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Time-resolved electrochemical impedance spectroscopy study of calcium fluoride formation and ion transport dynamics in highly concentrated CaSO₄–NaF systems 高浓度硫酸钙-NaF体系中氟化钙形成及离子传递动力学的时间分辨电化学阻抗谱研究
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-21 DOI: 10.1016/j.ijoes.2025.101249
Meryem Bensemlali , Halima Mortadi , Abdellatif Aarfane , Abdoullatif Baraket , Abdelowahed Hajjaji , Fouad Belhora , Mina Bakasse , Najoua Labjar , Said Laasri , Hamid Nasrellah
This work investigates the reaction kinetics in a highly concentrated (×50) mixture of calcium sulfate (CaSO₄) and sodium fluoride (NaF) using real-time, in-situ Electrochemical Impedance Spectroscopy (EIS) over 48 h. The primary objective was to establish the electrochemical profile and monitor ion transport dynamics under aggressive, non-equilibrium conditions designed to accelerate precipitation kinetics. Analysis of the complex conductivity spectra (σ′ and σ′′) and Nyquist plots, modeled with an equivalent electrical circuit R₁(R₂//CPE), revealed two distinct kinetic regimes. The temporal evolution of the dc conductivity (σ₀) showed an initial decrease, followed by a rise, culminating in stabilization after approximately 19 h. This stabilization is interpreted as the establishment of a dynamic equilibrium state. Concurrent trends in the high-frequency conductivity (σ∞), CPE exponent (p), and relaxation time (τ) suggest significant microstructural evolution within the system. While the electrochemical data are consistent with the expected precipitation of CaF₂ and provide a kinetic profile suggesting a potentially faster route to equilibrium than traditional methods, this study focuses on establishing EIS as a monitoring tool. Direct analytical confirmation of the solid phase and quantitative yield analysis are recognized as essential next steps and are the focus of immediate future work.
本研究使用实时原位电化学阻抗谱(EIS)在48 h内研究了高浓度(×50)硫酸钙(CaSO₄)和氟化钠(NaF)混合物中的反应动力学。主要目的是建立电化学谱和监测离子在侵略性,非平衡条件下的传输动力学,旨在加速沉淀动力学。对复合电导率谱(σ′和σ′)和Nyquist图的分析,用等效电路R₁(R₂//CPE)建模,揭示了两种不同的动力学机制。直流电导率(σ 0)的时间演化表现为先下降后上升,在大约19 h后达到稳定。这种稳定被解释为动态平衡状态的建立。高频电导率(σ∞)、CPE指数(p)和弛豫时间(τ)的同步趋势表明,体系内的微观结构发生了显著的变化。虽然电化学数据与预期的CaF 2沉淀一致,并提供了一个动力学剖面,表明比传统方法更快地达到平衡,但本研究的重点是建立EIS作为监测工具。固相的直接分析确认和定量产率分析被认为是必不可少的下一步,也是近期工作的重点。
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引用次数: 0
Highly sensitive and selective electrochemical detection of amlodipine besylate using β-alanine-modified α-Fe₂O₃ nanoparticles β-丙氨酸修饰α-Fe₂O₃纳米颗粒电化学检测苯磺酸氨氯地平的高灵敏度和选择性
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-19 DOI: 10.1016/j.ijoes.2025.101242
Ananya S. Agnihotri, M. Nidhin
In this study, we present a highly selective and sensitive electrochemical sensor for the detection of Amlodipine besylate (AMP) using α-Fe2O3 nanoparticles (IO) functionalized with alanine (IOALA) to enhance electrochemical activity. The IO nanoparticles were synthesized through a starch-assisted template method and then modified with alanine, improving their stability and reducing agglomerate size. Comprehensive characterization of IOALA was conducted using XRD, FTIR, DLS, VSM, FESEM-EDX, HRTEM, and SAED, confirming the structural integrity and functionalization of the nanomaterial. The IOALA was subsequently immobilized on a glassy carbon electrode (GCE) to fabricate the IOALA/GCE sensor, where electrochemical parameters, including scan rate, electrolyte pH, and AMP concentration, were meticulously optimized. Differential pulse voltammetry (DPV) was employed to achieve precise quantification of AMP, revealing a remarkable detection limit of 1.29 nM and a broad linear dynamic range of 3.89 nM to 500.03 nM. The sensor demonstrated excellent reproducibility and selectivity, exhibiting high resistance to interference, making it reliable for real-sample analysis. Practical application was validated by detecting AMP in generic drug formulations, highlighting the sensor's potential for real-world pharmaceutical monitoring. This novel IOALA/GCE platform offers an efficient, cost-effective, and robust approach for AMP detection, contributing to the advancement of electrochemical sensors in pharmaceutical analysis.
