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Manipulation of Niobium Dopant concentrations on TiO2 nanotube arrays film via dual-steps electrochemical method for humidity sensor 双步电化学方法控制湿度传感器用TiO2纳米管阵列膜上铌掺杂物浓度
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-09-05 DOI: 10.1007/s10934-025-01853-3
N. E. A. Azhar, N. H. Sulimai, M. J. Salifairus, M. H. Mamat, S. S. Shariffudin, A. Shuhaimi, M. F. Malek, K. A. Eswar, M. Rusop

Titanium dioxide (TiO2) material is suitable for sensing applications due to higher electron mobility, stability, high sensitivity to water vapor and more easily desorb physisorbed water molecules. However, the non-homogeneous formation of TiO2 nanotube arrays due to cracking structure is a common issue. Cracking during the preparation of TiO2 nanotube arrays (TiO2 NTAs) films can lead to the deterioration and malfunction of the nanotubes. The work presented here describes the niobium-doped TiO2 NTAs (Nb-doped TiO2 NTAs) films prepared by the dual-step electrochemical methods at different doping concentrations (1 to 7 at%). It was found that the film doped at 3 at% and annealed at 500 °C showed excellent conductivity with a value of 0.52 S. cm−1. Results showed that the TiO2 NTAs exhibited a humidity sensitivity of 239.85. The humidity sensing performance of the fabricated TiO2 NTAs has been enhanced to 602.15 by doping with 3 at% of Nb. The enlargement of the area facilitated a slight increment of humidity sensitivity of Nb-doped TiO2 NTAs films. This phenomenon was induced by reducing the average diameter of NTAs in TiO2 film when the Nb dopant occupied the TiO2 structure (59 to 48 nm). Nb is commonly combined with TiO2 material as its regarded as a promising dopant for modifying crystalline structure. The Nb-doped TiO2 NTAs shows high sensor stability since the Nb ions widen the host TiO2 lattice thus improving the conductivity of TiO2. The optimized Nb-doped TiO2 NTAs films using the electrochemical cathodization method shows it is applicable for humidity sensor.

二氧化钛(TiO2)材料由于具有较高的电子迁移率、稳定性、对水蒸气的高灵敏度和更容易解吸物理吸附的水分子而适合于传感应用。然而,由于结构开裂导致的TiO2纳米管阵列的不均匀形成是一个普遍的问题。二氧化钛纳米管阵列(TiO2 NTAs)薄膜在制备过程中产生的裂纹会导致纳米管的劣化和失效。本文描述了在不同掺杂浓度(1 ~ 7% at%)下,采用双步电化学方法制备的铌掺杂TiO2 NTAs (nb掺杂TiO2 NTAs)薄膜。结果表明,掺杂率为3 at%, 500℃退火后的薄膜电导率为0.52 S. cm−1。结果表明,TiO2 nta的湿度敏感性为239.85。通过添加3 at%的Nb,制备的TiO2 nta的湿度传感性能达到602.15。面积的增大有利于nb掺杂TiO2 NTAs薄膜湿度敏感性的轻微提高。当Nb掺杂物占据TiO2结构(59 ~ 48 nm)时,TiO2薄膜中nta的平均直径减小。铌通常与TiO2材料结合,被认为是一种很有前途的修饰晶体结构的掺杂剂。Nb掺杂的TiO2 NTAs表现出较高的传感器稳定性,因为Nb离子扩大了主体TiO2晶格,从而提高了TiO2的导电性。采用电化学阴极化法制备的nb掺杂TiO2 NTAs薄膜可用于湿度传感器。
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引用次数: 0
Properties of CrOx(inc)/MCM-41 catalysts obtained by chromium incorporation and its catalytic activity in the reaction of propane dehydrogenation in the presence of CO2 研究了铬掺杂制备的CrOx(inc)/MCM-41催化剂的性能及其在CO2存在下丙烷脱氢反应中的催化活性
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-09-02 DOI: 10.1007/s10934-025-01850-6
Omvir Singh, Marina A. Tedeeva, Maria S. Igonina, Petr V. Pribytkov, Konstantin B. Kalmykov, Gennadiy I. Kapustin, Vera D. Nissenbaum, Igor V. Mishin, Sergey F. Dunaev, Leonid M. Kustov, Alexander L. Kustov

