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Preparation and electrochemical performance of Nb-doped LiFePO₄/C regenerated from spent Li-ion battery cathodes 废锂离子电池负极再生nb掺杂lifepo4 /C的制备及其电化学性能
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-11 DOI: 10.1016/j.ijoes.2025.101261
Yuan Tang, Yanshuai Zhao, Kaixiong Xiang
This study explores a method for the large-scale recycling and reuse of spent LiFePO4 from industry by synthesizing regenerated LiFePO4/C materials via a carbothermal reduction method using Nb-doped spent LiFePO4 as precursors. Among these regenerated materials, the 3 wt% Nb-doped sample exhibits a first discharge capacity of 140.2 mA h/g at 1 C. At 0.1 C, 2 C, and 5 C, the first discharge capacities are 162.6, 125.4, and 75.3 mA h/g, respectively. These experimental results demonstrate the excellent electrochemical performance of the 3 wt% Nb-doped sample. The regeneration method employed in this study, which offers convenient operation, easy preparation, and low cost, proves to be a viable approach for recycling spent cathodes and reusing them.
本研究以掺杂铌的废LiFePO4为前驱体,通过碳热还原法制备再生LiFePO4/C材料,探索工业废LiFePO4大规模回收再利用的方法。在这些再生材料中,3 wt% nb掺杂样品在1 ℃下的首次放电容量为140.2 mA h/g。在0.1 C、2 C和5 C条件下,第一次放电容量分别为162.6、125.4和75.3 mA h/g。这些实验结果证明了3 wt% nb掺杂样品具有优异的电化学性能。本研究采用的再生方法具有操作方便、制备简单、成本低等优点,是一种可行的废阴极回收再利用方法。
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引用次数: 0
Electrochemical properties and preparation of LiNi0.5Mn1.5O4 cathode material by high-energy ball milling for Li-Ion batteries 高能球磨法制备锂离子电池用LiNi0.5Mn1.5O4正极材料及其电化学性能
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-11 DOI: 10.1016/j.ijoes.2025.101268
Mao He , Huili Jiang , Bin Zhang , Jihua Chen , Liangwei Jiang
The ultrafine LiNi0.5Mn1.5O4 with excellent electrochemical performance is successfully synthesized using carbonate as precursor (NiCO3, MnCO3 and Li2CO3) by high-energy ball milling followed by double sintering method. The influence of different ball milling time and the powders synthesized by double sintering method on the phase composition, morphological characteristics and the electrochemical performance was studied. The results indicate that the LiNi0.5Mn1.5O4 powders by ball-mill for 10 h followed by sintering at 700℃ for 5 h shows the well-ordered high crystalline with mean size of the primary nanoparticles about 100 nm, and the discharge capacity is 123.3 mAh g−1 at 0.1 C rate. Further sintering at 900℃ for 1 h, the LiNi0.5Mn1.5O4 powders have a cubic spinel structure (Fd3m) with higher crystallinity and exhibit a narrow size distribution with the particle size around 600 nm, and the highest discharge capacity of 143.3mAh g−1 at 0.1 C rate, 96.7 % capacity retention after 50 cycles at 2 C rate, and the coulombic efficiency exceeding 98.5 %.