在这项研究中,我们提出了一种高选择性和灵敏度的电化学传感器,用于检测苯磺酸氨氯地平(AMP),该传感器使用α-Fe2O3纳米粒子(IO)与丙氨酸(IOALA)功能化,以提高电化学活性。通过淀粉辅助模板法合成了IO纳米颗粒,然后用丙氨酸修饰,提高了其稳定性并减小了团聚体尺寸。利用XRD、FTIR、DLS、VSM、FESEM-EDX、HRTEM和SAED对IOALA进行了综合表征,证实了该纳米材料的结构完整性和功能化。随后将IOALA固定在玻璃碳电极(GCE)上制造IOALA/GCE传感器,并对扫描速率、电解质pH和AMP浓度等电化学参数进行了精心优化。采用差分脉冲伏安法(DPV)实现AMP的精确定量,检测限为1.29 nM,线性动态范围为3.89 nM ~ 500.03 nM。该传感器具有优异的再现性和选择性,具有高抗干扰性,可可靠地用于实际样品分析。通过检测仿制药配方中的AMP验证了实际应用,突出了传感器在现实世界药物监测中的潜力。这种新颖的IOALA/GCE平台为AMP检测提供了一种高效、经济、稳健的方法,促进了电化学传感器在药物分析中的发展。
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引用次数: 0
A comparative review of electrochemical sensing and QCL-based photoacoustic spectroscopy for ppb-Level SO₂ detection 电化学传感与qcl光声光谱在ppb级二氧化硫检测中的比较研究
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-17 DOI: 10.1016/j.ijoes.2025.101241
Yikun Wang, Wei Zhao, Yang Chen
The accurate monitoring of sulfur dioxide (SO2) at parts-per-billion (ppb) concentrations is critical for safeguarding public health and managing environmental quality. This review provides a critical comparative analysis of two prominent technologies for ppb-level detection: electrochemical (EC) sensors and Quantum Cascade Laser Photoacoustic Spectroscopy (QCL-PAS). These technologies represent a fundamental trade-off in modern gas sensing, pitting the low cost, scalability, and low power consumption of EC sensors against the superior sensitivity, selectivity, and stability of QCL-PAS. This paper delves into the materials science innovations driving the performance of EC sensors, including metal-oxide semiconductors, 2D materials, and metal-organic frameworks, while critically examining the persistent challenges of environmental susceptibility, cross-sensitivity to interfering gases, and long-term drift that complicate their field deployment. In parallel, the principles of QCL-PAS are detailed, highlighting system design advancements such as differential photoacoustic cells and quartz-enhanced photoacoustic spectroscopy that enable sub-ppb detection limits. The inherent limitations of this optical method, particularly the adsorption-desorption "memory effect" with polar molecules like SO2 and the influence of background gas composition on signal intensity, are thoroughly discussed. The analysis concludes that these technologies are not merely competitors but occupy distinct and complementary niches. Electrochemical sensors are ideally suited for high-density, spatially resolved monitoring networks where identifying trends and hotspots is prioritized, whereas QCL-PAS excels in applications demanding high-fidelity, legally defensible data, such as regulatory compliance, industrial process control, and reference-grade monitoring. The future of comprehensive SO2 monitoring likely lies in hybrid systems that leverage the strengths of both technologies, using high-accuracy QCL-PAS instruments to validate and calibrate vast networks of low-cost electrochemical sensors.
