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Fabrication of starch/PVA/CuO electrospun nanoscaffolds for enhanced antimicrobial activity 淀粉/PVA/CuO静电纺丝纳米支架的制备及其抗菌性能
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-16 DOI: 10.1007/s10971-026-07241-w
Gopika Mohanakumar, Suresh Subramaniyam, Sivaramakrishnan R, Gopalakrishnan Velliyur Kanniappan, Selvaraj Jayaraman, Chella Perumal Palanisamy

The increasing prevalence of antimicrobial resistance and the limitations of conventional wound dressings necessitate the development of sustainable and effective antimicrobial biomaterials. In this study, copper oxide nanoparticles (CuO NPs) were green synthesized using Turbinaria conoides extract and subsequently incorporated into starch/polyvinyl alcohol (PVA) electrospun nanofibrous scaffolds to enhance antimicrobial performance. The biosynthesized CuO NPs exhibited a characteristic surface plasmon resonance peak at 270–300 nm and a mean particle size of 68 nm with a zeta potential of −11.4 mV, indicating moderate colloidal stability. Structural and chemical analyses (FTIR and XRD) confirmed the formation of monoclinic CuO and phytochemical-mediated stabilization, while SEM revealed uniform nanoparticle distribution within nanofibers of 90–110 nm diameter. The CuO-loaded nanoscaffolds demonstrated significantly enhanced antimicrobial activity, with inhibition zones of 30 ± 0.2 mm (Escherichia coli), 27 ± 0.2 mm (Klebsiella pneumoniae), and 25 ± 0.3 mm (Staphylococcus aureus), outperforming both algal extract and CuO NPs alone. The improved efficacy is attributed to synergistic effects of nanoparticle incorporation and sustained release from the nanofibrous matrix. This study presents a novel integration of T. conoides-mediated CuO nanoparticles into biodegradable starch/PVA electrospun scaffolds, offering a sustainable and effective platform for antimicrobial wound dressing applications.

抗菌药物耐药性的日益普遍和传统伤口敷料的局限性要求开发可持续和有效的抗菌生物材料。在本研究中,我们利用鸢尾提取物合成了氧化铜纳米颗粒(CuO NPs),并将其加入淀粉/聚乙烯醇(PVA)静电纺丝纳米纤维支架中以提高其抗菌性能。生物合成的CuO纳米粒子在270 ~ 300 nm处有一个特征性的表面等离子体共振峰,平均粒径为68 nm, zeta电位为- 11.4 mV,具有中等的胶体稳定性。结构和化学分析(FTIR和XRD)证实了单斜CuO的形成和植物化学介导的稳定性,而扫描电镜显示纳米纤维在90-110 nm直径内均匀分布。负载CuO的纳米支架显示出显著增强的抗菌活性,其抑制区为30±0.2 mm(大肠杆菌),27±0.2 mm(肺炎克雷伯菌)和25±0.3 mm(金黄色葡萄球菌),优于藻类提取物和CuO NPs。这种改善的功效归因于纳米颗粒掺入和纳米纤维基质的持续释放的协同作用。本研究提出了一种新型的将T. conoides介导的CuO纳米颗粒整合到可生物降解的淀粉/PVA静电纺丝支架中,为抗菌伤口敷料的应用提供了一个可持续和有效的平台。
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引用次数: 0
Green synthesis of MgO nanoparticles using Mangifera indica extract and their electrophoretic deposition on Ti6Al4V for antibacterial application 芒果提取物绿色合成氧化镁纳米颗粒及其在Ti6Al4V表面的电泳沉积及其抗菌应用
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-14 DOI: 10.1007/s10971-026-07223-y
Ana Marques, Daniela Santo, Sandra Carvalho, Susana Devesa

