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Development of Fe/ZnO/H+-montmorillonite nanocomposite for effective cationic dye (Methylene blue) removal from aqueous solutions Fe/ZnO/H+-蒙脱土纳米复合材料对阳离子染料(亚甲基蓝)去除效果的研究
Pub Date : 2025-10-24 DOI: 10.1016/j.cinorg.2025.100128
Chandini Machahary , Angita Sarkar , Bipul Das , Sanjay Basumatary
Pollution from industrial dye waste is a major environmental concern, especially in water bodies. These synthetic dyes often contain toxic substances that harm aquatic life and affect water quality. In response to this matter, the current research goal is to enhance the Montmorillonite's (MMT) adsorption efficiency through its transformation with acid activation and doping of metal oxide. This study presents the synthesis of a hybrid composite (Fe/ZnO/H+-MMT), combining acid-activated MMT with Iron and zinc oxide nanoparticles as an efficient adsorbent for the extraction of MB dye from water. The composite was then characterized by multiple analytical techniques like Powder XRD, FT-IR, BET, FESEM, and HRTEM. At a neutral pH, 120 min of time period, 100 mg/L of starting dye concentration, and 0.8 g/L of adsorbent dose at room temperature, this composite removes MB to 97.54 ± 0.14 %. The Langmuir model revealed a highest monolayer adsorption capacity (qmax) of 169.49 mg/g with R2 = 0.9938 among the isotherm model, which indicates that the adsorption involves chemical interactions in the process of adsorption. In kinetic studies, this experiment fit the PSO quite well with R2 = 0.99887 and the BET surface area is 171.287 m2/g. These outcomes demonstrate the potential of the Fe/ZnO/H+-MMT composite as a highly effective and promising adsorbent for MB removal from aqueous medium.
工业染料废水的污染是一个主要的环境问题,特别是在水体中。这些合成染料通常含有有害水生生物和影响水质的有毒物质。针对这一问题,目前的研究目标是通过酸活化和掺杂金属氧化物对蒙脱土(MMT)的转化来提高其吸附效率。本研究合成了一种Fe/ZnO/H+-MMT杂化复合材料,将酸活化的MMT与氧化铁和氧化锌纳米粒子结合,作为一种高效的吸附剂,用于从水中提取MB染料。然后用粉末XRD、FT-IR、BET、FESEM和HRTEM等多种分析技术对复合材料进行了表征。在中性pH、120 min时间、起始染料浓度为100 mg/L、吸附剂剂量为0.8 g/L的室温条件下,该复合材料对MB的去除率为97.54±0.14%。Langmuir模型的吸附量最大,为169.49 mg/g,在等温线模型中R2 = 0.9938,说明吸附过程中存在化学相互作用。在动力学研究中,本实验与PSO拟合较好,R2 = 0.99887, BET表面积为171.287 m2/g。这些结果证明了Fe/ZnO/H+-MMT复合材料作为一种高效的、有前途的水介质中MB去除吸附剂的潜力。
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引用次数: 0
Comprehensive synthesis route of crystalline copper oxide nanoparticles: A crystallographic analysis with functional application 结晶氧化铜纳米颗粒的综合合成路线:晶体学分析及功能应用
Pub Date : 2025-10-17 DOI: 10.1016/j.cinorg.2025.100123
Md. Khalid Hossain Shishir , Mahfuzul Islam , Nafis Rahman Sayeem , Nurus Sabah Anam , Md. Rahadul Islam Shipon , Md. Rifat , Shanawaz Ahmed , Md. Tauhiduzzaman , Md. Ashraful Alam
The synthesis pathway plays a crucial role in determining the crystallographic and functional properties of copper oxide nanoparticles (CuO NPs). Here, present a comparative study of biological, chemical and physical synthesis routes, emphasizing their influence on structure–property relationships. Environmentally benign biological methods, utilizing plant extracts and microorganisms, yielded NPs with distinctive surface chemistries. In contrast, chemical techniques, such as precipitation and sol–gel, provided precise control over particle size and distribution. Physical methods, including thermal decomposition and laser ablation, produced highly pure nanostructures with well-defined crystallographic symmetry. Advanced characterization, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy and transmission electron microscopy revealed route-dependent variations in morphology, size and phase composition. XRD identified the (111) reflection as the most intense diffraction, though its dominance varied with growth conditions, confirming a monoclinic crystal structure and atomic packing factor of ∼0.65. XPS verified the CuO oxidation state and Fourier-transform infrared spectroscopy detected Cu–O stretching bands between 500 and 700 cm−1. The crystallographic attributes were directly linked to performance in antimicrobial activity, catalysis, gas sensing and energy storage. These findings establish a clear correlation between synthesis, structure and function, providing a framework for the targeted design of CuO NPs for advanced technological applications.