准确监测十亿分之一(ppb)浓度的二氧化硫(SO2)对于保障公众健康和管理环境质量至关重要。本文对电化学(EC)传感器和量子级联激光光声光谱(QCL-PAS)两种主要的ppb级检测技术进行了比较分析。这些技术代表了现代气体传感的基本权衡,将EC传感器的低成本、可扩展性和低功耗与QCL-PAS的高灵敏度、选择性和稳定性相结合。本文深入研究了推动EC传感器性能的材料科学创新,包括金属氧化物半导体、2D材料和金属有机框架,同时严格审查了环境敏感性、对干扰气体的交叉敏感性和使其现场部署复杂化的长期漂移等持续挑战。同时,详细介绍了QCL-PAS的原理,重点介绍了系统设计的进步,如差分光声电池和石英增强光声光谱,可实现亚ppb检测限。深入讨论了这种光学方法的固有局限性,特别是与SO2等极性分子的吸附-解吸“记忆效应”以及背景气体成分对信号强度的影响。分析得出的结论是,这些技术不仅是竞争对手,而且占据了独特而互补的利基。电化学传感器非常适合高密度、空间分辨的监测网络,在这些网络中,识别趋势和热点是优先考虑的,而QCL-PAS擅长要求高保真、合法可辩护的数据的应用,如法规遵守、工业过程控制和参考级监测。综合二氧化硫监测的未来可能在于利用这两种技术优势的混合系统,使用高精度的QCL-PAS仪器来验证和校准大量低成本的电化学传感器网络。
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引用次数: 0
Enhanced DC and RF performance of an SOI-MESFET with dual intrinsic layers and a doped channel bottom 具有双本质层和掺杂沟道底的SOI-MESFET的直流和射频性能增强
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-16 DOI: 10.1016/j.ijoes.2025.101240
Seyed Mohammad Razavi , Toktam Aghaee
In this paper, a proposed structure of SOI-MESFET with two intrinsic semiconductor layers at the top of the channel and an area with additional impurities in the channel bottom (IA-SOI) is presented. In addition to this structure, the transistor, which has only two intrinsic semiconductor layers at the top of the channel (I-SOI), is tested to determine the importance of the layer with more impurities in the channel bottom of IA-SOI. Some of the most important electrical parameters of the proposed transistors are studied and compared with those of the conventional structure (C-SOI). These parameters include drain current, electric field, breakdown voltage, gate-source capacitor, output resistance, maximum output power density and threshold voltage. The two intrinsic semiconductor layers of IA-SOI improve the breakdown voltage of this transistor by 45 % and reduce the gate-source capacitor by 18 % compared to those of the C-SOI. Also, the layer with additional impurities in the channel bottom of the proposed structure increases the drain current by 100 %. Simultaneous increase of drain current and breakdown voltage in IA-SOI significantly increases the maximum power density of this transistor compared to the conventional one. Comparing I-SOI with the conventional structure, it can be concluded that I-SOI increases the output resistance by 100 % compared to that in the C-SOI structure.
本文提出了一种SOI-MESFET的结构,该结构在沟道顶部有两个本禀半导体层,沟道底部有一个额外杂质区域(IA-SOI)。除了这种结构外,还测试了在通道(I-SOI)顶部只有两个本禀半导体层的晶体管,以确定IA-SOI通道底部含有更多杂质层的重要性。研究了所提出的晶体管的一些最重要的电参数,并与传统结构(C-SOI)的电参数进行了比较。这些参数包括漏极电流、电场、击穿电压、栅源电容、输出电阻、最大输出功率密度和阈值电压。与C-SOI相比,IA-SOI的两个本征半导体层使晶体管的击穿电压提高了45% %,栅极源电容减少了18% %。此外,在所提出的结构的通道底部具有额外杂质的层使漏极电流增加100 %。与传统晶体管相比,IA-SOI中漏极电流和击穿电压的同时增加显著提高了晶体管的最大功率密度。将I-SOI与常规结构进行比较,可以得出结论:与C-SOI结构相比,I-SOI的输出电阻增加了100 %。
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引用次数: 0
Flow field optimization for electrochemical machining of pit arrays in multiple rows 多排凹坑阵列电化学加工流场优化
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-12 DOI: 10.1016/j.ijoes.2025.101239
Bin He , Zhuwei Lu , Ziming Xue , Weining Lei
The flow field distribution is important to the processing quality of array structures in electrochemical machining (ECM). To solve the problem of poor consistency of multiple rows of pits, a flow field optimization method was proposed to reduce the height of the cathode teeth and add the flow channel and transition region. The flow field simulation results showed that there was evaporation under the initial flow field, and the flow velocity in the processing area of multiple rows of pits gradually decreased. The flow of electrolyte in the optimized flow field was more concentrated, the flow velocity in the processing area was greater than that in the non-processing area between rows, and the flow velocity in multiple rows of pits was more uniform. The pit arrays of 6 rows × 10 columns were processed by using the initial and optimized flow field. The pit arrays processed with the optimized flow field are more consistent; the standard deviations (SD) of the depth, length, and width of pits are 3.87μm, 10.16μm and 12.02μm, respectively. In addition, the optimized flow field also helps to reduce stray corrosion. This research has certain reference value for solving the processing problem of the anvil part of the endoscopic stapler.