Titanium alloys such as Ti6Al4V are widely used in biomedical implants; however, their susceptibility to bacterial colonization remains a major challenge. In this work, magnesium oxide (MgO) nanoparticles were synthesized via a green route using Mangifera indica peel extract and subsequently deposited onto Ti6Al4V substrates by electrophoretic deposition (EPD) to explore their potential as antibacterial coatings. Following thermal analysis, the synthesized powders were calcined at 500 °C (HT500) and 700 °C (HT700). XRD and Rietveld refinement confirmed the formation of crystalline cubic MgO, with phase purities of 82.01 wt.% and 98.72 wt.% for HT500 and HT700, respectively. Crystallite size increased with calcination temperature, reaching approximately 62 nm for HT700 according to Rietveld refinement. SEM analysis revealed a transition from highly agglomerated particles to more defined polyhedral morphologies at higher calcination temperatures. The antibacterial activity of HT700 nanoparticles was evaluated against Escherichia coli and Staphylococcus aureus. A concentration-dependent reduction in bacterial viability was observed, with significant inhibition of E. coli from 3 mg/mL and S. aureus from 6 mg/mL onwards. The antibacterial effect was accompanied by an increase in culture medium pH, reaching values close to 10 at the highest nanoparticle concentrations. EPD successfully produced homogeneous MgO coatings on Ti6Al4V substrates, which showed a reduction in bacterial viability, particularly against S. aureus. Overall, these results demonstrate the feasibility of combining green-synthesized MgO nanoparticles with electrophoretic deposition to produce antibacterial Ti-based surface coatings, providing a proof-of-concept for the development of sustainable surface modifications for future biomedical applications.

Ti6Al4V等钛合金广泛应用于生物医学植入物;然而,它们对细菌定植的易感性仍然是一个主要挑战。本研究以芒果皮提取物为原料,通过绿色途径合成氧化镁纳米颗粒,并通过电泳沉积(EPD)将其沉积在Ti6Al4V衬底上,探索其作为抗菌涂层的潜力。热分析后,将合成的粉末分别在500℃(HT500)和700℃(HT700)下煅烧。XRD和Rietveld细化证实形成了立方MgO晶体,相纯度为82.01 wt。%和98.72 wt。HT500和HT700分别为%。晶粒尺寸随着煅烧温度的升高而增大,根据Rietveld细化,HT700的晶粒尺寸达到约62 nm。扫描电镜分析显示,在较高的煅烧温度下,从高度凝聚的颗粒转变为更明确的多面体形态。研究了HT700纳米颗粒对大肠杆菌和金黄色葡萄球菌的抑菌活性。观察到细菌活力的浓度依赖性降低,大肠杆菌从3mg /mL开始显著抑制,金黄色葡萄球菌从6mg /mL开始显著抑制。抗菌效果伴随着培养基pH值的增加,在最高纳米颗粒浓度时达到接近10的值。EPD成功地在Ti6Al4V基质上制备了均匀的MgO涂层,这表明细菌活力降低,特别是对金黄色葡萄球菌。总的来说,这些结果证明了将绿色合成的MgO纳米颗粒与电泳沉积相结合以生产抗菌ti基表面涂层的可行性,为未来生物医学应用中可持续表面修饰的发展提供了概念验证。
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引用次数: 0
Synergistic effect of 3-mercaptopropionic acid and MOE: DMF solvent engineering on crystallization and charge transport in sol-gel derived CZTSSe thin films 3-巯基丙酸和MOE: DMF溶剂工程对溶胶-凝胶衍生CZTSSe薄膜结晶和电荷输运的协同效应
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-13 DOI: 10.1007/s10971-026-07247-4
Puteri Noor Safura Megat Mahmud, Yoganash Putthisigamany, Megat Mohd Izhar Sapeli, Vidhya Selvanathan, Kazi Sajedur Rahman, Ubaidah Syafiq, Kuhan Chandru, Brahim Aissa, Mohammad Istiaque Hossain, Norasikin Ahmad Ludin, Puvaneswaran Chelvanathan

This work systematically investigates the synergistic effect of 3-mercaptopropionic acid (MPA) coordination and solvent engineering on the structural, morphological, vibrational, and electrical properties of sol-gel-derived Cu2ZnSn(S,Se)4 (CZTSSe) thin films. CZTSSe absorbers were fabricated using precursor solutions with and without MPA under different solvent environments (MOE: DMF solvent ratios of 50:50 and 25:75), followed by selenization. GIXRD and Raman analyses confirmed the dominant formation of kesterite CZTSSe absorbers, while the MPA-treated samples exhibited larger crystallite sizes, reduced microstrain, and improved local structural ordering. FESEM and AFM observations revealed that MPA incorporation promoted grain coalescence, reduced surface roughness, and produced more compact absorber layers. Conductive AFM further revealed that the MPA-treated films exhibited a more spatially connected current distribution, indicating improved local electrical connectivity and reduced defect-assisted charge transport. Hall effect measurements further showed an increase in carrier concentration from ~1014 to ~1019 cm⁻³ and a corresponding reduction in resistivity, confirming improved charge transport after MPA incorporation. However, DMF-rich systems exhibited smaller crystallite sizes and greater electrical inhomogeneity than films prepared using balanced solvent compositions, suggesting that an excessive DMF fraction limits long-range crystallite development through changes in precursor coordination and film formation. Among all the samples, M5, prepared with MPA under balanced solvent conditions (MOE: DMF = 50:50), exhibited the most favorable combination of crystallinity, compact morphology, and electrical performance. This study highlights the importance of balancing ligand coordination and solvent chemistry to optimize solution-processed CZTSSe absorbers.