合成途径对氧化铜纳米颗粒的晶体学和功能特性起着至关重要的作用。本文对生物、化学和物理合成路线进行了比较研究,强调了它们对结构-性质关系的影响。环境友好的生物方法,利用植物提取物和微生物,产生具有独特表面化学性质的NPs。相比之下,沉淀法和溶胶-凝胶法等化学技术可以精确控制颗粒的大小和分布。物理方法,包括热分解和激光烧蚀,产生具有明确晶体对称性的高纯度纳米结构。高级表征,x射线衍射(XRD), x射线光电子能谱(XPS),扫描电子显微镜和透射电子显微镜揭示了路线依赖的形态,尺寸和相组成的变化。XRD发现(111)反射是最强烈的衍射,但其优势度随生长条件的变化而变化,证实了单斜晶结构和原子堆积系数为~ 0.65。XPS验证了CuO的氧化态,傅里叶变换红外光谱检测到500 ~ 700 cm−1之间的Cu-O拉伸带。晶体学属性与抗菌活性、催化、气体传感和储能性能直接相关。这些发现建立了合成、结构和功能之间的明确相关性,为有针对性地设计用于先进技术应用的CuO NPs提供了框架。
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引用次数: 0
Effect of reaction medium on crystallinity and morphological properties of precipitation-derived α-alumina nanocrystals 反应介质对沉淀衍生α-氧化铝纳米晶结晶度和形貌的影响
Pub Date : 2025-10-09 DOI: 10.1016/j.cinorg.2025.100124
Pulak Ghosh , Raton Kumar Bishwas , Md. Ashraful Alam , Fariha Zannat , Mohammad Mohsin , Shirin Akter Jahan
The synthesis of ultra-fine α-Al2O3 nanoparticles via the precipitation technique was explored with the influence of different reaction media such as deionized water, acetone, methanol, and ethanol on their crystallographic and morphological properties. The study highlights how medium polarity and surface energy affect crystal growth, structural organization, and phase purity. Characterization techniques, including XRD, DLS, UV–Vis spectroscopy, TGA-DSC, and zeta potential analysis, reveal distinct particle size, crystallinity, and thermal stability differences among the mediums. Crystallite size was calculated using multiple methods, including Scherrer, Williamson-Hall (W–H), Size-Strain Plot (S–S), Halder-Wagner (H–W), and Monshi-Scherer models, yielding sizes ranging from 53.54 nm to 85.61 nm. Methanol demonstrated the highest crystallinity (35.81 %), smallest crystallite size (53.54 nm), and notable thermal and mechanical properties. Bandgap analysis further supports superior mechanical performance for methanol-based synthesis, with a bandgap energy of 5.67 eV. These findings emphasize the potential of methanol as an optimal medium for the synthesis of α-Al2O3 nanoparticles with high industrial relevance in ceramics, coatings, and aerospace applications.