在电化学加工中,流场分布对阵列结构的加工质量有重要影响。针对多排凹坑一致性差的问题,提出了一种降低阴极齿高度、增加流道和过渡区的流场优化方法。流场模拟结果表明,初始流场下存在蒸发现象,多排凹坑加工区内的流速逐渐减小。优化后的流场中电解液流动更加集中,排间加工区内流速大于非加工区内流速,多排凹坑内流速更加均匀。利用初始流场和优化后的流场对6行× 10列的坑阵进行处理。优化后的流场处理后的坑阵更加一致;凹坑深度、长度和宽度的标准差分别为3.87μm、10.16μm和12.02μm。此外,优化后的流场也有助于减少杂散腐蚀。本研究对解决内镜吻合器砧部的加工问题具有一定的参考价值。
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引用次数: 0
Capillary electrophoresis with electrochemical detection: A promising platform for anti-doping analysis 毛细管电泳电化学检测:一个很有前途的反兴奋剂分析平台
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-10 DOI: 10.1016/j.ijoes.2025.101229
Haijun Zhan
Sports drug testing is crucial for protecting athlete health and upholding the integrity of fair competition. While chromatography coupled with mass spectrometry (MS) remains the gold standard in world anti-doping agency (WADA) accredited laboratories, its logistical and economic constraints limit the scope and frequency of testing, creating a significant detection gap. This gap highlights an urgent need for analytical platforms that are rapid, cost-effective, and adaptable for high-throughput screening and on-site testing. This review critically examines capillary electrophoresis coupled with electrochemical detection (CE-EC) as a powerful and versatile platform poised to fill this specific need. This review posits that CE-EC's primary role is not to replace the confirmatory power of MS, but to act as a vital complementary technology. This review provides a comprehensive analysis of technological advances that have enhanced CE-EC performance, including nanomaterial-modified electrodes and molecularly imprinted polymers for superior sensitivity, miniaturization into lab-on-a-chip formats for high-throughput analysis, and advanced detection modalities such as pulsed amperometric detection and capacitively coupled contactless conductivity detection. Concurrently, this review addresses the core challenges that have hindered its adoption, including the debate over sensitivity relative to MS, matrix effects in biological samples, and the need for robust, validated methods. By presenting evidence from recent literature, this review delineates the specific contexts in which CE-EC is a viable platform. Finally, this review explores future directions, focusing on portable, on-site CE-EC devices that could revolutionize anti-doping strategies by shifting the paradigm from centralized detection to widespread, real-time deterrence.