本文系统地研究了3-巯基丙酸(MPA)配位和溶剂工程对溶胶-凝胶衍生Cu2ZnSn(S,Se)4 (CZTSSe)薄膜结构、形态、振动和电学性能的协同效应。在不同的溶剂环境下(MOE: DMF溶剂比分别为50:50和25:75),用含和不含MPA的前驱体溶液制备CZTSSe吸光剂,并进行硒化处理。GIXRD和Raman分析证实了kesterite CZTSSe吸收剂的主要形成,而mpa处理的样品显示出更大的晶体尺寸,减少了微应变,改善了局部结构有序。FESEM和AFM观察表明,MPA的加入促进了晶粒聚结,降低了表面粗糙度,并产生了更致密的吸收层。导电AFM进一步显示,mpa处理后的薄膜呈现出更多空间连接的电流分布,表明改善了局部电连通性,减少了缺陷辅助的电荷传输。霍尔效应测量进一步显示载流子浓度从~1014增加到~1019 cm(⁻³),电阻率也相应降低,证实了加入MPA后电荷输运的改善。然而,与使用平衡溶剂组成制备的薄膜相比,富含DMF的体系表现出更小的晶体尺寸和更大的电不均匀性,这表明过量的DMF分数通过改变前驱体配位和薄膜形成限制了长期的晶体发育。在所有样品中,在平衡溶剂条件下(MOE: DMF = 50:50)用MPA制备的M5在结晶度、致密形貌和电性能方面表现出最有利的组合。本研究强调了平衡配体配位和溶剂化学对优化溶液处理CZTSSe吸收剂的重要性。
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引用次数: 0
MOF-derived hierarchical FeCo3S4@graphitic carbon/rGO nanoarchitectures for high-energy and high-power supercapacitors mof衍生的分层FeCo3S4@graphitic碳/氧化石墨烯纳米结构用于高能和高功率超级电容器
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-13 DOI: 10.1007/s10971-026-07246-5
Ahmad Gholizadeh, Elham Mazaheri

A hierarchical FeCo₃S₄@gC/rGO (Fe-Co-S@gC/rGO) hybrid nanocomposite was synthesized through a MOF-assisted solution-mediated assembly and two-step thermal treatment strategy for supercapacitor applications. The resulting architecture integrates reduced graphene oxide (rGO), graphitic carbon (gC), and cobalt sulfide-based nanostructures to improve electrical conductivity, electrolyte accessibility, and structural stability. Structural characterization confirmed the formation of a porous Fe-Co-S@gC/rGO framework with uniformly distributed Fe, Co, S, C, N, and O species. Electrochemical measurements showed that the optimized Fe-Co-S@gC/rGO electrode delivered a high specific capacitance of 1827 F g−1 at 0.5 A g−1 and retained strong cycling durability. An asymmetric supercapacitor assembled using Fe-Co-S@gC/rGO as the positive electrode and rGO as the negative electrode exhibited favorable energy-storage performance and long-term stability. The device delivered 974.1 F g⁻¹ at 0.5 A g⁻¹ and achieved a high energy density of 541.2 Wh kg⁻¹ at a power density of 8213.4 W kg⁻¹. Additionally, long-term durability was confirmed over 12,000 charge–discharge cycles and 10,000 voltammetry cycles. The enhanced electrochemical behavior is attributed to the combined effects of hierarchical porosity, conductive graphitic carbon/rGO networks, and abundant redox-active sites. These results suggest that Fe-Co-S@gC/rGO is a promising electrode material for advanced supercapacitor applications.