研究了沉淀法合成超细α-Al2O3纳米颗粒的方法,考察了不同反应介质(去离子水、丙酮、甲醇、乙醇)对其结晶学和形貌的影响。该研究强调了介质极性和表面能如何影响晶体生长、结构组织和相纯度。表征技术,包括XRD、DLS、UV-Vis光谱、TGA-DSC和zeta电位分析,揭示了不同介质之间不同的粒度、结晶度和热稳定性。采用Scherrer、Williamson-Hall (W-H)、size - strain Plot (S-S)、Halder-Wagner (H-W)和Monshi-Scherer模型等多种方法计算晶体尺寸,得到的晶体尺寸范围为53.54 nm ~ 85.61 nm。甲醇的结晶度最高(35.81%),晶粒尺寸最小(53.54 nm),具有良好的热力学性能。带隙分析进一步支持甲醇基合成具有优越的机械性能,带隙能量为5.67 eV。这些发现强调了甲醇作为合成α-Al2O3纳米颗粒的最佳介质的潜力,在陶瓷、涂料和航空航天应用中具有很高的工业相关性。
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引用次数: 0
Fe3O4 nanoparticle-modified exfoliated carbon paste electrode for enhanced electrochemical detection of dopamine 纳米Fe3O4修饰的脱屑碳糊电极增强多巴胺的电化学检测
Pub Date : 2025-10-04 DOI: 10.1016/j.cinorg.2025.100125
Soukaina El Abbadi , Abdelaziz Elgamouz , Abdel-Nasser Kawde , Mohamed Douma , Hajar El Moustansiri , Najib Tijani
An exfoliated carbon paste electrode modified with Fe3O4 (CPE/Fe) has been developed as an advanced electrochemical sensor for detecting dopamine in aqueous solutions. The structural and morphological characteristics of the modified electrode were investigated using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). A series of CPE/Fe were fabricated with varying concentrations (10–30 wt%) of Fe3O4. Among these, the electrode containing 20wt% Fe3O4 and exfoliated under the optimal conditions [CPE/Fe-20% (5V; 1s)], demonstrated the highest electrochemical area (0.323 cm2), as evaluated using the Ferri/Ferrocyanide redox system. DPV was identified as the best electrochemical technique for dopamine detection, showing a pronounced response of 34 μA for 0.5 μM DA in phosphate-buffered saline (PBS, pH 7.0). The sensor exhibited a wide linear detection range (1–1000 μM), with a limit of detection (LOD) of 0.024 μM and a limit of quantification (LOQ) of 0.081 μM. Importantly, the sensor demonstrated excellent selectivity for dopamine, with minimal interference (%RSD) from common compounds found in biological matrices such as uric acid (±3.1%), ascorbic acid (±4.2%), alanine (±5.3%), and adenine (±9.1%). It also effectively detected DA in human serum, highlighting its practical applicability. The CPE/Fe-20% (5V; 1s) electrode enables precise DA detection with high sensitivity and stability. This This electrode configuration supports advanced applications in neuroprosthetics and brain-machine interfaces driven by intelligent feedback systems.
制备了一种以Fe3O4 (CPE/Fe)修饰的剥离碳糊电极,作为检测水溶液中多巴胺的先进电化学传感器。利用x射线衍射(XRD)、傅里叶变换红外光谱(FTIR)和扫描电镜(SEM)研究了修饰电极的结构和形态特征。用不同浓度(10-30 wt%)的Fe3O4制备了一系列CPE/Fe。其中,在最佳条件[CPE/Fe-20% (5V; 1s)]下剥离的Fe3O4含量为20wt%的电极电化学面积最大(0.323 cm2),采用Ferri/ ferro氰氧化还原体系进行评价。DPV被认为是检测多巴胺的最佳电化学技术,在0.5 μM DA的磷酸盐缓冲盐水(PBS, pH 7.0)中表现出34 μA的显著响应。该传感器具有较宽的线性检测范围(1 ~ 1000 μM),检测限为0.024 μM,定量限为0.081 μM。重要的是,该传感器对多巴胺具有极好的选择性,对生物基质中常见化合物的干扰最小(%RSD),如尿酸(±3.1%)、抗坏血酸(±4.2%)、丙氨酸(±5.3%)和腺嘌呤(±9.1%)。该方法还能有效检测人血清中的DA,突出了其实用性。CPE/Fe-20% (5V; 1s)电极可实现精确的DA检测,具有高灵敏度和稳定性。这种电极配置支持由智能反馈系统驱动的神经修复和脑机接口的高级应用。
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引用次数: 0
Magnetized retrieve of Ag–TeO3/Fe3O4@TiO2 hybrid nanocomposites for optical, kinetically, half-life period and its photocatalytic assessment of methylene blue and methyl orange dyes Ag-TeO3 /Fe3O4@TiO2杂化纳米复合材料的光学、动力学、半衰期及其对亚甲基蓝和甲基橙染料的光催化评价
Pub Date : 2025-09-27 DOI: 10.1016/j.cinorg.2025.100122