The oxidative dehydrogenation of propane (ODP) using CO2 offers a promising route to propylene production, as CO2 acts as a milder oxidant than O2. This study focuses on the synthesis and characterization of CrOx/MCM-41 catalysts prepared by co-precipitation of chromium nitrate and tetraethyl orthosilicate (TEOS) in the presence of the C16TMABr template. The resulting MCM-41-supported catalysts, along with the initial MCM-41 support, were characterized by N2 physisorption, TG-DTG-DTA, XRD, FT-IR spectroscopy, SEM-EDS, UV-Vis DRS, XPS, TPR-H2, and small-angle X-ray scattering. Analysis revealed that Cr in the 1-5Crinc/MCM-41 samples primarily exists as Cr6+, while in the 7-9Crinc/MCM-41 samples, both Cr3+ and Cr6+ are present, with Cr3+ being the dominant species. Catalytic testing conducted at an atmospheric pressure in the temperature range of 550–750 °C showed that the 5Crinc/MCM-41 and 3Crinc/MCM-41 catalysts achieved the highest propylene selectivity (68% at 575 °C with a 19% propane conversion and 69% at 600 °C with a 13% propane conversion, respectively). Notably, the incorporated Crinc/MCM-41 catalysts exhibited a 1.5–2.5 times higher productivity compared to supported Cr/MCM-41 catalysts.

利用二氧化碳氧化脱氢丙烷(ODP)为丙烯生产提供了一条很有前途的途径,因为二氧化碳是一种比O2更温和的氧化剂。研究了在C16TMABr模板存在下,硝酸铬与正硅酸四乙酯(TEOS)共沉淀法制备的CrOx/MCM-41催化剂的合成与表征。通过N2物理吸附、TG-DTG-DTA、XRD、FT-IR、SEM-EDS、UV-Vis DRS、XPS、TPR-H2和小角x射线散射对MCM-41载体和MCM-41载体进行了表征。分析表明,Cr在1-5Crinc/MCM-41样品中主要以Cr6+形式存在,而在7-9Crinc/MCM-41样品中,Cr3+和Cr6+同时存在,以Cr3+为主。在550-750℃的常压下进行的催化测试表明,5Crinc/MCM-41和3Crinc/MCM-41催化剂的丙烯选择性最高(在575℃,丙烷转化率为19%,丙烯选择性为68%;在600℃,丙烷转化率为13%,丙烯选择性为69%)。值得注意的是,加入的Crinc/MCM-41催化剂的产率比负载的Cr/MCM-41催化剂高1.5-2.5倍。
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引用次数: 0
Influencing factors and mechanisms in the magnetic silica molecular sieves Preparation process 磁性硅分子筛制备过程中的影响因素及机理
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-09-02 DOI: 10.1007/s10934-025-01838-2
Lei Zhang, Haocheng Zhao, Qi Wang, Lei Zhang, Ruikang Song

Magnetic silica molecular sieves have garnered significant attention for their combined molecular sieving properties and magnetic responsiveness, offering promising applications in catalysis and environmental remediation. This study systematically investigates the hydrothermal synthesis of silicalite-1 composites incorporating transition metal ferrites (Mg, Zn, Ni, Co) to develop magnetically separable molecular sieves. Through controlled variation of synthesis parameters including template concentration, water-to-silicon ratio, crystallization temperature and duration, we established optimal conditions yielding well-defined crystalline materials with preserved framework integrity. Comprehensive characterization through vibrating sample magnetometry, X-ray diffraction, and electron microscopy revealed that the incorporated magnetic nanoparticles (12–18 nm) maintain their spinel structure while causing only minimal distortion to the host molecular sieve matrix. The optimized composites demonstrated tunable soft magnetic properties with saturation magnetization values spanning 0.52–16.13 emu/g, dependent on ferrite composition and loading. Notably, the synthesis protocol achieved precise control over particle size (400–600 nm) and crystallinity while enabling efficient magnetic separation. This work provides fundamental insights into the structure-property relationships of magnetic zeolite composites, establishing a robust platform for their rational design in advanced separation and catalytic applications.