以碳酸盐为前驱体(NiCO3、MnCO3和Li2CO3),采用高能球磨-双烧结法制备了具有优异电化学性能的超细LiNi0.5Mn1.5O4。研究了不同球磨时间和双烧结法合成的粉末对其相组成、形貌特征和电化学性能的影响。结果表明:LiNi0.5Mn1.5O4粉体经球磨机烧结10 h,在700℃烧结5 h,得到了有序的高晶,初晶平均尺寸约为100 nm, 0.1 C速率下的放电容量为123.3 mAh g−1。在900℃下烧结1 h,制备的LiNi0.5Mn1.5O4粉末具有立方尖晶石结构(Fd3m),结晶度较高,粒径分布较细,粒径约为600 nm,在0.1 C速率下放电容量最高可达143.3mAh g−1,在2 C速率下循环50次后容量保持率为96.7 %,库仑效率超过98.5 %。
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引用次数: 0
Influence of surface oxide layer formed during hot rolling on the atmospheric corrosion resistance of 720 weathering steel 热轧过程中表面氧化层对720耐候钢耐大气腐蚀性能的影响
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-10 DOI: 10.1016/j.ijoes.2025.101269
Huan Wei , Mingqi Xiao , Huajie Zhu , Duoyao Liang , Yue Wang , Lin Liao , Huayun Du , Yinghui Wei
Weathering steel has potential use in solar photovoltaic brackets owing to its satisfactory atmospheric corrosion resistance and good mechanical properties. In this study, an exposure experiment was conducted in an industrial atmospheric environment. The corrosion weight gain, macro-morphology, micro-morphology, X-ray diffraction (XRD), Raman, and electrochemical characteristics of a new 720 weathering steel with and without a surface oxide layer and Q235 with a surface oxide layer formed during hot rolling were compared. The corrosion characteristics were identified, and the underlying mechanism of the effect of the surface oxide layer formed during hot rolling on corrosion resistance was analyzed. The experimental and analytical results show that the rusting coat on Q235O and WS is relatively loose with cracks, and the main component is γ-FeOOH, while the rust of WSO is dense, and stable α-FeOOH formed in the inner rust layer after exposure for 8 months. The Cu element is enriched in the rust layer, which hinders the diffusion of corrosive Cl ions into the substrate. The surface oxide layer formed during hot rolling accelerates the formation of a stabilized rust layer in weathering steel and significantly reduces its corrosion rate of weathering steel in atmospheric corrosion.
耐候钢具有良好的耐大气腐蚀性能和良好的力学性能,在太阳能光伏支架中具有潜在的应用前景。本研究在工业大气环境中进行了暴露实验。比较了具有和不具有表面氧化层的新型720耐候钢和具有热轧表面氧化层的Q235耐候钢的腐蚀增重、宏观形貌、微观形貌、x射线衍射(XRD)、拉曼光谱(Raman)和电化学特性。识别了腐蚀特征,分析了热轧过程中表面氧化层对耐蚀性影响的潜在机理。实验和分析结果表明:q2350和WS的锈蚀层相对疏松,有裂纹,主要成分为γ-FeOOH,而WSO的锈蚀致密,暴露8个月后,内部锈蚀层形成稳定的α-FeOOH。铜元素在锈层中富集,阻碍了腐蚀性Cl离子向基体扩散。热轧过程中形成的表面氧化层加速了耐候钢稳定锈层的形成,显著降低了耐候钢在大气腐蚀中的腐蚀速率。
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引用次数: 0
Electrocatalytic oxygen evolution on Ni-modified Sr@TiO₂ nanotubes in alkaline medium 碱性介质中ni修饰Sr@TiO₂纳米管的电催化析氧
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-10 DOI: 10.1016/j.ijoes.2025.101271
Inam Omar, Khadijah M. Emran
Among the most pressing problems in improving the technology of water electrolysis is the reduced speed of O2 evolution. Accordingly, there is a serious demand for more competent, robust, and economically sustainable catalysts for the oxygen evolution reaction (OER). In the current work, nickel (Ni) layers, as active electrochemical catalysts, were electrodeposited with various potentials on free-standing titanium dioxide nanotubes (TNT/Ni) and a strontium/titanium dioxide nanotube doped (Sr@TNT/Ni) on an Au electrode for the development of OER. TNTs and Sr@TNTs were examined utilizing SEM, EDS, XRD, and Raman spectroscopy. Cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and linear polarization (LP) responses have been used in potassium hydroxide solution to investigate the activity of TNTs, Sr@TNT, TNT/Ni, and Sr@TNT/Ni as catalysts. The reaction followed the Volmer-like mechanism. Among all the studied catalysts, the superior Au/Sr@TNT/Ni catalyst exhibited the highest oxygen evolution rate of 79.6 mA cm−2 at an applied potential of 900 mV, demonstrating considerable stability of the catalyst.