A. Anbu , M. Dilipkumar , K. Jeyajothi , M. Rajasimman , M.S. Manojkumar
The present research effectively constructed a core-shell-shell structure of Ag–TeO3/Fe3O4@TiO2 utilizing Capsicum frutescence extract, which is both magnetized highly recoverable. The catalyst was applied to photo catalytically degrade the colorants methyl orange (MO) and methylene blue (MB). The catalyst's function was further examined using XRD, FTIR, SEM, TEM/HRTEM, VSM, BET isotherm and UV–Visible spectroscopic analysis. Thus, Ag–TeO3/Fe3O4@TiO2 exhibited magnetized characteristics, including a saturation magnetic of 51.9 emu/g and a bandwidth value of 2.5 eV and half life period of 91.9min−1. The photocatalytic breaking down of MO and MB dyes mirrored the Langmuir-Hinshelwood pattern. Breakdown could be observed at the MO and MB dyes after 45 and 50 min of radiation exposure, with MO and MB dye elimination efficiencies reaching 99.2 % and 98.2 %, correspondingly. Following five attempts of regenerating Ag–TeO3/Fe3O4@TiO2 demonstrated 96.96 % MO and MB dye elimination performance.
本研究利用辣椒提取物有效地构建了Ag-TeO3 /Fe3O4@TiO2的核-壳-壳结构,该结构具有高磁化可回收性。应用该催化剂对着色剂甲基橙(MO)和亚甲基蓝(MB)进行光催化降解。采用XRD、FTIR、SEM、TEM/HRTEM、VSM、BET等温线和紫外-可见光谱分析对催化剂的功能进行了进一步的表征。Ag-TeO3 /Fe3O4@TiO2的饱和磁性为51.9 emu/g,带宽值为2.5 eV,半衰期为91.9min−1。MO和MB染料的光催化分解反映了Langmuir-Hinshelwood模式。MO和MB染料在辐照45 min和50 min后均被击穿,MO和MB染料的去除率分别达到99.2%和98.2%。经过五次再生Ag-TeO3 /Fe3O4@TiO2,其MO和MB染料去除率达到96.96%。
{"title":"Magnetized retrieve of Ag–TeO3/Fe3O4@TiO2 hybrid nanocomposites for optical, kinetically, half-life period and its photocatalytic assessment of methylene blue and methyl orange dyes","authors":"A. Anbu ,&nbsp;M. Dilipkumar ,&nbsp;K. Jeyajothi ,&nbsp;M. Rajasimman ,&nbsp;M.S. Manojkumar","doi":"10.1016/j.cinorg.2025.100122","DOIUrl":"10.1016/j.cinorg.2025.100122","url":null,"abstract":"<div><div>The present research effectively constructed a core-shell-shell structure of Ag–TeO<sub>3</sub>/Fe<sub>3</sub>O<sub>4</sub>@TiO<sub>2</sub> utilizing <em>Capsicum frutescence extract</em>, which is both magnetized highly recoverable. The catalyst was applied to photo catalytically degrade the colorants methyl orange (MO) and methylene blue (MB). The catalyst's function was further examined using XRD, FTIR, SEM, TEM/HRTEM, VSM, BET isotherm and UV–Visible spectroscopic analysis. Thus, Ag–TeO<sub>3</sub>/Fe<sub>3</sub>O<sub>4</sub>@TiO<sub>2</sub> exhibited magnetized characteristics, including a saturation magnetic of 51.9 emu/g and a bandwidth value of 2.5 eV and half life period of 91.9min<sup>−1</sup>. The photocatalytic breaking down of MO and MB dyes mirrored the Langmuir-Hinshelwood pattern. Breakdown could be observed at the MO and MB dyes after 45 and 50 min of radiation exposure, with MO and MB dye elimination efficiencies reaching 99.2 % and 98.2 %, correspondingly. Following five attempts of regenerating Ag–TeO<sub>3</sub>/Fe<sub>3</sub>O<sub>4</sub>@TiO<sub>2</sub> demonstrated 96.96 % MO and MB dye elimination performance.</div></div>","PeriodicalId":100233,"journal":{"name":"Chemistry of Inorganic Materials","volume":"7 ","pages":"Article 100122"},"PeriodicalIF":0.0,"publicationDate":"2025-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145264795","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Structural evolution of inorganic SinPd2 (n = 1–17) clusters 无机SinPd2 (n = 1-17)簇的结构演化