磁性二氧化硅分子筛因其综合分子筛性能和磁性响应性而受到广泛关注,在催化和环境修复方面具有广阔的应用前景。本研究系统地研究了水热合成含有过渡金属铁氧体(Mg, Zn, Ni, Co)的硅石-1复合材料,以制备磁性可分离分子筛。通过控制合成参数的变化,包括模板浓度、水硅比、结晶温度和持续时间,我们建立了最佳条件,得到了定义明确的晶体材料,并保持了框架的完整性。通过振动样品磁强计、x射线衍射和电子显微镜的综合表征表明,加入的磁性纳米颗粒(12-18 nm)保持了其尖晶石结构,同时对宿主分子筛基质只造成最小的畸变。优化后的复合材料具有可调的软磁性能,其饱和磁化强度值在0.52-16.13 emu/g之间,取决于铁氧体成分和负载。值得注意的是,合成方案实现了对粒度(400-600 nm)和结晶度的精确控制,同时实现了高效的磁分离。这项工作为磁性沸石复合材料的结构-性能关系提供了基本的见解,为其在高级分离和催化应用中的合理设计建立了一个强大的平台。
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引用次数: 0
Synthesis of modified hydrophobic hybrid biopolymer alginate/soy protein isolates aerogels via scCO2 drying for oil removal scCO2干燥脱油法制备海藻酸盐/大豆蛋白改性疏水杂化生物聚合物
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-26 DOI: 10.1007/s10934-025-01836-4
Hannah Sofiah Roslan, Ana Najwa Mustapa, Ahmad Naqiuddin Muhamad Tajuddin, Suhaiza Hanim Hanipah, Ángel Martín, María José Cocero

Oil pollution poses significant environmental challenges, necessitating the development of effective and sustainable solutions for oil absorbents. In this work, sodium alginate (ALG) and soy protein isolate (SPI) were combined via a sol–gel method, followed by surface functionalization using methyltrimethoxysilane (MTMS) and tetraethyl orthosilicate (TEOS) and dried by supercritical carbon dioxide (scCO2) to produce a hybrid aerogel oil absorbent. ALG concentration was varied from 1 to 3% w/w, while SPI concentrations were constant at 0.5 and 1.5% w/w. Results showed that the one-step surface modification successfully changed the ALG/SPI aerogel to hydrophobic. ALG/SPI aerogels are capable of absorbing model pollutants (i.e., waste engine oil, heavy-duty oil and chloroform) ranging from 1.34 to 10.3 g/g, with the highest absorption efficiency reaching 91%. Notably, ALG/SPI 1_1.5 appears as the most effective, absorbing waste oil at temperatures from 40 to 80 °C, has a high surface area (210 m2∙g−1), lightweight (0.107 g·cm−3), thermally stable over 196 °C, and is reusable up to four times. ALG/SPI aerogel remains afloat, retaining absorbed pollutants and is biodegradable, hence reducing post-use environmental impact. This study demonstrated that the hybrid ALG/SPI aerogels are promising materials as oil absorbents in the oil/water separation industry.

