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Sensitive determination of hydroquinone and catechol using an electrochemical sensor based on nitrogen-doped malic acid carbon quantum dots 利用基于掺氮苹果酸碳量子点的电化学传感器灵敏测定对苯二酚和邻苯二酚
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-22 DOI: 10.1016/j.matchemphys.2024.130077
Cheng Rong , Yanmei Huang , Xinyu Zheng
This study introduces an advanced electrochemical sensor fabricated by immobilizing nitrogen-doped malic acid carbon quantum dots (N-MCQDs) onto a glassy carbon electrode (GCE) via microwave-assisted synthesis and electrodeposition. The N-MCQDs were comprehensively characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and atomic force microscopy (AFM), confirming their successful synthesis and uniform distribution on the GCE surface. The N-MCQDs-modified GCE electrode (N-MCQDs/GCE) sensor displayed a remarkable linear detection range of 1–500 μM for hydroquinone (HQ) and 1–200 μM for catechol (CC), with ultra-low detection limits of 0.18 μM for HQ and 0.13 μM for CC. It also exhibits commendable stability, interference resistance, and the capability to accurately measure in complex real sample. These superior characteristics were attributed to the enhanced electrical conductivity and increased active sites due to nitrogen doping. This study not only broadens the application spectrum of carbon quantum dots but also offers a novel perspective for the design of high-performance electrochemical sensors for environmental analysis.
本研究介绍了一种先进的电化学传感器,其制作方法是通过微波辅助合成和电沉积将掺氮苹果酸碳量子点(N-MCQDs)固定在玻璃碳电极(GCE)上。利用高分辨率透射电子显微镜(HRTEM)、X 射线衍射(XRD)、傅立叶变换红外光谱(FTIR)、X 射线光电子能谱(XPS)、拉曼光谱和原子力显微镜(AFM)对 N-MCQDs 进行了全面表征,证实了它们的成功合成和在 GCE 表面的均匀分布。经 N-MCQDs 修饰的 GCE 电极(N-MCQDs/GCE)传感器对对苯二酚(HQ)的线性检测范围为 1-500 μM,对邻苯二酚(CC)的线性检测范围为 1-200 μM,对苯二酚(HQ)的超低检测限为 0.18 μM,对邻苯二酚(CC)的超低检测限为 0.13 μM。此外,它还具有出色的稳定性和抗干扰性,能够准确测量复杂的实际样品。这些优异特性归功于氮掺杂增强的导电性和增加的活性位点。这项研究不仅拓宽了碳量子点的应用范围,还为设计用于环境分析的高性能电化学传感器提供了新的视角。
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引用次数: 0
Enriched photocatalytic degradation of methylene orange dye using carbon quantum dots surface-decorated TiO2 nanocomposites 利用碳量子点表面装饰的 TiO2 纳米复合材料富集亚甲基橙染料的光催化降解能力
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-21 DOI: 10.1016/j.matchemphys.2024.130049
Asrianti B.T. Sunardi , Fadhillah Choirunnisa , Atika S.P. Dewi , Hendri Widiyandari , Yayuk Astuti , Osi Arutanti , Ali A. Salim , Nandang Mufti
Complex molecules in methylene orange (MO) dye-contaminated water are carcinogenic and mutagenic risks to human health. Carbon quantum dot surface-decorated titanium dioxide nanocomposites (CQD-TiO2 NCs) were synthesized via a sustainable hydrothermal method at concentrations of 1.5–3 mL. These NCs exhibits superior electron transfer, light harvesting capabilities, high stability, easy modification, optical characteristics, and photocatalytic properties. The surface morphology, porosity, physiochemical, and optical features of these CQD-TiO2 NCs were characterized using TEM, UV–Vis, PL, BET, BJH micromeritics, pHzpc, and photoelectrochemical measurements. The prepared NCs were evaluated against the photocatalytic degradation of MO dye molecules using a solar simulator system. The TEM revealed ultra-sensitive and tiny CQD materials with graphite phases ranging from 5 to 10 nm and attached to the octahedron surface of TiO2 NCs. The PL analysis observed three distinct emission peaks in the visible region, attributed to the near band edge, interstitial (Tii), and oxygen vacancy (V0). The BET and BJH analyses were conducted to determine the N2 adsorption-desorption surface area and mesoporous structure with pore sizes ranging from 2 to 50 nm. These NCs showed excellent photocatalytic performance, effectively degrading MO up to 99.00 % in a 3 mL variation, indicating that they could be a great candidate for photocatalytic purification of wastewater containing MO dyes.