Pub Date : 2025-09-24 DOI: 10.1016/j.cinorg.2025.100121
Madison Winkeler, Ciara N. Richardson, Ryan Carlin, Jonathan T. Lyon
The structures of silicon clusters doped with two palladium atoms have been explored using an unbiased global optimization technique, and the candidate structures further analyzed using density functional theory. The optimized geometries, stabilities, and electronic structures of Si1Pd2 – Si17Pd2 are reported, and several new lowest energy isomers are located for the first time impacting the relative cluster stabilities. Based on the relative energies, Si5Pd2, Si10Pd2, and Si16Pd2 are predicted to be the most stable clusters for the sizes considered here. A growth pattern in this size range is noted that primarily consists of trigonal and pentagonal structural motifs, the latter dominating for larger clusters once Pd atoms become encompassed in the silicon cluster framework. Palladium atoms bind exohedrally to the base cluster for smaller sized clusters, but begin to bind endohedrally once the cluster size reaches Si11Pd2 (for the first Pd atom) and Si16Pd2 (for the second Pd atom). Detailed analysis of the cluster's electronic structure indicate that palladium atoms have only a small partial charge, and that the frontier molecular orbitals consist primarily of palladium d and silicon p atomic orbitals.
利用无偏全局优化技术研究了掺杂两个钯原子的硅簇结构,并用密度泛函理论进一步分析了候选结构。本文报道了Si1Pd2 - Si17Pd2的优化几何形状、稳定性和电子结构,并首次发现了影响相对簇稳定性的几个新的最低能异构体。基于相对能量,Si5Pd2、Si10Pd2和Si16Pd2被预测为最稳定的星团。在此尺寸范围内的生长模式主要由三角形和五边形结构基序组成,一旦Pd原子被包含在硅簇框架中,后者就占主导地位。对于较小尺寸的簇,钯原子以外面状结合到基簇上,但一旦簇大小达到Si11Pd2(第一个Pd原子)和Si16Pd2(第二个Pd原子),钯原子就开始以内面状结合。对团簇电子结构的详细分析表明,钯原子只有少量的部分电荷,前沿分子轨道主要由钯d和硅p原子轨道组成。
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引用次数: 0
Advancements in thermoelectric materials and their performance for thermoelectric generators (TEGs): A short review 热电材料及其热电发电机性能的研究进展
Pub Date : 2025-09-20 DOI: 10.1016/j.cinorg.2025.100118
Md Habibur Rahman Aslam
Thermoelectric generators (TEGs) have garnered growing interest in recent years for their ability to convert heat directly into electricity through a solid-state, environmentally friendly, and low-maintenance process. Their noiseless operation and long service life make them attractive for a variety of applications. However, their broader deployment remains constrained by relatively low energy conversion efficiency, which is fundamentally determined by the dimensionless figure of merit (ZT) of the thermoelectric materials employed. This review provides a detailed examination of key thermoelectric materials, focusing on their ZT performance and relevance to TEG efficiency. The evolution of TEG technology is outlined-from its 19th-century origins to modern advancements aimed at enhancing performance. Particular emphasis is placed on widely used materials such as bismuth telluride, lead telluride, and skutterudites, alongside emerging candidates like clathrates and half-Heusler compounds. By exploring current trends and challenges in material development, this work offers valuable insights for improving TEG efficiency and advancing their role in sustainable energy systems, particularly for harvesting waste heat and other low-grade thermal sources.