石油污染带来了重大的环境挑战,需要开发有效和可持续的吸油剂解决方案。本研究通过溶胶-凝胶法将海藻酸钠(ALG)和大豆分离蛋白(SPI)结合,然后用甲基三甲氧基硅烷(MTMS)和正硅酸四乙酯(TEOS)进行表面功能化,再用超临界二氧化碳(scCO2)干燥制得混合气凝胶吸油剂。ALG浓度为1 ~ 3% w/w, SPI浓度为0.5和1.5% w/w。结果表明,一步表面改性成功地改变了ALG/SPI气凝胶的疏水性。ALG/SPI气凝胶能够吸收1.34 ~ 10.3 g/g的模型污染物(即废机油、重质油和氯仿),最高吸收效率可达91%。值得注意的是,ALG/SPI 1_1.5似乎是最有效的,在40至80°C的温度下吸收废油,具有高表面积(210 m2∙g−1),重量轻(0.107 g·cm−3),在196°C以上热稳定,可重复使用多达四次。ALG/SPI气凝胶保持漂浮,保留吸收的污染物,可生物降解,从而减少使用后对环境的影响。该研究表明,ALG/SPI混合气凝胶是油水分离行业中很有前途的吸油材料。
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引用次数: 0
Porous silica nanoparticles as natural drug delivery system inhibit myocardial ischemia-reperfusion injury by alleviating oxidative stress 多孔二氧化硅纳米颗粒作为天然给药系统通过减轻氧化应激抑制心肌缺血再灌注损伤
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-11 DOI: 10.1007/s10934-025-01842-6
Jun Pu, Rongchuan Yue, Yanman Li, Ofe Eugene Kwaku

In this study, we developed a novel drug delivery system, PAA-2@pSiNPs@1, designed to enhance drug loading capacity and control drug release, particularly for the treatment of AMI. The composite material was synthesized by incorporating PAA-2 into pSiNPs, with compound 1 successfully encapsulated within the structure. The PAA-2 coating significantly influenced the drug release kinetics, improving the stability of the drug-loaded nanoparticles. Furthermore, the PAA-2@pSiNPs@1 system demonstrated excellent selective detection of Troponin in complex environments, making it especially suitable for AMI diagnosis and monitoring. Additionally, drug release studies were conducted in phosphate-buffered saline (PBS) at different pH values (pH 7.4, 6.5, and 4) to simulate physiological conditions. The results revealed pH-dependent release characteristics. At physiological pH (7.4), drug release was slow, whereas at lower pH values, the release rate was faster, showcasing the system’s potential for controlled drug release. The composite material exhibited high drug loading efficiencies for both hydrophilic and hydrophobic drugs, such as DOX, paclitaxel (PTX), and SN-38, further confirming its broad applicability in various drug delivery systems. Finally, using an ischemia/reperfusion (I/R) injury model in H9c2 cells, we evaluated the inhibitory effect of PAA-2@pSiNPs@1 on oxidative stress-induced myocardial cell damage.

在这项研究中,我们开发了一种新的药物递送系统PAA-2@pSiNPs@1,旨在提高药物负载能力和控制药物释放,特别是用于治疗AMI。将PAA-2加入到pSiNPs中合成复合材料,化合物1成功封装在结构中。PAA-2包被显著影响了载药纳米颗粒的释放动力学,提高了载药纳米颗粒的稳定性。此外,PAA-2@pSiNPs@1系统在复杂环境下对肌钙蛋白具有出色的选择性检测,特别适用于AMI的诊断和监测。此外,在不同pH值(pH 7.4、6.5和4)的磷酸盐缓冲盐水(PBS)中进行药物释放研究,以模拟生理条件。结果显示ph依赖性释放特性。在生理pH值(7.4)下,药物释放缓慢,而在较低的pH值下,释放速度更快,表明该系统具有控制药物释放的潜力。该复合材料对DOX、紫杉醇(PTX)、SN-38等亲疏水性药物均表现出较高的载药效率,进一步证实了其在各种药物传递系统中的广泛适用性。最后,通过H9c2细胞缺血再灌注(I/R)损伤模型,我们评估了PAA-2@pSiNPs@1对氧化应激诱导的心肌细胞损伤的抑制作用。
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引用次数: 0
Highly porous cross-linked graphene nanoplatelets-polyvinyl alcohol (GNP/PVA) aerogel for the removal of Ciprofloxacin from water 用于从水中去除环丙沙星的高孔交联石墨烯纳米片聚乙烯醇(GNP/PVA)气凝胶
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-11 DOI: 10.1007/s10934-025-01845-3
Nursyahirah Che Abd Rahman, Wan Hazman Danial, Ahmad Fakhrurrazi Ahmad Noorden, Zaiton Abdul Majid