亚甲基橙(MO)染料污染的水中的络合分子对人类健康具有致癌和致突变风险。通过可持续的水热法合成了碳量子点表面装饰的二氧化钛纳米复合材料(CQD-TiO2 NCs),浓度为 1.5-3 mL。这些纳米复合材料具有优异的电子传递、光收集能力、高稳定性、易改性、光学特性和光催化性能。利用 TEM、UV-Vis、PL、BET、BJH 微精密度、pHzpc 和光电化学测量对这些 CQD-TiO2 NCs 的表面形貌、孔隙率、物理化学和光学特征进行了表征。利用太阳能模拟系统对制备的 NCs 进行了 MO 染料分子光催化降解评估。TEM 显示了超灵敏的微小 CQD 材料,其石墨相从 5 纳米到 10 纳米不等,附着在 TiO2 NCs 的八面体表面上。聚光分析在可见光区域观察到三个不同的发射峰,分别归因于近带边、间隙(Tii)和氧空位(V0)。通过 BET 和 BJH 分析,确定了 N2 的吸附-解吸表面积以及孔径为 2 至 50 nm 的介孔结构。这些 NCs 表现出优异的光催化性能,在 3 mL 的变化中有效降解 MO 达 99.00%,表明它们是光催化净化含 MO 染料废水的理想候选材料。
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引用次数: 0
The differential influence of biochar and graphite precursors on the structural, optical, and electrochemical properties of graphene oxide 生物炭和石墨前驱体对氧化石墨烯结构、光学和电化学特性的不同影响
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130070
Hamidatu Alhassan , Voo Nyuk Yoong , Ying Woan Soon , Anwar Usman , Muhammad Saifullah Abu Bakar , Ashfaq Ahmed , Montri Luengchavanon
This study investigates the synthesis and characterization of graphene oxide (GO) derived from two distinct precursors: graphite and pyrolyzed acacia wood sawdust via a modified Hummers method. As hypothesized, the commercial graphite-derived GO (GOG) exhibited a more ordered structure characterized by a well-defined diffraction peak with interlayer separation of 0.86 nm and crystalline order of 8.18 nm, consistent with extensive oxidation. Conversely, the biochar-derived GO (GOB) displayed a heterogenous structure with a less defined (001) plane and an emerging (002) plane corresponding to mixed hybridization states (sp2/sp3) and mixed crystallinity at different regions in the materials. Additionally, it retained excess aromatic carbons (C–H bond) on its basal plane increasing its disorderliness and defect density. As a result, despite the G bands showing greater incorporation of functional groups in GOG, GOB recorded a higher ID/IG ratio (0.95 vs. 0.93). By retaining a relatively higher proportion of sp2 domains, GOB demonstrated enhanced light absorption through additional electronic transmission evident by its lower bandgap energy (2.93) compared to GOG (4.20), extending absorption into the visible range. Its improved properties were further characterized by enhanced conductivity, surface area, porosity, and decreased charge transfer and ion diffusion resistance. The study emphasizes that the nature of defects and their distribution, influenced by the precursor material can influence GO properties than those predicted by oxidation levels alone. It opens a new pathway to exploring bio-precursors and their potential in tailoring the properties of GO for specific applications.