近年来,热电发电机(teg)因其通过固态、环保和低维护的过程将热量直接转化为电能的能力而引起了越来越多的兴趣。它们的无噪音操作和长使用寿命使它们对各种应用具有吸引力。然而,它们的广泛应用仍然受到相对较低的能量转换效率的限制,这从根本上取决于所使用的热电材料的无量纲性能图(ZT)。这篇综述提供了一个详细的检查关键热电材料,重点是他们的ZT性能和相关的TEG效率。概述了TEG技术的演变-从19世纪的起源到旨在提高性能的现代进步。特别强调的是广泛使用的材料,如碲化铋,碲化铅和滑石,以及新兴的候选物,如包合物和半赫斯勒化合物。通过探索材料发展的当前趋势和挑战,这项工作为提高TEG效率和推进其在可持续能源系统中的作用提供了有价值的见解,特别是在收集废热和其他低品位热源方面。
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引用次数: 0
Preferred crystallographic design of monoclinic tenorite (CuO) nanocrystals by powder X-ray line diffraction 单斜钙长石(CuO)纳米晶体的粉末x射线线衍射优选结晶学设计
Pub Date : 2025-09-19 DOI: 10.1016/j.cinorg.2025.100119
Md. Ashraful Alam , Shanawaz Ahmed , Debasish Sarkar , Raton Kumar Bishwas , Shirin Akter Jahan
Explored extensive data analysis of the preferred design of monoclinic copper oxide (CuO) nanocrystals (NCs) synthesized by the unique co-precipitation route. The study highlights the effectiveness of XRD data analysis in obtaining comprehensive nanoparticle (NPs) properties, reducing the need for multiple experiments. Rietveld refinement analysis indicated that 100 % of the synthesized material comprised crystalline CuO NPs produced by the WPPF technique. XRD characterized the prominent crystalline phase, offering insights into the lattice parameters where a= 4.6864, b= 3.4287, c= 5.1321; α=β= 90°,γ= 99.4°; lattice volume 81.357 Å3, crystallite size 27.94 nm, microstrain 0.00414 Nm−2, specific surface area 34.03 m2/g, dislocation density 1.28 × 10−3 nm−2, preference growth 0.117, stress is 455.4 MPa, energy density 942.7 kJ/m3, crystallinity index 2.0559 and atomic packing factor (APF) 72.13 %. The nanoscale size was confirmed by UV absorbance at 224.12 nm (0.191 a. u.), an optical band gap of 5.99 eV, and an average zeta potential value of −31.0 mV, indicating good stability in the medium. TEM explored an average particle size of 11.99 nm with a uniform distribution of inner core structure, while a lower particle size explored that the surface to volume ratio is too high. The SAED denoted as (110), (11-1), (111), and (11-2) planes, which were revealed by XRD. The sharp ring spot pattern suggested that the synthesized CuO NCs were in a polycrystalline nature. The synthesized CuO NPs are completely pure and have an atomic mass of 79.89 % Cu and 20.11 % O, almost similar to the stoichiometry value. The crystallographic data confirm the efficient formation of highly crystalline and preferred growth of monoclinic CuO NPs, with an improved crystallinity of 47.48 %, surpassing the ICDD standard [04-012-7238] of 45.91 %.