体育药物检测对于保护运动员健康和维护公平竞争的完整性至关重要。虽然色谱联用质谱(MS)仍然是世界反兴奋剂机构(WADA)认可的实验室的金标准,但其后勤和经济限制了测试的范围和频率,造成了重大的检测差距。这一差距凸显了对快速、经济、适应高通量筛选和现场测试的分析平台的迫切需求。这篇综述严格审查毛细管电泳耦合电化学检测(CE-EC)作为一个强大的和通用的平台准备满足这一特定需求。本综述认为CE-EC的主要作用不是取代质谱的确认能力,而是作为一种重要的补充技术。这篇综述全面分析了提高CE-EC性能的技术进步,包括纳米材料修饰电极和分子印迹聚合物的高灵敏度,小型化到芯片实验室的高通量分析,以及先进的检测方式,如脉冲安培检测和电容耦合非接触式电导率检测。同时,这篇综述解决了阻碍其采用的核心挑战,包括相对于质谱的敏感性的争论,生物样品中的基质效应,以及对可靠的、经过验证的方法的需求。通过展示来自最近文献的证据,本综述描述了CE-EC是可行平台的具体背景。最后,本综述探讨了未来的发展方向,重点是便携式现场CE-EC设备,这些设备可以通过将范式从集中检测转变为广泛的实时威慑来彻底改变反兴奋剂策略。
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引用次数: 0
Investigation of the effect of chloride ions on the corrosion of DH36 steel in acidic solution 氯离子对DH36钢在酸性溶液中腐蚀影响的研究
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-10 DOI: 10.1016/j.ijoes.2025.101230
Jiantao Wang, Bochen Jiang
This study systematically investigates the corrosion behavior of DH36 steel under the combined influence of chloride (Cl⁻) and hydrogen (H⁺) ions, simulating marine splash zone environments. Electrochemical techniques—including potentiodynamic polarization measurements and electrochemical impedance spectroscopy (EIS)—coupled with microstructural analyses (SEM and EDS) were employed to evaluate corrosion mechanisms in NaCl solutions (1–7.5 wt%) and in acidic solutions containing 3.5 wt% NaCl with HCl concentrations ranging from 0 to 0.6 mol/L. Results reveal that with increasing Cl concentration, the corrosion potential decreases from − 519 mV to − 588 mV and the corrosion current density increases from 0.0137 mA/cm² to 0.0279 mA/cm², indicating accelerated corrosion rates. Notably, at > 5 wt% NaCl, pit density surges to 11,440 pits/mm² (7.5 wt%), while pit size expands by ∼ 80 %. In acidic Cl⁻-rich environments (HCl ≥ 0.4 mol/L), corrosion intensifies, and corrosion products become porous, facilitating longitudinal grooves and deep pits. EIS data confirm decreased polarization resistance (e.g., Rp drops from 4211 Ω·cm² to 2297 Ω·cm² in 7.5 wt% NaCl), and Warburg impedance emerges, signifying diffusion-controlled corrosion. The dominant mechanism involves electrochemical reactions where Cl⁻ and H⁺ act in concert to aggressively promote Fe dissolution via soluble complexes (e.g., [FeCl(OH)]⁻ad), while acidic conditions inhibit passivation. These findings highlight the critical vulnerability of DH36 steel in aggressive marine settings, providing essential insights for enhancing corrosion resistance in offshore structures.
本研究模拟海洋飞溅区环境,系统地研究了氯(Cl⁻)和氢(H⁺)离子对DH36钢的腐蚀行为。电化学技术——包括动电位极化测量和电化学阻抗谱(EIS)——结合微观结构分析(SEM和EDS),研究了NaCl溶液(1-7.5 wt%)和NaCl含量为3.5 wt%、HCl浓度为0 - 0.6 mol/L的酸性溶液中的腐蚀机理。结果表明,随着Cl−浓度的增加,腐蚀电位从−519 mV降低到−588 mV,腐蚀电流密度从0.0137 mA/cm²增加到0.0279 mA/cm²,腐蚀速率加快。值得注意的是,在>; 5 wt% NaCl下,坑密度激增至11,440个坑/mm²(7.5 wt%),而坑尺寸扩大了~ 80 %。在酸性Cl -富环境中(HCl≥0.4 mol/L),腐蚀加剧,腐蚀产物多孔,形成纵槽和深坑。EIS数据证实极化电阻降低(例如,在7.5% wt% NaCl中,Rp从4211 Ω·cm²降至2297 Ω·cm²),并且出现Warburg阻抗,表明扩散控制腐蚀。主要的机理涉及电化学反应,其中Cl -⁻和H +协同作用,通过可溶配合物(例如[FeCl(OH)]毒化)积极促进铁的溶解,而酸性条件抑制钝化。这些发现突出了DH36钢在恶劣海洋环境中的严重脆弱性,为提高海上结构的耐腐蚀性提供了重要见解。
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引用次数: 0
Barium titanate-modified carbon cloth for high-performance air-cathode microbial fuel cells 高性能空气阴极微生物燃料电池用钛酸钡改性碳布
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-07 DOI: 10.1016/j.ijoes.2025.101227
Yuvraj Maphrio Mao , Ramya K. , Somil Thakur , Rajnish Kaur Calay , Sanket Goel