采用mof辅助溶液介导组装和两步热处理策略合成了一种用于超级电容器的FeCo₃S₄@gC/rGO (Fe-Co-S@gC/rGO)复合纳米材料。由此产生的结构集成了还原氧化石墨烯(rGO)、石墨碳(gC)和硫化钴基纳米结构,以提高导电性、电解质可及性和结构稳定性。结构表征证实形成了具有均匀分布的Fe、Co、S、C、N和O的多孔Fe-Co-S@gC/rGO框架。电化学测量表明,优化后的Fe-Co-S@gC/rGO电极在0.5 a g−1时具有1827 F g−1的高比电容,并保持了较强的循环耐久性。以Fe-Co-S@gC/rGO为正极,rGO为负极组装的非对称超级电容器具有良好的储能性能和长期稳定性。该装置以0.5 A g⁻¹的速度传递974.1 F g⁻¹,以8213.4 W kg⁻¹的功率密度达到541.2 Wh kg⁻¹的高能量密度。此外,经过12,000次充放电循环和10,000次伏安循环,其长期耐用性得到了证实。电化学性能的增强是由于分层孔隙度、导电石墨碳/还原氧化石墨烯网络和丰富的氧化还原活性位点的综合作用。这些结果表明Fe-Co-S@gC/rGO是一种很有前途的高级超级电容器电极材料。
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引用次数: 0
Spinel MnFe2O4 nanoparticles with improved surface area and charge transfer characteristics for next-generation supercapacitors 具有改进表面积和电荷转移特性的尖晶石MnFe2O4纳米颗粒用于下一代超级电容器
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-08 DOI: 10.1007/s10971-026-07250-9
Ali Mujtaba, A. F. A. Kadir, Aqsa Saeed, Mohamed Bouzidi, Ghada Ragheb Elnaggar, H. Khan, Faisal Alresheedi

The growing demand for sustainable and efficient energy storage devices has accelerated the development of advanced electrode materials for high-performance supercapacitors. In this work, MnFe₂O₄ nanoparticles were successfully synthesized through a novel green co-precipitation approach using Curcuma longa extract as a natural reducing and stabilizing agent. XRD analysis confirmed the formation of highly crystalline spinel MnFe₂O₄ with an average crystallite size of 19.9 nm and excellent phase purity. Raman spectroscopy further validated the characteristic vibrational modes of the spinel ferrite structure, while BET analysis revealed an enhanced surface area with mesoporous characteristics favorable for ion diffusion. SEM images demonstrated porous cauliflower-like interconnected morphology, and EDX confirmed the homogeneous distribution of Mn, Fe, and O elements without impurities. Electrochemical studies exhibited remarkable pseudocapacitive behavior with a high specific capacitance of 295 F g⁻¹ at 0.8 A g⁻¹ and 87.3% capacitance retention after 5000 charge–discharge cycles. Furthermore, EIS analysis revealed low charge transfer resistance and enhanced ion diffusion kinetics, confirming the strong potential of green-synthesized MnFe₂O₄ for sustainable next-generation supercapacitor applications.

对可持续和高效储能器件的需求不断增长,加速了高性能超级电容器的先进电极材料的发展。本研究以姜黄提取物为天然还原剂和稳定剂,采用绿色共沉淀法成功合成了MnFe₂O₄纳米颗粒。XRD分析证实形成了高结晶尖晶石MnFe₂O₄,平均晶粒尺寸为19.9 nm,相纯度优异。拉曼光谱进一步验证了尖晶石铁氧体结构的特征振动模式,而BET分析显示,尖晶石铁氧体的表面积增加,具有有利于离子扩散的介孔特征。SEM图像显示多孔的菜花状互连形态,EDX证实Mn, Fe和O元素分布均匀,没有杂质。电化学研究显示出显著的赝电容行为,在0.8 a g⁻¹时的高比电容为295 F g⁻¹,在5000次充放电循环后电容保持率为87.3%。此外,EIS分析显示低电荷转移电阻和增强的离子扩散动力学,证实了绿色合成的MnFe₂O₄在可持续的下一代超级电容器应用中的强大潜力。
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引用次数: 0
Heterogeneous photosensitizers based on iridium polypyridine complexes immobilized on periodic mesoporous organosilica for aza–Henry reaction and CO2 reduction 基于周期性介孔有机二氧化硅固定的铱多吡啶络合物的非均相光敏剂用于aza-Henry反应和CO2还原
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-05 DOI: 10.1007/s10971-026-07244-7
Minoru Waki, Masamichi Ikai, Yoshifumi Maegawa, Shinji Inagaki