在改进水电解技术中最紧迫的问题是降低氧的析出速度。因此,对出氧反应(OER)的催化剂有更强的能力,强大的,经济上可持续的需求。在本工作中,镍(Ni)层作为活性电化学催化剂,以不同电位沉积在独立的二氧化钛纳米管(TNT/Ni)上,并在Au电极上掺杂锶/二氧化钛纳米管(Sr@TNT/Ni),用于OER的开发。利用SEM、EDS、XRD和拉曼光谱对tnt和Sr@TNTs进行了表征。利用循环伏安法(CV)、电化学阻抗谱法(EIS)和线性极化法(LP)在氢氧化钾溶液中考察了TNT、Sr@TNT、TNT/Ni和Sr@TNT/Ni作为催化剂的活性。反应遵循沃尔默式机制。在所有催化剂中,优异的Au/Sr@TNT/Ni催化剂在900 mV的应用电位下表现出最高的析氧速率,为79.6 mA cm−2,表现出较好的稳定性。
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引用次数: 0
Layer-by-layer assembled AuNP/γ-MnO₂–chitosan modified GCE for ultrasensitive detection of carcinoembryonic antigen 逐层组装AuNP/γ- mno2 -壳聚糖修饰的GCE用于癌胚抗原的超灵敏检测
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-09 DOI: 10.1016/j.ijoes.2025.101255
Lu Wang , Shanshan Mu , Lina Zhang, Na Wang, Lei Zhang, Yan Zhang, Xia Han
The sensitive detection of carcinoembryonic antigen (CEA), a critical tumor marker, is paramount for early-stage cancer diagnosis and management. This study reports the development of a novel, label-free electrochemical immunosensor based on a layer-by-layer (LbL) assembly of gold nanoparticles (AuNPs) and a gamma-phase manganese dioxide–chitosan (γ-MnO₂–CS) nanocomposite on a glassy carbon electrode (GCE). The engineered sensing interface leverages the synergistic properties of its constituents: the porous, high-surface-area γ-MnO₂–CS matrix provides an ideal scaffold for high-density antibody immobilization, while the integrated AuNPs create a highly conductive network that significantly amplifies the electrochemical signal. The immunosensor operates by measuring the impedance to electron transfer from a [Fe(CN)₆]³ ⁻/⁴⁻ redox probe, which is proportionally hindered by the binding of CEA to surface-immobilized antibodies. The platform demonstrated exceptional analytical performance, exhibiting an ultra-wide linear dynamic range spanning seven orders of magnitude from 10 fg mL−1 to 100 ng mL−1, with an extremely low limit of detection of 9.6 fg mL−1. Furthermore, the sensor showed excellent precision, with inter-day CVs below 9 % for mid- and high-range concentrations, and demonstrated high selectivity against common interferents. Its practical utility was confirmed in diluted human serum, achieving spike-recovery rates between 94.1 % and 104.6 %, validating its potential as a powerful and reliable tool for clinical applications.