本研究探讨了通过改进的 Hummers 方法合成和表征两种不同前体(石墨和热解相思木锯屑)衍生的氧化石墨烯 (GO)。正如假设的那样,商用石墨衍生的 GO(GOG)表现出更有序的结构,其特征是具有明确的衍射峰,层间间隔为 0.86 nm,结晶阶数为 8.18 nm,这与广泛的氧化作用相一致。相反,生物炭衍生的 GO(GOB)则显示出一种异质结构,其(001)平面不那么清晰,而(002)平面正在出现,这与材料中不同区域的混合杂化状态(sp2/sp3)和混合结晶度相对应。此外,它的基面上保留了过量的芳香碳(C-H 键),增加了其无序性和缺陷密度。因此,尽管 GOG 中的 G 带显示了更多的官能团,但 GOB 的 ID/IG 比值更高(0.95 对 0.93)。与 GOG(4.20)相比,GOB 的带隙能(2.93)更低,通过保留相对较高比例的 sp2 结构域,GOB 通过额外的电子传输增强了对光的吸收,从而将吸收范围扩大到可见光范围。其性能的改善还表现在导电性、表面积、孔隙率的提高,以及电荷转移和离子扩散阻力的降低。这项研究强调,缺陷的性质及其分布受前驱体材料的影响,对 GO 性能的影响超过了仅由氧化水平预测的影响。该研究为探索生物前驱体及其为特定应用定制 GO 性能的潜力开辟了一条新途径。
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引用次数: 0
Synthesis and EMI shielding study of Ni (II) semicarbazone driven nickel nanoparticles 镍 (II) 半咔唑酮驱动的镍纳米粒子的合成和电磁干扰屏蔽研究
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130064
Mruganchali A. Joshi, Pawan K. Khanna, Naeem Mohammad, Prasad Ganesh Joshi
Herein, we report the synthesis of nickel nanoparticles (Ni-NPs) from Ni (II) complexes of cyclic semicarbazone derivatives and their electromagnetic interference (EMI) shielding behaviour. Ni (II) complexes of cyclic semicarbazones were synthesized and characterized by various spectroscopic tools. It was observed that such complexes are excellent precursors for the synthesis of Ni-NPs when reduced by hydrazine hydrate. It is expected that the reaction kinetics will be ably normalized by the presence of semicarbazone ligand and that upon dissociation and partial consumption during nano-particle formation, will provide an added advantage of mild functionality around the particles. Overall various nickel complexes obtained from cyclic semicarbazones were tested as an effective precursor for the synthesis of Ni-NPs which were characterized by XRD, TEM, SEM, and AFM, and their magnetic behaviour was studied by VSM. EMI shielding efficiency of flexible Ni/PVA composite films showed shielding efficiency of about minus (−) 30 dB in X-band (8–12 GHz) for about 25 % loading in the PVA matrix.
在此,我们报告了利用环状半咔唑酮衍生物的 Ni (II) 复合物合成镍纳米颗粒(Ni-NPs)及其电磁干扰(EMI)屏蔽行为。研究人员合成了环状半咔唑酮的 Ni (II) 复合物,并利用各种光谱工具对其进行了表征。研究发现,当这种配合物被水合肼还原时,是合成镍-氮磷的极佳前体。预计半咔唑酮配体的存在将使反应动力学正常化,而且在纳米颗粒形成过程中,半咔唑酮配体的解离和部分消耗将为颗粒周围的温和功能性提供额外的优势。通过 XRD、TEM、SEM 和 AFM 对从环状半咔唑酮中获得的各种镍络合物进行了测试,将其作为合成 Ni-NPs 的有效前体,并通过 VSM 对其磁性行为进行了研究。柔性镍/PVA 复合薄膜的电磁干扰屏蔽效率显示,在 PVA 基体中的负载量约为 25% 时,X 波段(8-12 GHz)的屏蔽效率约为负(-)30 dB。
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引用次数: 0
Synthesis and characterization of ZnO and CuO coatings for antibacterial and antiviral applications 用于抗菌和抗病毒的氧化锌和氧化铜涂层的合成与表征
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130071
Zied Mannai , Wiem Bouslama , Ines Karkouch , Lamjed Bouslama , Kaouther Khlifi , Khalil Aouadi , Fatma Nouira
Copper oxide (CuO) and Zinc oxide (ZnO), coating have attracted attention for their potential antiviral properties, including their ability to combat virus. This study focuses on the development and characterization of self-disinfecting surface passivation films composed of CuO and ZnO, obtained using the spin-coating technique. The research aims to develop surfaces that can actively eliminate harmful microorganisms, reducing the risk of infections, while also offering strong mechanical resistance and adhesion to withstand external factors, which is crucial for ensuring long-term effectiveness. Additionally, the microstructural properties of the elaborated films were analyzed using SEM/EDS, which stands for Scanning Electron Microscopy/Energy Dispersive X-ray Spectroscopy and X-Ray diffraction analysis (XRD). The mechanical behavior was assessed through Vickers hardness and scratch resistance tests. It was found a dense and homogeneous thin films. The hardness of CuO and ZnO films were 11.14 ± 0.04 GPa, and 8.89 ± 0.04 GPa respectively. Therefore, scratching tests revealed high adhesion properties with a critical load LC1 of 1.89 ± 0.02 N and 1.04 ± 0.02 N for CuO and ZnO films respectively. Then, this study revealed that CuO and ZnO films exhibit excellent antimicrobial activity against Staphylococcus aureus ATCC 29213, as well as outstanding antiviral activity against the HSV-2 virus.