Iridium bis(phenylpyridine)(bipyridine) complex, Ir(ppy)₂(bpy)⁺, which exhibits outstanding photophysical and photochemical properties as a photosensitizer, was immobilized on 2,2′-bipyridine-bridged mesoporous organosilica (BPyPMO) to afford Ir-BPyPMO. Successful immobilization of the iridium complex within the PMO framework was confirmed by X-ray absorption fine structure analysis. Ir-BPyPMO exhibited a characteristic UV–vis diffuse-reflectance spectrum with a metal-to-ligand charge-transfer (MLCT) band at a wavelength comparable to that of the corresponding MLCT band of the homogeneous Ir(ppy)₂(bpy)⁺ complex, indicating that the photophysical properties of the iridium complex were retained after immobilization. Under visible-light irradiation, Ir-BPyPMO functioned as an efficient heterogeneous photosensitizer for the aza–Henry reaction through C–H functionalization of 2-phenyl-1,2,3,4-tetrahydroisoquinoline. Furthermore, co-immobilization of a rhenium tricarbonyl complex on Ir-BPyPMO afforded Re-Ir-BPyPMO, which efficiently catalyzed CO₂ reduction in the presence of a sacrificial electron donor. These results demonstrate that the immobilized iridium complex functions effectively as a heterogeneous photosensitizer and highlight the potential of BPyPMO as a versatile platform for constructing photocatalytic systems.

铱双(苯基吡啶)(联吡啶)配合物Ir(ppy) 2 (bpy)⁺作为光敏剂具有优异的光物理和光化学性质,将其固定在2,2′-联吡啶桥接介孔有机硅(BPyPMO)上,得到Ir-BPyPMO。x射线吸收精细结构分析证实了铱配合物在PMO框架内的成功固定。Ir- bpypmo表现出特有的UV-vis漫反射光谱,其金属到配体电荷转移(MLCT)带的波长与Ir(ppy) 2 (bpy) +均相配合物相应的MLCT带相当,表明固定后铱配合物的光物理性质得以保留。在可见光照射下,Ir-BPyPMO通过2-苯基-1,2,3,4-四氢异喹啉的C-H官能化,作为一种高效的非均相光敏剂参与了氮杂-亨利反应。此外,三羰基铼配合物在Ir-BPyPMO上共固定得到Re-Ir-BPyPMO,在牺牲电子给体存在下有效催化CO₂还原。这些结果表明,固定化铱配合物作为一种多相光敏剂具有有效的功能,并突出了BPyPMO作为构建光催化体系的多功能平台的潜力。
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引用次数: 0
Author Correction: Comparison of sol–gel derived carbon xerogels synthesized from different phenolic precursors and solvents: electrical conductivity and dielectric relaxation 作者更正:由不同酚醛前体和溶剂合成的溶胶-凝胶衍生碳干凝胶的比较:电导率和介电弛豫
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-10-01 DOI: 10.1007/s10971-026-07252-7
Aymen Belguesmi, Amal Souilah, Aya Gharsallah, Abel García-Bernabé, Arbi Fattoum, Mourad Arous, Elimame Elaloui
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引用次数: 0
Ni-Doped ZnO nanoparticles prepared by sol–gel: enhanced electrical conductivity and transition from non-magnetic to magnetic behavior 溶胶-凝胶法制备ni掺杂ZnO纳米颗粒:增强电导率和从非磁性到磁性的转变
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-09-30 DOI: 10.1007/s10971-026-07243-8
Sharaa A. Alqarni, Ramzi Dhahri, Majdi Benamara, Imen Hammami, Hasan B. Albargi, Elkenany Brens Elkenany, Giovanni Neri, M.P.F. Graça

Zinc oxide (ZnO) is a widely investigated semiconductor owing to its versatility in electronic and optoelectronic applications. However, its intrinsic diamagnetism and relatively low electrical conductivity limit its performance in advanced electronic and spintronic systems. In this work, we investigate the effect of nickel-induced hybridization in ZnO nanoparticles with a nominal Ni concentration of 20%, focusing on the resulting structural, electrical, dielectric, and magnetic properties. The incorporation of Ni ions into the ZnO lattice promotes hybridization between Ni 3 d and O 2p orbitals, leading to modifications in the electronic structure and defect landscape. This effect results in a significant enhancement of electrical conductivity, with a thermally activated conduction mechanism characterized by a low activation energy of approximately 84 meV, indicating facilitated charge transport via defect-related states. Magnetic measurements reveal a transition from diamagnetic to superparamagnetic behavior, with a saturation magnetization of 6 emu/g at 5 K, decreasing to 1.5 emu/g at 300 K. Overall, the observed hybridization-driven tuning of electrical and magnetic properties highlights the potential of Ni-doped ZnO nanoparticles for applications in electronic devices, spintronics, gas sensing, photocatalysis, and magnetic hyperthermia.