对采用独特的共沉淀法合成单斜氧化铜纳米晶(CuO)的优选设计进行了广泛的数据分析。该研究强调了XRD数据分析在获得纳米颗粒(NPs)综合性能方面的有效性,减少了多次实验的需要。Rietveld细化分析表明,合成材料100%由WPPF技术产生的CuO纳米粒子组成。XRD表征了突出的晶相,并提供了晶格参数的分析,其中a= 4.6864, b= 3.4287, c= 5.1321;α=β= 90°,γ= 99.4°;晶格体积81.357 Å3,晶尺寸27.94 nm,微应变0.00414 nm−2,比表面积34.03 m2/g,位错密度1.28 × 10−3 nm−2,偏好生长0.117,应力455.4 MPa,能量密度942.7 kJ/m3,结晶度指数2.0559,原子堆积系数(APF) 72.13%。紫外吸光度为224.12 nm (0.191 a.u),光学带隙为5.99 eV,平均zeta电位值为- 31.0 mV,表明该材料在介质中具有良好的稳定性。TEM发现平均粒径为11.99 nm,内核结构分布均匀,而较低粒径则发现表面体积比过高。SAED分别表示为(110)、(11-1)、(111)、(11-2)面,由XRD分析得到。尖锐的环状斑点图表明合成的CuO纳米碳化物具有多晶性质。合成的CuO NPs完全纯净,Cu和O的原子质量分别为79.89%和20.11%,与化学计量值基本一致。晶体学数据证实了单斜CuO NPs的高效形成和高结晶性生长,结晶度提高了47.48%,超过了ICDD标准[04-012-7238]的45.91%。
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引用次数: 0
Highly sensitive and selective sensing of H2S gas based on CuO–SnO2 nanocomposite 基于CuO-SnO2纳米复合材料的高灵敏度和选择性H2S气体传感
Pub Date : 2025-09-18 DOI: 10.1016/j.cinorg.2025.100120
Sharad B. Patil , Ganesh E. Patil , Sarika D. Shinde , Dnyaneshwari Y. Patil , Dnyaneshwar D. Kajale , Fabian I. Ezema
This study investigates the influence of Cu/Sn atomic ratio on the structural, microstructural, electrical, and gas sensing properties of CuO–SnO2 nanocomposite thin films synthesized via air-assisted spray pyrolysis. X-ray diffraction (XRD) analysis confirmed the formation of a tetragonal SnO2 phase and monoclinic CuO phase, with dominant diffraction peaks corresponding to (110), (101), (200), and (211) planes of SnO2, along with (110) and (111) planes of CuO. The average crystallite sizes, calculated using the Scherrer formula, were found to be 26 nm, 30 nm, and 38 nm for samples with Cu/Sn atomic ratios of 0.54, 0.63, and 1.41 respectively. Scanning electron microscopy (SEM) revealed a direct correlation between Cu/Sn ratio and surface morphology. At a lower Cu/Sn ratio of 0.54, the films exhibited a dense structure with small, uniformly distributed grains, enhancing surface area and active sites for gas adsorption. At 0.63, grain growth increased moderately, balancing surface area and electrical conductivity. At the highest Cu/Sn ratio of 1.41, SEM images showed larger faceted grains with increased crystallinity and porosity, improving charge carrier mobility but reducing gas sensitivity due to a decreased active surface area. Elemental analysis (EDAX) confirmed the composition of Cu, Sn, and O in the films, with Cu (at%) increasing from 13.26 % to 16.69 % as the Cu/Sn ratio increased. Electrical conductivity measurements confirmed the semiconducting behavior of the films, with conductivity increasing with temperature. Gas sensing studies demonstrated that the Cu/Sn 50:50 composition exhibited the highest sensitivity to H2S gas at 350°C, with a maximum response of 4590 at 50 ppm concentration. Response and recovery times were recorded as ∼60 s and ∼110 s, respectively. The enhanced gas sensing performance is attributed to optimized heterojunction formation between p-type CuO and n-type SnO2, leading to improved charge carrier separation and sensor response. These findings underscore the crucial role of Cu/Sn ratio in tailoring film morphology and optimizing gas sensing performance. The study provides a foundation for developing high-performance metal oxide-based gas sensors with improved selectivity and response characteristics.