氧化铜(CuO)和氧化锌(ZnO)涂层因其潜在的抗病毒特性(包括抗病毒能力)而备受关注。本研究的重点是开发和表征利用旋涂技术获得的由氧化铜和氧化锌组成的自消毒表面钝化膜。该研究旨在开发能主动消除有害微生物、降低感染风险的表面,同时还能提供强大的机械阻力和附着力,以抵御外部因素的影响,这对于确保长期有效性至关重要。此外,还使用 SEM/EDS(即扫描电子显微镜/能量色散 X 射线光谱和 X 射线衍射分析 (XRD))分析了精心制作的薄膜的微观结构特性。机械性能通过维氏硬度和抗划痕测试进行评估。结果发现薄膜致密且均匀。氧化铜和氧化锌薄膜的硬度分别为 11.14 ± 0.04 GPa 和 8.89 ± 0.04 GPa。因此,划痕测试表明 CuO 和 ZnO 薄膜具有很高的附着力,临界载荷 LC1 分别为 1.89 ± 0.02 N 和 1.04 ± 0.02 N。研究还发现,CuO 和 ZnO 薄膜对金黄色葡萄球菌 ATCC 29213 具有出色的抗菌活性,对 HSV-2 病毒也具有出色的抗病毒活性。
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引用次数: 0
Antibacterial and wound healing activity of non-thermal plasma treated and MXene (Ti3C2TX)/ WO3 coated cotton fabrics 非热等离子体处理和 MXene (Ti3C2TX)/WO3 涂层棉织物的抗菌和伤口愈合活性
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130072
Udaya Vaka, M.C. Ramkumar
In this study, MXene (Ti3C2Tx)/WO3 nanocomposite was directly deposited on the surface of non-thermal plasma treated cotton fabrics. Initially, argon was used as a plasma forming gas to treat the surface of cotton fabrics. Subsequently, the MXene (Ti3C2Tx)/WO3 nanocomposite was deposited on the surface of non-thermal plasma treated cotton fabrics by co-precipitation method. As prepared cotton fabrics were characterized by various characterization techniques that includes, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Field emission scanning electron microscopy (FESEM) with energy-dispersive X-ray (EDX) analysis, and Contact Angle (CA) measurement. SEM and FTIR analysis confirmed the presence of MXene (Ti3C2Tx)/WO3 nanocomposite on the surface of cotton fabrics. In addition, contact angle analysis unveiled the super hydrophilic nature of cotton fabrics after surface modification. The antibacterial activity and the wound healing assay of the untreated and surface modified cotton fabrics were examined by in vitro analysis. Results unveiled that the surface modified cotton fabrics showed excellent antibacterial activity against gram-negative bacteria (Escherichia coli) and gram-positive bacteria (Staphylococcus aureus) and substantial wound healing activity. From this investigation it is inferred that plasma treated and nanocomposite functionalised cotton fabrics have the potential to be employed as wound dressing material.