Ciprofloxacin (CIP), a widely used fluoroquinolone antibiotic, has emerged as a significant pharmaceutical contaminant in water bodies, raising environmental and public health concerns due to its persistence and resistance to conventional wastewater treatment methods. This study reports the fabrication and application of a highly porous, cross-linked graphene nanoplatelets/polyvinyl alcohol (GNP/PVA) composite aerogel for the adsorption-based removal of CIP from aqueous solutions. The aerogel was synthesized via solution casting and freeze-drying, with maleic acid serving as the cross-linking agent. Characterization using Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), and Thermogravimetric Analysis (TGA) confirmed the aerogel’s porous structure, chemical cross-linking, and thermal stability. The adsorption of CIP by the aerogel was investigated through a batch adsorption process, optimizing various parameters such as solution pH, aerogel dosage, and initial CIP concentration over a three-day period. The optimization revealed that the adsorption process was most efficient at pH 4, using 60 mg of aerogel and an initial CIP concentration of 23 ppm. Under these conditions, the cross-linked GNP/PVA aerogel demonstrated promising potential for effective CIP removal, highlighting its applicability for treating pharmaceutical-laden effluents in municipal and hospital wastewater systems.

环丙沙星(CIP)是一种广泛使用的氟喹诺酮类抗生素,已成为水体中重要的药物污染物,由于其持久性和对传统废水处理方法的抗性,引起了环境和公共卫生问题。本研究报道了一种高孔交联石墨烯纳米片/聚乙烯醇(GNP/PVA)复合气凝胶的制备和应用,用于吸附去除水溶液中的CIP。以顺丁酸为交联剂,通过溶液浇铸和冷冻干燥法制备了该气凝胶。利用扫描电镜(SEM)、傅里叶变换红外光谱(FTIR)和热重分析(TGA)进行表征,证实了气凝胶的多孔结构、化学交联和热稳定性。通过对溶液pH、气凝胶用量、初始CIP浓度等参数的优化,研究了气凝胶对CIP的吸附效果。优化结果表明,在pH为4、气凝胶用量为60 mg、初始CIP浓度为23 ppm时,吸附效果最佳。在这些条件下,交联GNP/PVA气凝胶显示出有效去除CIP的潜力,突出了其在处理市政和医院废水系统中含有药物的废水中的适用性。
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引用次数: 0
Development of α-mangostin-loaded silica nanoparticles with enhanced protein-bound uremic toxin adsorption and biocompatibility α-山竹苷负载的二氧化硅纳米颗粒的开发,具有增强的蛋白结合尿毒症毒素吸附和生物相容性
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-11 DOI: 10.1007/s10934-025-01843-5
Sumarni Mansur, Muhammad Nidzhom Zainol Abidin

Hemoperfusion is a promising alternative to hemodialysis, particularly for removing protein-bound uremic toxins such as p-Cresol, which are poorly eliminated by conventional dialysis due to their strong affinity to plasma proteins. However, current adsorbents often suffer from limited adsorption efficiency and poor biocompatibility. This study presents the development of α-mangostin-loaded silica nanoparticles to enhance both adsorption performance and biocompatibility for potential blood purification applications. Mesoporous silica nanoparticles (15–25 nm) were synthesized and functionalized with 0.5 and 1.5 wt% α-mangostin. Their performance was evaluated through p-Cresol adsorption and nitric oxide scavenging assays. At an initial p-Cresol concentration of 250 mg/L, the adsorption capacities of pure α-mangostin, silica, silica/0.5mangostin, and silica/1.5mangostin were 15.87, 197.67, 179.49, and 185.67 mg/g, respectively. The incorporation of α-mangostin preserved silica’s adsorption capacity while enhancing antioxidant properties. Compared to plain silica, the α-mangostin-loaded nanoparticles increased clotting time by 21.5% and reduced reactive oxygen species by 36%, indicating improved biocompatibility. These results suggest that α-mangostin-loaded silica nanoparticles are promising candidates for multifunctional adsorbents with enhanced biocompatibility for blood purification.