癌胚抗原(CEA)是一种重要的肿瘤标志物,对早期癌症的诊断和治疗至关重要。本研究报道了一种新型无标记电化学免疫传感器的开发,该传感器基于在玻碳电极(GCE)上逐层组装金纳米粒子(AuNPs)和γ相二氧化锰-壳聚糖(γ-MnO₂-CS)纳米复合材料。设计的传感界面利用其成分的协同特性:多孔,高表面积的γ- mno2 -CS矩阵为高密度抗体固定提供了理想的支架,而集成的AuNPs创建了一个高导电性网络,显着放大了电化学信号。这种免疫传感器通过测量[Fe(CN)₆]³ 的电子传递阻抗来工作,因为CEA与表面固定抗体的结合成比例地阻碍了这种传递。该平台具有优异的分析性能,具有从10 fg mL−1到100 ng mL−1的超宽线性动态范围,检测限极低,为9.6 fg mL−1。此外,该传感器具有优异的精度,在中高浓度范围内的日间CVs低于9 %,并且对常见干扰具有高选择性。在稀释的人血清中证实了其实用性,峰值回收率在94.1 %和104.6 %之间,验证了其作为临床应用的强大可靠工具的潜力。
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引用次数: 0
Effect of composite additives in fine water mist on suppressing thermal runaway in lithium batteries 细水雾中复合添加剂对抑制锂电池热失控的影响
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-09 DOI: 10.1016/j.ijoes.2025.101270
Xu Qinkun, Xia Xin, Tian Tingting
To address the safety hazards of lithium battery fires, the limitations of low cooling efficiency of fine water mist fire-extinguishing technology, and the research gap regarding composite additives, this study conducted experiments on the suppression of lithium battery fires by fine water mist containing different additives based on a self-built experimental platform. The study used NCM ternary lithium batteries as the research object and triggered thermal runaway through external heating. The experimental results indicate that the higher the battery SOC (State of Charge), the earlier the thermal runaway is triggered, the higher the peak temperature, and the more intense the combustion phenomena. Under the action of fine water mist, the thermal runaway process of lithium batteries can be divided into four stages, but reignition phenomena still occurs. Each additive has an optimal mass fraction (0.15 % for FeCl2, 2.5 % for sodium lactate, and 0.3 % for both urea and Tween 20). Among them, FeCl2 and sodium lactate perform excellently in suppressing the temperature rise during thermal runaway, while urea and Tween 20 have more advantages in enhancing cooling performance. The composite additives demonstrate the best overall performance, especially the combinations of FeCl2 + Tween 20 and sodium lactate + Tween 20, which can reduce the maximum temperature to about 650℃ (an improvement of about 35 % in suppression effect compared with pure water mist) and effectively prevent reignition. This study provides theoretical support and technical references for the safety design, fire prevention, and emergency response of lithium batteries.
针对锂电池火灾的安全隐患、细水雾灭火技术冷却效率低的局限性以及复合添加剂的研究空白,本研究在自建实验平台上开展了含不同添加剂的细水雾对锂电池火灾的扑灭实验。本研究以NCM三元锂电池为研究对象,通过外部加热触发热失控。实验结果表明,电池荷电状态越高,引发热失控的时间越早,峰值温度越高,燃烧现象越强烈。在细水雾作用下,锂电池热失控过程可分为4个阶段,但仍会出现重燃现象。每种添加剂都有最佳质量分数(FeCl2为0.15 %,乳酸钠为2.5 %,尿素和Tween 20为0.3 %)。其中FeCl2和乳酸钠在抑制热失控过程中的温升方面表现优异,而尿素和Tween 20在提高冷却性能方面更有优势。复合添加剂综合性能最好,特别是FeCl2 + Tween 20和乳酸钠+ Tween 20的组合,可将最高温度降低至650℃左右(抑制效果比纯水雾提高约35 %),有效防止再燃。本研究为锂电池的安全设计、防火和应急响应提供理论支持和技术参考。
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引用次数: 0
Lithium nitrate/Lithium bis(oxalate)borate dual-salt in sulfolane as nonflammable electrolyte for stable lithium-metal batteries 亚砜中硝酸锂/双(草酸)硼酸锂双盐作为稳定锂金属电池的不燃电解质
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-08 DOI: 10.1016/j.ijoes.2025.101267
Chun-Jern Pan , Yi-Yu Chen , Shih-Che Lin , Bing-Joe Hwang , Chia-Hsin Wang , Chun-I. Lee