在这项研究中,MXene(Ti3C2Tx)/WO3 纳米复合材料被直接沉积在经过非热等离子体处理的棉织物表面。首先,使用氩气作为等离子体形成气体来处理棉织物表面。随后,通过共沉淀法将 MXene(Ti3C2Tx)/WO3 纳米复合材料沉积在经过非热等离子体处理的棉织物表面。对制备的棉织物采用了多种表征技术,包括 X 射线衍射 (XRD)、傅立叶变换红外光谱 (FTIR)、场发射扫描电子显微镜 (FESEM) 和能量色散 X 射线 (EDX) 分析以及接触角 (CA) 测量。扫描电子显微镜和傅立叶变换红外光谱分析证实了棉织物表面存在 MXene(Ti3C2Tx)/WO3 纳米复合材料。此外,接触角分析揭示了棉织物表面改性后的超亲水性。体外分析检验了未处理棉织物和表面改性棉织物的抗菌活性和伤口愈合试验。结果表明,表面改性棉织物对革兰氏阴性菌(大肠杆菌)和革兰氏阳性菌(金黄色葡萄球菌)具有极佳的抗菌活性,并具有显著的伤口愈合活性。这项研究推断,经过等离子处理和纳米复合功能化的棉织物有望用作伤口敷料。
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引用次数: 0
Nanostructural evolution by applying various fuels in combustion design of CuZnAl mixed-oxides over HZSM-5 used in one-step production of CH3–O–CH3 在一步法生产 CH3-O-CH3 的 HZSM-5 上使用 CuZnAl 混合氧化物的燃烧设计中应用各种燃料实现纳米结构演变
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130063
Reza Khoshbin , Mohammad Haghighi , Shima Oruji
The influence of different fuels (urea, ethylene glycol and citric acid) in combustion-based design of nano-structured CuO–ZnO–Al2O3/HZSM-5 catalyst was investigated. The catalytic performance were evaluated in a single step production of dimethyl ether form syngas. The X-ray diffraction, Field emission scanning electron microscopy, Transmission electron microscopy, Energy-dispersive x-ray, Temperature Programmed Reduction-H2, N2 Adsorption and Desorption isotherms and Fourier-transform infrared spectroscopy techniques were used to characterize physico-chemical properties of prepared nanocatalysts. The X-ray diffraction results clarified that application of citric acid increased relative crystallinity of Cu and Zn oxides existed in catalyst structure. The Fourier-transform infrared spectroscopy results demonstrated that the zeolite structure was not destroyed after CuO–ZnO–Al2O3/HZSM-5 introduction. The Field emission scanning electron microscopy and Transmission electron microscopy images illustrated that the nanocatalyst synthesized with citric acid has the highest porosity and less population of particle agglomerations. The highest amount of surface area was obtained when citric acid was used as fuel. According to Temperature Programmed Reduction-H2 profiles, the reducibility of nanocatalyst synthesized with citric acid is higher than other samples. The activity of the fabricated nanocatalysts for syngas to Dimethyl ether process were tested at temperature and pressure range of 225–300 °C and 10–40 bar, respectively. Using citric acid as fuel led to achieve greater amount carbon monoxide conversion and Dimethyl ether yield. Furthermore, stability test represented that the activity of this nanocatalyst remained quite stable during 1060 min.
研究了不同燃料(尿素、乙二醇和柠檬酸)对基于燃烧设计的纳米结构 CuO-ZnO-Al2O3/HZSM-5 催化剂的影响。评估了催化剂在以合成气为原料单步生产二甲醚过程中的性能。利用 X 射线衍射、场发射扫描电子显微镜、透射电子显微镜、能量色散 X 射线、温度编程还原-H2、N2 吸附和解吸等温线以及傅立叶变换红外光谱技术对制备的纳米催化剂的物理化学性质进行了表征。X 射线衍射结果表明,柠檬酸的使用增加了催化剂结构中铜和锌氧化物的相对结晶度。傅立叶变换红外光谱结果表明,在引入 CuO-ZnO-Al2O3/HZSM-5 后,沸石结构没有被破坏。场发射扫描电子显微镜和透射电子显微镜图像表明,用柠檬酸合成的纳米催化剂具有最高的孔隙率和较少的颗粒团聚。使用柠檬酸作为燃料时,获得的表面积最大。根据温度编程还原-H2 曲线,用柠檬酸合成的纳米催化剂的还原性高于其他样品。在温度和压力分别为 225-300 ℃ 和 10-40 巴的范围内,测试了合成气制二甲醚过程中制备的纳米催化剂的活性。使用柠檬酸作为燃料可获得更高的一氧化碳转化率和二甲醚产率。此外,稳定性测试表明,这种纳米催化剂在 1060 分钟内保持了相当稳定的活性。
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引用次数: 0
Facile preparation of three-dimensional copper foam incorporated with Au/CuO nanorods as a durable, reusable and efficient SERS substrate 简便制备加入金/铜氧化物纳米棒的三维泡沫铜,作为耐用、可重复使用和高效的 SERS 基底
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130067
Huy Hoang Do , Cong Doanh Sai , Quang Hoa Nguyen , Bach Pham , Le Thanh Son , Tung Duy Vu