氧化锌(ZnO)是一种广泛应用于电子和光电子领域的半导体材料。然而,其固有的抗磁性和相对较低的导电性限制了其在先进电子和自旋电子系统中的应用。在这项工作中,我们研究了镍诱导杂化对ZnO纳米粒子的影响,其标称镍浓度为20%,重点研究了由此产生的结构、电学、介电和磁性能。在ZnO晶格中加入Ni离子促进了Ni 3d和o2p轨道之间的杂化,导致了电子结构和缺陷景观的改变。这种效应导致电导率显著增强,具有热激活传导机制,其特征是活化能约为84 meV,表明通过缺陷相关状态促进电荷传输。磁性测量显示了从抗磁性到超顺磁性的转变,在5k时饱和磁化强度为6 emu/g,在300 K时下降到1.5 emu/g。总的来说,观察到的杂化驱动的电学和磁性调谐突出了ni掺杂ZnO纳米颗粒在电子器件、自旋电子学、气体传感、光催化和磁热疗方面的应用潜力。
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引用次数: 0
Preparation and properties of ZrO2/SiO2 composite films modified with PVA and silane coupling agents PVA和硅烷偶联剂改性ZrO2/SiO2复合膜的制备及性能
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-09-23 DOI: 10.1007/s10971-026-07226-9
Li-wei Chen, Shu-fang Yan, Zhan-lin Li, Wei-dong Chen

ZrO2/SiO2 composite film was prepared on the surface of zirconium hydride by anodic oxidation+sol-gel sealing composite process to solve the problem of insufficient hydrogen resistance caused by defects such as micropores and microcracks in the anodic oxidation film of zirconium hydride. Using tetraethoxysilane (TEOS) as precursor, polyvinyl alcohol (PVA), silane coupling agent KH570 and A171 were introduced to regulate the sol structure, and the film was densified and stabilized by stepwise heat treatment. The microstructure, composition, phase, thermal behavior and molecular structure of the composite film were systematically analyzed by means of SEM, EDS, XRD, TGDSC and FTIR. The thickness, adhesion, microhardness and hydrogen resistance of the film were tested to reveal the defect repair mechanism and hydrogen resistance mechanism. The results show that PVA and silane coupling agent can significantly refine the sol particle size, improve the film density and interfacial bonding strength. The optimized composite film has a thickness of 27.15μm, a binding force of 70.74 N, a microhardness of 457HV, and an initial dehydrogenation temperature of 710°C, showing excellent mechanical properties and high-temperature hydrogen resistance. The composite film forms a double-layer protective structure through anodic oxide layer support + sol-gel layer sealing, which blocks cracks and pores macroscopically. At the micro level, O-H and C-H chemical bonds are used to capture hydrogen atoms and inhibit diffusion, so as to achieve high-efficiency hydrogen resistance modification of zirconium hydride.Distinct from traditional single-layer hydrogen-resistant coatings, this work constructs a double-layer barrier via anodic oxidation and ternary PVA/KH570/A171 modified sol-gel, and reveals a dual-scale hydrogen resistance mechanism. This process can provide theoretical basis and technical reference for the surface strengthening of zirconium hydride based hydrogen barrier materials in nuclear industry and space energy field.