Lithium metal batteries have shown great potential in energy storage applications, and the development of novel electrolytes provide new opportunities to enhance their performance. This study proposes an innovative dual-lithium-salt electrolyte composed of lithium nitrate (LiNO3) and lithium bis(oxalato)borate (LiBOB) in sulfolane solvent. The electrolyte exhibits high Li plating/stripping reversibility and stability, effectively improving electrode interfacial compatibility. The introduction of LiBOB regulates the solvation structure, optimizes lithium-ion transport, and promotes the formation of a robust solid electrolyte interphase, which is crucial for interfacial stability and prolonged battery life. NMR spectra reveal that oxygen-rich groups in bis(oxalato)borate anion (BOB-) participate in Li+ solvation, increasing electron cloud density. This structural reorganization facilitates Li+ dissociation and further improves ionic conductivity. The electrolyte maintains stable Li plating/stripping voltage profiles with significantly lower polarization over long-term cycling in Li//Li cells, demonstrating smooth Li+ transport and stable interfaces that suppress dendrite growth and impedance rise. In Li//Cu cell, the electrolyte achieves an average coulombic efficiency of 97.85 %, showing high reversibility and stable interfacial behavior. Furthermore, in the Li//LiMn2O4 half-cell tests, the electrolyte demonstrated outstanding performance under various operating conditions. It achieved stable cycling for 680 cycles at 100 mA g−1 while maintaining an average coulombic efficiency of 99.2 % and a capacity retention of 84.54 %. Even at a high current rate of 500 mA g−1, the cell continued to operate stably for more than 260 cycles with a coulombic efficiency of approximately 99.2 %. Under elevated-temperature conditions of 60 °C, the electrolyte also exhibited excellent cycling stability and thermal tolerance. Overall, the novel electrolyte combines high ionic conductivity, superior thermal and electrochemical stability, and long cycling life, confirming its potential as a safe and high-performance electrolyte candidate for lithium metal batteries.
锂金属电池在储能应用中显示出巨大的潜力,新型电解质的开发为提高其性能提供了新的机遇。本研究提出了一种在亚砜溶剂中由硝酸锂(LiNO3)和硼酸锂(LiBOB)组成的新型双锂盐电解质。该电解质具有较高的镀/剥离锂的可逆性和稳定性,有效地改善了电极界面相容性。LiBOB的引入调节了溶剂化结构,优化了锂离子的输运,促进了坚固的固体电解质界面相的形成,这对界面稳定性和延长电池寿命至关重要。核磁共振谱显示,硼酸铋阴离子(BOB-)中的富氧基团参与Li+溶剂化,增加了电子云密度。这种结构重组有利于Li+解离,进一步提高离子电导率。电解质在Li//Li电池中长期循环时保持稳定的镀/剥离电压分布,极化显著降低,显示出Li+的平滑传输和稳定的界面,抑制枝晶生长和阻抗上升。在Li//Cu电池中,电解质的平均库仑效率为97.85 %,具有较高的可逆性和稳定的界面行为。此外,在Li//LiMn2O4半电池测试中,电解质在各种操作条件下都表现出优异的性能。在100 mA g−1下稳定循环680次,平均库仑效率为99.2% %,容量保持率为84.54 %。即使在500 mA g−1的高电流下,电池也能以约99.2% %的库仑效率持续稳定运行260多个循环。在60℃的高温条件下,电解质也表现出良好的循环稳定性和耐热性。总的来说,这种新型电解质结合了高离子电导率、优异的热稳定性和电化学稳定性以及长循环寿命,证实了其作为锂金属电池安全和高性能电解质候选材料的潜力。
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引用次数: 0
M-ZIF-67 (M = Cu, Ni, Fe, Zn) derived bimetallic porous polyhedrons for non-enzymatic amperometric glucose detection M- zif -67 (M = Cu, Ni, Fe, Zn)衍生双金属多孔多面体用于非酶安培葡萄糖检测
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-07 DOI: 10.1016/j.ijoes.2025.101266
Hui Yang, Xiaopeng Wang, Kongxiang Quan, Changchang Zhang, Zhiqiang Wei
Co in the lattice of ZIF-67 can be easily replaced by non-precious metal (Cu, Ni, Fe, Zn) to prepare non-precious metal (Cu, Ni, Fe, Zn) doped ZIF-67, which can be employed as excellent precursors to prepare bimetallic porous polyhedrons. In these bimetallic porous polyhedrons, hybrids containing carbon and nitrogen (C/N hybrids) are the basic framework, and bimetallic oxides are the key catalytic active centers. C/N hybrids possess good biocompatibility, bimetallic oxides own unique bimetallic synergistic catalytic effects, which jointly achieve the non-enzymatic electrochemical sensing for glucose. These bimetallic porous polyhedrons (Cu(2 %)&Co@PCN, Ni(1 %)&Co@PCN, Fe(1 %)&Co@PCN and Zn(1 %)&Co@PCN) not only reveal excellent performance for glucose amperometric detection, but also can be employed to detect glucose in the human serum samples, indicating that they have great commercial value for developing a new generation of non-enzymatic glucose electrochemical sensors.