血液灌流是一种很有前途的血液透析替代方案,特别是用于去除蛋白质结合的尿毒症毒素,如对甲酚,由于其与血浆蛋白的强亲和力,传统透析很难消除对甲酚。然而,目前的吸附剂往往存在吸附效率有限和生物相容性差的问题。本研究提出了α-山竹苷负载二氧化硅纳米颗粒的发展,以提高吸附性能和生物相容性,潜在的血液净化应用。合成了介孔二氧化硅纳米颗粒(15-25 nm),并以0.5和1.5 wt% α-山竹苷进行了功能化。通过对甲酚吸附和一氧化氮清除试验对其性能进行评价。对甲酚初始浓度为250 mg/L时,纯α-山竹苷、二氧化硅、二氧化硅/0.5山竹苷和二氧化硅/1.5山竹苷的吸附量分别为15.87、197.67、179.49和185.67 mg/g。α-山竹苷的掺入保留了二氧化硅的吸附能力,同时增强了其抗氧化性能。与普通二氧化硅相比,α-山竹苷纳米颗粒的凝血时间延长了21.5%,活性氧减少了36%,表明生物相容性得到改善。这些结果表明,α-山竹苷负载的二氧化硅纳米颗粒是具有增强生物相容性的多功能吸附剂,用于血液净化。
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引用次数: 0
High thermal insulation and thermal stability of silica aerogels via Ca2+ secondary phase doping 通过Ca2+二相掺杂制备高绝热性和热稳定性的二氧化硅气凝胶
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-11 DOI: 10.1007/s10934-025-01841-7
Chunman Li, Tong Liu, Weichun Chang, Wei Sun, Dong Su, Xiaolei Li

SiO2 aerogel has broad application prospects in thermal insulation fields such as aerospace, industrial energy conservation, and building energy saving. However, the high preparation cost and poor high-temperature stability limit its large-scale industrial production and application. Herein, CaSO4-modified SiO2 aerogel (SC) with low cost and high thermal stability was synthesized from water glass and CaSO4 via the sol-gel and supercritical drying route. The effect of CaSO4 doping amount on the morphology, pore structure and physical properties of SC was investigated. Results show that the effective doping of CaSO4 can significantly improve the heat resistance ability of SC at the temperature of 800–1000 ℃. After heated at 800 ℃ for 2 h, the weight loss of the modified aerogels was less than 7%, and the volume shrinkage rate was as low as 4%. The specific surface area of SCs (≥ 166 m2/g) after calcined at 1000 ℃ for 2 h were higher than that of the unmodified aerogels (119 m2/g). Mechanism analysis shows that not only Ca2+ can replace the active group Si-OH on the surface of the gel, reducing the intrinsic surface energy and sintering driving force of the gel particles and but also the Ca2SiO4 second phase is generated during the heating process, which hinders the contact growth of the particles and further improves the temperature resistance of the aerogel. These findings propose feasible ideas and methods for the application of SiO2 aerogel materials in high-temperature thermal insulation.

SiO2气凝胶在航空航天、工业节能、建筑节能等保温领域具有广阔的应用前景。但制备成本高,高温稳定性差,限制了其大规模工业生产和应用。以水玻璃和CaSO4为原料,经溶胶-凝胶和超临界干燥工艺合成了低成本、高热稳定性的CaSO4修饰SiO2气凝胶(SC)。研究了CaSO4掺杂量对SC的形貌、孔隙结构和物理性能的影响。结果表明,CaSO4的有效掺杂可以显著提高SC在800 ~ 1000℃的耐热性能。经800℃加热2 h后,改性气凝胶的失重率小于7%,体积收缩率低至4%。经1000℃煅烧2 h后,sc的比表面积(≥166 m2/g)高于未改性气凝胶的比表面积(119 m2/g)。机理分析表明,Ca2+不仅可以取代凝胶表面的活性基团Si-OH,降低凝胶颗粒的内在表面能和烧结驱动力,而且在加热过程中还会生成Ca2SiO4第二相,阻碍颗粒的接触生长,进一步提高气凝胶的耐温性。这些研究结果为SiO2气凝胶材料在高温绝热材料中的应用提供了可行的思路和方法。
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引用次数: 0
Methodological aspects of producing aluminosilicalites with typological structure of HZSM-5. Rational design and catalytic properties HZSM-5型铝硅石的生产方法研究。合理的设计和催化性能
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-08-11 DOI: 10.1007/s10934-025-01840-8
Elena Domoroshchina, Galina Kuz’micheva, Alexander Vasiliev, Ivan Pavlov, Larisa Pirutko, Olga Tkachenko, Alexander Kustov

