica aerogel, we introduce an in-situ acid catalysis strategy for rapidly crafting high-performance SiO<sub>2</sub> aerogel materials under ambient conditions. The resultant SiO<sub>2</sub> aerogels exhibit remarkable porosity (95%) and a substantial specific surface area (759 m²/g). Furthermore, SiO<sub>2</sub> aerogel composites display low thermal conductivity (0.015 W·m<sup>−1</sup> K<sup>−1</sup>), coupled with commendable mechanical property. More importantly, we reveal the mechanism of the in-situ acid catalysis (ISAC) strategy. The entire production cycle of SiO<sub>2</sub> aerogel composites and powder is only 6 and 4 h respectively, which greatly reduces the preparation time while ensuring excellent performances. This study introduces a novel approach for the industrial, low-cost, and rapid preparation of SiO<sub>2</sub> aerogel materials through ambient pressure drying.</p><h3>Graphical Abstract</h3><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":"112 1","pages":"127 - 139"},"PeriodicalIF":2.3,"publicationDate":"2024-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142195978","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 : 2024-08-16DOI: 10.1007/s10971-024-06476-9
Eneyew Tilahun Bekele, Fasika Dereje Ambecha, C. R. Ravikumar, Taymour A. Hamdalla, H. C. Ananda Murthy, Defaru Negera Duke
The current world is exposed to immense classes of challenges, of which antimicrobial-caused infectious diseases have been ranked the third killer disease due to their high resistance capability. Oxidative stress is also the other problem faced by the current world. In the current study, a leaf of Foeniculum Vulgare was employed for the synthesis of silver nanoparticles (Ag NPs) within the 1:3, 1:1, and 3:1 compositions using 0.1 M of AgNO3. The calculated average crystalline size from X-ray diffraction (XRD) was found to be 12.6, 13.7, and 21.6 nm for the 1:3, 1:1, and 3:1 volume ratios, respectively. Scanning electron microscope coupled with energy dispersive spectroscopy (SEM-EDS) analysis depicts the quasi-spherical shape with an intense Ag peak at around 3.00 eV. Transmission electron microscope coupled with high-resolution transmission microscope with surface area electron diffraction pattern (TEM-HRTEM with SAED) showed spherical shaped Ag NPs. The electronic bandgap energy was calculated as 3.1, 3.2, and 3.3 eV for the 1:1, 3:1, and 1:3 volume compositions, respectively. Ag NPs show 13.5, 12.5, and 11.0 mm zones of inhibition for the 1:3, 1:1, and 3:1 ratios, respectively. The antifungal activity was found to be 16.9, 11.2, and 10.5 mm for the 3:1, 1:3 and 1:1 ratios, respectively. Lastly, the antioxidant activity was estimated to be 42.4, 28.94, and 27.39% RSA for the 1:1, 3:1, and 1:3 volume ratios respectively. All the ratios of Ag NPs showed promised antimicrobial and antioxidant activity in the presence of 2, 2-Diphenyl-1-picrylhydrazyl (DPPH) due to the enhanced generation of reactive oxygen species (ROS).
{"title":"Foeniculum Vulgare leaf extract loaded synthesis of silver nanoparticles in different volume ratios for antimicrobial and antioxidant activities: Comparative study of composition","authors":"Eneyew Tilahun Bekele, Fasika Dereje Ambecha, C. R. Ravikumar, Taymour A. Hamdalla, H. C. Ananda Murthy, Defaru Negera Duke","doi":"10.1007/s10971-024-06476-9","DOIUrl":"10.1007/s10971-024-06476-9","url":null,"abstract":"<div><p>The current world is exposed to immense classes of challenges, of which antimicrobial-caused infectious diseases have been ranked the third killer disease due to their high resistance capability. Oxidative stress is also the other problem faced by the current world. In the current study, a leaf of <i>Foeniculum Vulgare</i> was employed for the synthesis of silver nanoparticles (Ag NPs) within the 1:3, 1:1, and 3:1 compositions using 0.1 M of AgNO<sub>3</sub>. The calculated average crystalline size from X-ray diffraction (XRD) was found to be 12.6, 13.7, and 21.6 nm for the 1:3, 1:1, and 3:1 volume ratios, respectively. Scanning electron microscope coupled with energy dispersive spectroscopy (SEM-EDS) analysis depicts the quasi-spherical shape with an intense Ag peak at around 3.00 eV. Transmission electron microscope coupled with high-resolution transmission microscope with surface area electron diffraction pattern (TEM-HRTEM with SAED) showed spherical shaped Ag NPs. The electronic bandgap energy was calculated as 3.1, 3.2, and 3.3 eV for the 1:1, 3:1, and 1:3 volume compositions, respectively. Ag NPs show 13.5, 12.5, and 11.0 mm zones of inhibition for the 1:3, 1:1, and 3:1 ratios, respectively. The antifungal activity was found to be 16.9, 11.2, and 10.5 mm for the 3:1, 1:3 and 1:1 ratios, respectively. Lastly, the antioxidant activity was estimated to be 42.4, 28.94, and 27.39% RSA for the 1:1, 3:1, and 1:3 volume ratios respectively. All the ratios of Ag NPs showed promised antimicrobial and antioxidant activity in the presence of 2, 2-Diphenyl-1-picrylhydrazyl (DPPH) due to the enhanced generation of reactive oxygen species (ROS).</p><h3>Graphical Abstract</h3><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":"112 1","pages":"112 - 126"},"PeriodicalIF":2.3,"publicationDate":"2024-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142225056","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}