An exceptionally durable and recyclable three-dimensional copper foam (CF) modified CuO nanorods with Au nanostructures on its surface is noticeable for the application in surface-enhanced Raman scattering (SERS). The utilization of CF as a 3D frame substrate allowed for the advancement of its beneficial characteristics, such as an increased surface-active area resulting from its high porosity and superior chemical/physical stability. By thermally oxidizing CF at a temperature of 500 °C, CuO nanorods were fabricated directly onto CF to exploit its advantageous properties, such as its high surface-active area and photodegradation effect. Following that, Au nanostructures were deposited onto the surfaces of CuO nanorods via photoreduction. The purpose of incorporating Au nanostructures was to optimize the SERS phenomenon, since Au exhibits high SERS efficiency and excellent surface stability. The Au/CuO@CF SERS substrate demonstrated the capability to measure MB at a concentration of 0.1 nM. Meanwhile, the recyclability of the Au/CuO@CF was evaluated by subjecting it to UV irradiation three times while utilizing MB samples. Subsequently, the Au/CuO@CF substrate's physical durability was evaluated via sandpaper abrasion test. In addition to confirming the long-term usability, the Au/CuO@CF demonstrated its resilience by maintaining good measurement performance even after being subjected to ambient air for up to 25 days.
一种非常耐用且可回收的三维泡沫铜(CF)改性氧化铜纳米棒,其表面具有金纳米结构,可用于表面增强拉曼散射(SERS)。利用 CF 作为三维框架基底可提高其有益特性,如高孔隙率带来的更大表面活性面积和优异的化学/物理稳定性。通过在 500 °C 的温度下对 CF 进行热氧化,直接在 CF 上制备出氧化铜纳米棒,以利用其优势特性,如高表面活性面积和光降解效应。随后,通过光诱导将金纳米结构沉积到 CuO 纳米棒的表面。加入金纳米结构的目的是优化 SERS 现象,因为金具有很高的 SERS 效率和出色的表面稳定性。Au/CuO@CF SERS 基底能够测量浓度为 0.1 nM 的甲基溴。同时,在使用甲基溴样品时,对 Au/CuO@CF 进行了三次紫外线照射,以评估其可回收性。随后,通过砂纸磨损测试评估了 Au/CuO@CF 基质的物理耐久性。除了证实其长期可用性外,Au/CuO@CF 在环境空气中暴露长达 25 天后仍能保持良好的测量性能,这也证明了它的韧性。
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引用次数: 0
Microstructural analysis of inversion degree in sol-gel synthesized spinel MnCo2O4 particles 溶胶凝胶合成尖晶石 MnCo2O4 粒子反转度的微观结构分析
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130069
Erik Padilla-Zarate , Priscila Sepúlveda , Ana C. Murrieta , Miguel Hesiquio-Garduño , Danyel Cavazos-Cavazos , M.B. Hernández , J.A. Aguilar-Martínez , Flavio F. Contreras-Torres
Spinel-type compounds exhibit versatile structural and functional properties, which stems from the unique cation distribution that spans a spectrum from partial to total cell inversion degrees.
In this study, we investigated the preparation of MnCo₂O₄ particles synthesized via a modified sol-gel method. The synthesized particles were thoroughly characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy, and Rietveld refinements to assess their microstructural properties. The impact of different annealing temperatures (1000, 1100, and 1200 °C) and durations (1 and 8 h) on the crystal evolution of the synthesized particles was systematically investigated to assess the structural adaptability of the MnCo₂O₄ spinel under these synthesis conditions. The degree of inversion and oxygen positional parameters within the crystalline systems were quantified using the Bertaut method to obtain the specific arrangement of manganese and cobalt ions for inversion degrees from approximately 0.85 (random) to 1.00 (inversion) with the presence of a secondary phase of Co3O4 (20 wt%). The lattice parameter was determined from Rietveld analysis to be 8.2720 and 8.2927 Å for the normal and inverted spinel, respectively. Finally, the I(220)/I(400) and I(400)/I(422) intensity ratios were identified as reliable indicators of inversion degree, with these intensities ratios significantly influenced by the oxygen positional parameter.