采用阳极氧化+溶胶-凝胶密封复合工艺在氢化锆表面制备了ZrO2/SiO2复合膜,解决了氢化锆阳极氧化膜存在微孔、微裂纹等缺陷导致的抗氢能力不足的问题。以四乙氧基硅烷(TEOS)为前驱体,加入聚乙烯醇(PVA)、硅烷偶联剂KH570和A171调节溶胶结构,通过分步热处理使膜致密稳定。采用SEM、EDS、XRD、TGDSC和FTIR等手段对复合膜的微观结构、成分、物相、热行为和分子结构进行了系统分析。对膜的厚度、附着力、显微硬度和抗氢性能进行了测试,揭示了膜的缺陷修复机理和抗氢机理。结果表明,PVA和硅烷偶联剂能显著细化溶胶粒径,提高膜密度和界面结合强度。优化后的复合膜厚度为27.15μm,结合力为70.74 N,显微硬度为457HV,初始脱氢温度为710℃,具有优异的力学性能和耐高温氢性能。复合膜通过阳极氧化层支撑+溶胶-凝胶层密封形成双层保护结构,宏观上阻断裂缝和孔隙。在微观层面,利用O-H和C-H化学键捕获氢原子并抑制扩散,从而实现氢化锆的高效抗氢改性。与传统的单层防氢涂层不同,本研究通过阳极氧化和三元PVA/KH570/A171改性溶胶-凝胶构建了双层防氢膜,揭示了双尺度的防氢机理。该工艺可为核工业和空间能源领域氢化锆基氢障材料的表面强化提供理论依据和技术参考。
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引用次数: 0
The key to carbon aerogel microbeads: xanthan gum-mediated shape retention during gelation of resorcinol formaldehyde droplets 碳气凝胶微珠的关键:间苯二酚甲醛滴凝胶过程中黄原胶介导的形状保持
IF 4.2 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-09-15 DOI: 10.1007/s10971-026-07224-x
Thomas Anklam, Seeni Meera Kamal Mohamed, Philip Niemeyer, Rebekka Probst, Beruktayet Fekadu, Frederic Kreps, Marina Schwan, René Tannert, Barbara Milow

Their high porosity, high surface area, and low density render resorcinol-formaldehyde (RF) aerogels attractive precursors to their carbon analogs which have interesting applications, for instance in adsorption, catalysis, or electrochemical energy storage. While they are conventionally produced by pyrolysis as monoliths in a laboratory scale, a large-scale production would be more facile if they were produced in the form of microbeads. The direct bead formation of RF solution by the dropping method is limited because of their inability to preserve the spherical shape until gelation due to the low viscosity of RF solution. Therefore, within this work, we aimed to improve the viscosity by adding the polysaccharide-based thickener xanthan gum (XG) to the RF solution and pre-gelling them, followed by dropping into an acid bath for rapid gelation. We were thus able to produce RF aerogel beads (RFB) and subsequently carbon aerogel beads (CB) with diameters ranging from 2.0–2.6 mm. Here, we investigated the physicochemical properties of the resulting RF and CB using various physicochemical techniques by varying the XG concentration and the type of acid gelation bath. N2 physisorption analysis showed that CBs developed with high surface areas up to 1205 m2/g, micropore volumes up to 0.43 cm3/g and, bulk (tap) density of 0.31 g/cm3. In order to evaluate the use of these CBs for applications such as carbon capture and electrode material, we furthermore investigated their CO2 sorption capacity, electrical conductivity, and mechanical properties. These findings presented in this work demonstrate the promising potential of the carbon aerogel microbeads for such applications.

它们的高孔隙率、高表面积和低密度使间苯二酚-甲醛(RF)气凝胶具有吸引碳类似物的前体,具有有趣的应用,例如吸附、催化或电化学储能。虽然它们通常是在实验室规模上通过热解作为整体生产的,但如果它们以微珠的形式生产,大规模生产将更加容易。由于RF溶液的低粘度,它们无法在凝胶形成之前保持球形,因此通过滴注方法直接形成RF溶液的头是有限的。因此,在这项工作中,我们的目标是通过将基于多糖的增稠剂黄原胶(XG)添加到RF溶液中并预凝胶化,然后滴入酸浴中进行快速凝胶化来提高粘度。因此,我们能够生产RF气凝胶珠(RFB)和随后的碳气凝胶珠(CB),直径范围为2.0-2.6 mm。在这里,我们通过不同的物理化学技术,通过改变XG浓度和酸凝胶浴的类型,研究了得到的RF和CB的物理化学性质。N2物理吸附分析表明,CBs发育的比表面积高达1205 m2/g,微孔体积高达0.43 cm3/g,体积(水龙头)密度为0.31 g/cm3。为了评估这些CBs在碳捕获和电极材料等方面的应用,我们进一步研究了它们的二氧化碳吸附能力、电导率和机械性能。这些发现表明了碳气凝胶微珠在此类应用中的巨大潜力。
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Journal of Sol-Gel Science and Technology
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