本文研究了Cu/Sn原子比对气助喷雾热解法制备CuO-SnO2纳米复合薄膜的结构、微观结构、电学和气敏性能的影响。x射线衍射(XRD)分析证实形成了SnO2的四方相和CuO的单斜相,主要衍射峰对应于SnO2的(110)、(101)、(200)和(211)面,以及CuO的(110)和(111)面。根据Scherrer公式计算,当Cu/Sn原子比为0.54、0.63和1.41时,样品的平均晶粒尺寸分别为26 nm、30 nm和38 nm。扫描电镜(SEM)结果表明,铜锡比与表面形貌有直接关系。当Cu/Sn比为0.54时,薄膜结构致密,颗粒小且分布均匀,增加了表面面积和气体吸附活性位点。在0.63时,晶粒生长适度增加,使表面积和电导率达到平衡。当Cu/Sn比达到1.41时,SEM图像显示出更大的多面晶粒,结晶度和孔隙度增加,提高了载流子迁移率,但由于活性表面积的减少而降低了气敏性。元素分析(EDAX)证实了薄膜中Cu、Sn和O的组成,随着Cu/Sn比的增加,Cu (at%)从13.26%增加到16.69%。电导率测量证实了薄膜的半导体行为,电导率随温度升高而增加。气敏研究表明,Cu/Sn 50:50组合物在350°C时对H2S气体的灵敏度最高,在50 ppm浓度下的最大响应为4590。反应时间和恢复时间分别记录为~ 60 s和~ 110 s。p型CuO和n型SnO2之间形成的异质结优化了气敏性能的增强,从而改善了载流子分离和传感器响应。这些发现强调了Cu/Sn比在调整膜形态和优化气敏性能方面的关键作用。该研究为开发具有更高选择性和响应特性的高性能金属氧化物气体传感器奠定了基础。
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引用次数: 0
Effect of ball milling jar geometry on MnO2 nanoparticle morphology and supercapacitor performance 球磨罐几何形状对二氧化锰纳米颗粒形貌和超级电容器性能的影响
Pub Date : 2025-09-15 DOI: 10.1016/j.cinorg.2025.100117
Dadaso D. Mohite , Sachin S. Chavan , Prasad E. Lokhande , P.B. Karandikar , P.V. Londhe , Udayabhaskar Rednam , Waqqas Ahsan , Vaishnavi B. Mohite
The performance of supercapacitors strongly depends on the structural and morphological characteristics of electrode materials. In this study, manganese dioxide (MnO2) nanoparticles were synthesized through optimized ball milling, and their electrochemical behavior was systematically evaluated. A Taguchi L9 orthogonal array was employed to optimize four key milling parameters - jar shape, ball size, milling speed, and milling time - using mass density as the primary response. Structural analysis (XRD, FTIR) confirmed the formation of crystalline tetragonal MnO2 with high phase purity, while SEM and EDS revealed nanoscale morphology and elemental uniformity. Among the parameters, ball size emerged as the most influential factor, followed by jar geometry, with the pentagonal jar enhancing particle refinement and compaction. These improvements translated into superior electrochemical performance, with the optimized MnO2 electrode delivering a specific capacitance of 276.53 F g−1 at 10 mV s−1 and retaining 80.52 % capacitance after 5000 cycles. The electrode exhibited a combination of EDLC-like and pseudocapacitive behavior, with Mn4+/Mn3+ redox features confirming its charge storage mechanism. This study demonstrates that rational design of milling parameters, particularly jar geometry, can effectively tailor MnO2 morphology and significantly enhance its supercapacitor performance.
超级电容器的性能在很大程度上取决于电极材料的结构和形态特征。本研究通过优化球磨法制备了二氧化锰纳米颗粒,并对其电化学性能进行了系统评价。以质量密度为主要响应参数,采用田口L9正交试验优化了球缸形状、球尺寸、铣削速度和铣削时间4个关键铣削参数。结构分析(XRD, FTIR)证实形成了具有高相纯度的方形MnO2晶体,SEM和EDS显示了纳米级形貌和元素均匀性。在各参数中,球的大小是影响最大的因素,其次是振子的几何形状,五角形的振子有利于颗粒的细化和压实。这些改进转化为优异的电化学性能,优化后的MnO2电极在10 mV s−1下的比电容为276.53 F g−1,在5000次循环后保持80.52%的电容。该电极表现出类似edlc和假电容的行为,Mn4+/Mn3+氧化还原特性证实了其电荷存储机制。该研究表明,合理设计铣削参数,特别是罐的几何形状,可以有效地定制MnO2的形态,并显着提高其超级电容器性能。
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Chemistry of Inorganic Materials
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