In this work, the analysis and generalization of data on the elemental, phase and surface composition, crystal structure and microstructure of MFI-type HZSM-5 with Si/Al = 12, 25, 40, 300 were presented. Relationships between the composition of zeolite in HZSM-5 samples with different Si/Al and pore volume, specific surface, and framework voids area were established. Data obtained by electron microscopy and energy dispersive X-ray microanalysis explained the discrepancy between HZSM-5 real composition and the initial (as synthesized) one. Samples with the maximum content of Brønsted (HZSM-5 with Si/Al = 25) and Lewis (HZSM-5 with Si/Al = 12) acid sites responsible for the catalytic activity were identified using diffuse reflectance Fourier transform infrared spectroscopy. N2O decomposition reaction rate was found to decrease in the row HZSM-5(25) > HZSM-5(12) > HZSM-5(40) > HZSM-5(40)C > > HZSM-5(300). The high N2O decomposition rate demonstrated by HZSM-5(25) makes it promising catalyst. The second phase of iron oxides, found in all studied HZSM-5 as an impurity of the initial components, and the presence of faceted particles {001} oriented in HZSM-5(25) were shown to contribute to its maximum catalytic activity in N2O decomposition. The applied methodology for studying aluminosilicalites with different silicon to aluminum ratio and the revealed correlations can provide a fundamental perspective in studying other zeolites.

本文对Si/Al = 12、25、40、300时mfi型HZSM-5的元素组成、相组成、表面组成、晶体结构和显微组织等数据进行了分析和归纳。建立了不同Si/Al HZSM-5样品中沸石组成与孔隙体积、比表面积和骨架空隙面积的关系。电子显微镜和能量色散x射线显微分析数据解释了HZSM-5实际成分与初始(合成)成分之间的差异。利用漫反射傅里叶变换红外光谱技术鉴定了具有最大含量Brønsted (HZSM-5, Si/Al = 25)和Lewis (HZSM-5, Si/Al = 12)酸位的样品。N2O分解反应速率在HZSM-5(25) > HZSM-5(12) > HZSM-5(40) > HZSM-5(40)C > > HZSM-5(300)组依次降低。HZSM-5(25)具有较高的N2O分解率,是一种很有前景的催化剂。在所有研究的HZSM-5中都发现了氧化铁的第二相,作为初始组分的杂质,以及HZSM-5中定向的多面颗粒{001}的存在(25)被证明有助于其N2O分解的最大催化活性。研究不同硅铝比的铝硅石及其相关性的应用方法可为其他沸石的研究提供基础视角。
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引用次数: 0
Synthesis and hydrophobic modification of silica-CNT hybrid aerogels via one-pot and sol-gel methods using sustainable precursor 采用可持续前驱体的单罐法和溶胶-凝胶法合成二氧化硅-碳纳米管杂化气凝胶及其疏水改性
IF 3.2 4区 材料科学 Q2 CHEMISTRY, APPLIED Pub Date : 2025-07-24 DOI: 10.1007/s10934-025-01830-w
Emine Yapıcı, Berat Keçeci, Sevil Yücel