In this study, an evaluation of textile-based cathodes and their surface modifications is conducted to enhance the performance of air-cathode MFCs. Among the tested materials, carbon cloth (CC) modified with Barium Titanate (BaTiO₃) demonstrated the highest power output of 9.81 µW/cm², outperforming both unmodified and other modified electrodes. Electrochemical characterization using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) confirmed improved electron transfer and reduced charge transfer resistance, while nitrogen adsorption–desorption (BET) analysis revealed a high surface area and mesoporous structure for BaTiO₃, correlating strongly with its enhanced electrochemical activity. Structural and compositional analyses via X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) validated successful perovskite modification. Electrolyte analysis revealed a neutral pH of 7.04 and a chemical oxygen demand (COD) of 1500 mg/L before operation, indicating a suitable environment for microbial activity and energy harvesting. Repeatability analysis over 10 operational cycles showed exceptional consistency with CC/BaTiO₃ achieving 89.97 % repeatability, and all CC-based electrodes maintaining over 45 % stability of the peak power obtained during a 3-hour operational run. Scanning electron microscopy (SEM) revealed favorable surface morphology supporting enhanced electrochemical activity. These results establish CC/BaTiO₃ as a robust and high-performing cathode material, offering significant potential for scalable, efficient, and reliable air-cathode MFC applications. The work ahead may focus on integrating CC/BaTiO3 as the electrode materials into miniaturized Air-Cathode MFCs for real-world and real-time energy harvesting applications.
在这项研究中,对纺织阴极及其表面改性进行了评估,以提高空气阴极mfc的性能。在测试的材料中,钛酸钡(BaTiO₃)改性的碳布(CC)的输出功率最高,为9.81 µW/cm²,优于未改性的和其他改性的电极。利用循环伏安法(CV)和电化学阻抗谱(EIS)的电化学表征证实了BaTiO₃提高了电子转移和降低了电荷转移电阻,而氮吸附-解吸(BET)分析表明,BaTiO₃具有高比表面积和介孔结构,这与它增强的电化学活性密切相关。通过x射线衍射(XRD)和x射线光电子能谱(XPS)的结构和成分分析验证了钙钛矿改性的成功。电解液分析显示,操作前的中性pH为7.04,化学需氧量(COD)为1500 mg/L,表明该环境适合微生物活动和能量收集。超过10个操作周期的重复性分析表明,CC/BaTiO₃具有出色的一致性,重复性达到89.97 %,并且所有CC基电极在3小时的操作运行中保持超过45 %的峰值功率稳定性。扫描电子显微镜(SEM)显示良好的表面形貌支持增强的电化学活性。这些结果确立了CC/BaTiO₃作为一种坚固耐用的高性能阴极材料,为可扩展,高效和可靠的空气阴极MFC应用提供了巨大的潜力。未来的工作重点可能是将CC/BaTiO3作为电极材料集成到小型化的空气阴极mfc中,用于现实世界和实时能量收集应用。
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引用次数: 0
Electrochemical determination of paclitaxel using a poly(3-nitro-L-tyrosine)/WC NPs modified gold electrode 聚(3-硝基- l -酪氨酸)/WC纳米粒子修饰金电极电化学测定紫杉醇
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-07 DOI: 10.1016/j.ijoes.2025.101223
Basima A.A. Saleem , Amer Th. Al-Taee , Salim A. Mohammed
Given critical therapeutic role and formulation challenges for paclitaxel, the accurate quantification of PAC in pharmaceutical products and biological samples is of great importance. In this study, we developed a novel electrochemical sensor by electropolymerizing 3-nitro tyrosine on a gold electrode, followed by modification with tungsten carbamide (WC) nanoparticles to enhance conductivity and surface area. Scanning electron microscopy confirmed a uniform nanostructured coating with high electroactive surface roughness. The fabricated P3NLT/WC/AuE sensor exhibited a distinct oxidation signal at −1.13 mV, which shifted positively upon interaction with PAC, indicating a selective recognition process between the polymeric layer and the drug. Using differential pulse voltammetry, the sensor displayed a broad linear dynamic range (1.33E-09 mol.L−1 to 5.42E-06 mol.L−1) and an ultra-low detection limit of 1.20E-11 mol.L−1. The applicability of the developed platform was validated through the determination of PAC in commercial injection formulations, achieving recovery rates between 99.01 % and 101.02 %. These results highlight the P3NLT /WC/AuE sensor as a promising, sensitive, and selective analytical tool for pharmaceutical quality control and therapeutic drug monitoring of paclitaxel in clinical practice.