尖晶石型化合物具有多变的结构和功能特性,这源于其独特的阳离子分布,其分布范围从部分晶胞反转度到完全晶胞反转度。利用 X 射线衍射、扫描电子显微镜、拉曼光谱和里特维尔德细化法对合成颗粒进行了全面表征,以评估其微观结构特性。系统研究了不同退火温度(1000、1100 和 1200 °C)和持续时间(1 和 8 小时)对合成颗粒晶体演化的影响,以评估锰钴₂O₄尖晶石在这些合成条件下的结构适应性。使用 Bertaut 方法对晶体系统中的反转度和氧位置参数进行了量化,从而得到了锰和钴离子在反转度约为 0.85(随机)到 1.00(反转)之间的特定排列,同时还存在 Co3O4(20 wt%)辅助相。根据里特维尔德分析法,正常尖晶石和反转尖晶石的晶格参数分别为 8.2720 Å 和 8.2927 Å。最后,I(220)/I(400)和 I(400)/I(422)强度比被确定为反转程度的可靠指标,这些强度比受到氧位置参数的显著影响。
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引用次数: 0
One-step synthesis of Zn-doped nickel sulfide/graphene derived from Ni-MOF for supercapacitor application 一步合成由 Ni-MOF 衍生的掺杂锌的硫化镍/石墨烯,用于超级电容器
IF 4.3 3区 材料科学 Q2 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-10-19 DOI: 10.1016/j.matchemphys.2024.130068
Morteza Moradi , Shokoufeh Zolfaghari , Mehdi Pooriraj , Mohsen Babamoradi , Shaaker Hajati
A metal sulfide derived from a metal-organic framework (MOF) was synthesized to be used as the active material for the supercapacitor's electrode. In this article, nickel-MOF was hydrothermally synthesized through a facile method; then, the synthesized MOF was doped with Zinc and composited with graphene oxide (GO) in different concentrations. Then, the composites that were achieved were sulfurized to study the improvement of the synthesized active materials. The synthesized materials were characterized with XRD, FESEM, EDS, and N2 adsorption-desorption hysteresis techniques. The fabricated electrodic active materials were studied employing cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy techniques. Comparing the electrochemical performance of the synthesized sulfides revealed that the electrode with a higher amount of GO has the best electrochemical performance among other compositions with the specific capacitance of 442.66 F/g, which was obtained at a current density of 1 A/g. In addition, the asymmetric supercapacitor cell consisting of the mentioned electrode as the positive electrode and activated carbon as the negative electrode provided a power density of 774.99 W/kg at the maximum energy density of 2.142 Wh/kg and a higher cycling stability of 96 % retention at about 10,000 cycles.
本文合成了一种由金属有机框架(MOF)衍生的金属硫化物,并将其用作超级电容器电极的活性材料。本文通过一种简便的方法水热合成了镍-MOF,然后在合成的 MOF 中掺入锌,并与不同浓度的氧化石墨烯 (GO) 复合。然后,对得到的复合材料进行硫化处理,以研究合成活性材料的改进情况。利用 XRD、FESEM、EDS 和 N2 吸附-解吸滞后技术对合成材料进行了表征。利用循环伏安法、电静态充放电法和电化学阻抗谱技术对制备的电化学活性材料进行了研究。比较合成的硫化物的电化学性能发现,在电流密度为 1 A/g 时,含有较多 GO 的电极的比电容为 442.66 F/g,是其他成分中电化学性能最好的。此外,以上述电极为正极、活性炭为负极的不对称超级电容器电池在最大能量密度为 2.142 Wh/kg 时的功率密度为 774.99 W/kg,循环稳定性更高,在约 10,000 次循环中的保持率为 96%。
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Materials Chemistry and Physics
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