Silica-CNT hybrid aerogels (SCHAs) were fabricated using both one-pot synthesis (OPS) and conventional sol-gel methods. Following gelation, the samples were dried using two different techniques: ambient pressure drying (APD) and supercritical (CO_2) drying (SCD). Sustainable sodium silicate precursor was used. The gels were surface modified with trimethylchlorosilane (TMCS) and hexamethyldisilazane (HMDS), which acted as hydrophobizing silylating agents. The prepared aerogel was characterized by Brunauer-Emmett-Teller (BET) and Barrett–Joyner–Halenda (BJH) analyzer, thermogravimetric and differential thermal analyzer (TG-DTA), Fourier transform infrared spectrometer (FT-IR), field emission scanning electron microscope (FE-SEM) and contact angle analyzer for structural, thermal, functional, surface, morphological properties. Thermal stability of SCHAs investigated by TG-DTA shows a hydrophobic nature up to 600 °C. FE-SEM images confirmed the mesoporous nature of aerogels. The surface area and pore size were measured to range from 133 to 535 (m^2/g) and 3.55 to 9.46 nm, respectively, while the total pore volume was found to range from 0.24 to 1.39 (cm^3/g). The water contact angle (WCA) measurements affirm that most of the synthesized SCHAs exhibit excellent superhydrophobicity, with contact angles exceeding 154°.

采用一锅法和常规溶胶-凝胶法制备了二氧化硅-碳纳米管杂化气凝胶(SCHAs)。凝胶化后,使用两种不同的技术对样品进行干燥:环境压力干燥(APD)和超临界干燥 (CO_2) 干燥(SCD)。采用可持续硅酸钠前驱体。用三甲基氯硅烷(TMCS)和六甲基二矽氮烷(HMDS)作为疏水硅化剂对凝胶进行表面改性。采用brunauer - emmet - teller (BET)和Barrett-Joyner-Halenda (BJH)分析仪、热重和差热分析仪(TG-DTA)、傅里叶红外光谱仪(FT-IR)、场发射扫描电镜(FE-SEM)和接触角分析仪对制备的气凝胶进行了结构、热、功能、表面、形貌等方面的表征。TG-DTA对scha的热稳定性进行了研究,发现其在600℃以下具有疏水性。FE-SEM图像证实了气凝胶的介孔性质。表面积和孔径的测量范围为133 ~ 535 (m^2/g) 孔径大小分别为3.55 ~ 9.46 nm,总孔容大小为0.24 ~ 1.39 nm (cm^3/g). 水接触角(WCA)测量证实,大多数合成的scha具有优异的超疏水性,接触角超过154°。
{"title":"Synthesis and hydrophobic modification of silica-CNT hybrid aerogels via one-pot and sol-gel methods using sustainable precursor","authors":"Emine Yapıcı,&nbsp;Berat Keçeci,&nbsp;Sevil Yücel","doi":"10.1007/s10934-025-01830-w","DOIUrl":"10.1007/s10934-025-01830-w","url":null,"abstract":"<p>Silica-CNT hybrid aerogels (SCHAs) were fabricated using both one-pot synthesis (OPS) and conventional sol-gel methods. Following gelation, the samples were dried using two different techniques: ambient pressure drying (APD) and supercritical <span>(CO_2)</span> drying (SCD). Sustainable sodium silicate precursor was used. The gels were surface modified with trimethylchlorosilane (TMCS) and hexamethyldisilazane (HMDS), which acted as hydrophobizing silylating agents. The prepared aerogel was characterized by Brunauer-Emmett-Teller (BET) and Barrett–Joyner–Halenda (BJH) analyzer, thermogravimetric and differential thermal analyzer (TG-DTA), Fourier transform infrared spectrometer (FT-IR), field emission scanning electron microscope (FE-SEM) and contact angle analyzer for structural, thermal, functional, surface, morphological properties. Thermal stability of SCHAs investigated by TG-DTA shows a hydrophobic nature up to 600 °C. FE-SEM images confirmed the mesoporous nature of aerogels. The surface area and pore size were measured to range from 133 to 535 <span>(m^2/g)</span> and 3.55 to 9.46 nm, respectively, while the total pore volume was found to range from 0.24 to 1.39 <span>(cm^3/g)</span>. The water contact angle (WCA) measurements affirm that most of the synthesized SCHAs exhibit excellent superhydrophobicity, with contact angles exceeding 154°.</p>","PeriodicalId":660,"journal":{"name":"Journal of Porous Materials","volume":"32 6","pages":"2197 - 2210"},"PeriodicalIF":3.2,"publicationDate":"2025-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145493602","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}
引用次数: 0
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Journal of Porous Materials
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