鉴于紫杉醇的重要治疗作用和配方挑战,准确定量紫杉醇在药品和生物样品中的含量是非常重要的。在这项研究中,我们开发了一种新的电化学传感器,通过在金电极上电聚合3-硝基酪氨酸,然后用碳化钨(WC)纳米粒子修饰,以提高电导率和表面积。扫描电镜证实了具有高电活性表面粗糙度的均匀纳米结构涂层。制备的P3NLT/WC/AuE传感器在- 1.13 mV处表现出明显的氧化信号,与PAC相互作用后,氧化信号正向偏移,表明聚合物层与药物之间存在选择性识别过程。采用差分脉冲伏安法,该传感器具有较宽的线性动态范围(1.33E-09 mol.L−1 ~ 5.42E-06 mol.L−1),超低检出限为1.20E-11 mol.L−1。通过对商业注射剂配方中PAC的测定,验证了该平台的适用性,回收率在99.01 % ~ 101.02 %之间。这些结果表明,P3NLT /WC/AuE传感器在紫杉醇药物质量控制和治疗药物监测方面具有良好的应用前景和选择性。
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引用次数: 0
Electrodeposition of gradient Ni/SiO₂ nanocomposite coatings on St.37 steel: Microstructure, mechanical properties, and corrosion resistance St.37钢上梯度Ni/SiO 2纳米复合镀层的电沉积:显微组织、力学性能和耐蚀性
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-11-07 DOI: 10.1016/j.ijoes.2025.101226
P. Ashtari, T. Gholizadeh
This research focused on the possibility of fabricating a gradient Ni/SiO2 nanocomposite coating on a St. 37 substrate using the electrodeposition method from a Watts bath. The effects of applied current density and nanoparticle (NP) concentration on the coatings' composition, microstructure, microhardness, and corrosion resistance were investigated. GDS and EDS analyses were used to quantify the NP concentration and evaluate the NP dispersion in the coating, respectively. Response Surface Methodology (RSM) was employed via Design-Expert software for process optimization. Following the determination of optimized parameters, a gradient coating was successfully produced under three distinct deposition conditions. The microstructure of the coatings was studied using XRD, and the mechanical and electrochemical properties were evaluated through microhardness measurements and potentiodynamic polarization tests, respectively. Findings confirmed the successful production of a gradient coating, with SiO2 content precisely controlled from 0.69 wt% at the interface to a maximum of 3.49 wt% at the surface. The incorporation of SiO2 NPs induced significant grain refinement, reducing the average crystallite size from 138 nm to 90 nm. This microstructural modification resulted in a corresponding increase in microhardness to 359 Hv. The corrosion current density decreases by up to 8.9 times compared to low-nanoparticle content layers.
本研究的重点是在St. 37衬底上利用瓦特浴电沉积方法制备梯度Ni/SiO2纳米复合涂层的可能性。研究了外加电流密度和纳米粒子浓度对镀层组成、显微组织、显微硬度和耐蚀性的影响。利用GDS和EDS分析分别量化NP浓度和评价NP在涂层中的分散程度。通过Design-Expert软件,采用响应面法(RSM)进行工艺优化。在确定了优化参数后,在三种不同的沉积条件下成功地制备了梯度涂层。采用XRD研究了涂层的微观结构,并分别通过显微硬度测试和动电位极化测试对涂层的力学性能和电化学性能进行了评价。结果证实了梯度涂层的成功生产,SiO2含量精确控制在界面处的0.69 wt%到表面处的最大3.49 wt%。SiO2纳米颗粒的掺入导致晶粒细化,平均晶粒尺寸从138 nm减小到90 nm。这种显微组织的改变导致显微硬度相应提高到359 Hv。与低纳米颗粒含量层相比,腐蚀电流密度降低了8.9倍。
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International Journal of Electrochemical Science
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