ZIF-67晶格中的Co很容易被非贵金属(Cu、Ni、Fe、Zn)取代,制备出掺杂非贵金属(Cu、Ni、Fe、Zn)的ZIF-67,可以作为制备双金属多孔多面体的优良前驱体。在这些双金属多孔多面体中,碳氮杂化体(C/N杂化体)是基本骨架,双金属氧化物是关键的催化活性中心。C/N杂化物具有良好的生物相容性,双金属氧化物具有独特的双金属协同催化效应,共同实现了对葡萄糖的非酶电化学传感。这些双金属多孔多面体(Cu(2 %)&Co@PCN, Ni(1 %)&Co@PCN, Fe(1 %)&;Co@PCN和Zn(1 %)&Co@PCN)不仅在葡萄糖安培检测中表现出优异的性能,而且可以用于检测人血清样品中的葡萄糖,这表明它们在开发新一代非酶葡萄糖电化学传感器方面具有很大的商业价值。
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引用次数: 0
Electrochemical detection of diroximel fumarate using an α-cyclodextrin-based molecularly imprinted polymer sensor in human serum 基于α-环糊精的分子印迹聚合物传感器电化学检测人血清中富马酸二呋辛美尔
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-06 DOI: 10.1016/j.ijoes.2025.101265
Mahmoud Roushani , Zahra Mirzaei Karazan , Husam Jalil Abdulkahim
Diroximel fumarate (DRF) is a new oral fumarate applied in the treatment of multiple sclerosis (MS). The present work introduces a new method for the detection of DRF drugs through a molecularly imprinted polymer (MIP). The MIP was synthesized on the glassy carbon electrode (GCE) using the electropolymerization of monomer α‑cyclodextrin (α-CD) and the DRF template. In this sense, an electrochemical sensor incorporating a MIP was designed particularly to detect DRF for the first time. The modified GCE was investigated via differential pulse voltammetry (DPV), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and scanning electron microscopy (SEM). The designed sensor provided acceptable selectivity, reproducibility, repeatability, and stability. Additionally, the modified electrode showed a good linear response from 0.01 to 1300 nM with a low detection limit (LOD) of 0.0033 nM. The MIP/GCE was applied for DRF detection in a real sample with success. To find out the reliability of the proposed strategy, high performance liquid chromatography (HPLC) technique was employed to detect DRF in the real sample.
富马酸地洛昔梅尔(DRF)是一种用于治疗多发性硬化症(MS)的新型口服富马酸药物。本文介绍了一种利用分子印迹聚合物(MIP)检测DRF药物的新方法。采用单体α-环糊精(α- cd)和DRF模板电聚合的方法在玻璃碳电极(GCE)上合成了MIP。从这个意义上讲,首次设计了一种结合MIP的电化学传感器来检测DRF。采用差分脉冲伏安法(DPV)、电化学阻抗谱法(EIS)、循环伏安法(CV)和扫描电镜(SEM)对改性GCE进行了表征。所设计的传感器具有可接受的选择性、再现性、重复性和稳定性。此外,修饰电极在0.01 ~ 1300 nM范围内具有良好的线性响应,检出限(LOD)为0.0033 nM。将MIP/GCE应用于实际样品的DRF检测,取得了成功。为了验证该方法的可靠性,采用高效液相色谱(HPLC)技术对实际样品中的DRF进行了检测。
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引用次数: 0
Pt/flaky graphite–NiO composite electrocatalyst for the alkaline hydrogen evolution reaction Pt/片状石墨- nio复合电催化剂的碱性析氢反应
IF 2.4 4区 化学 Q4 ELECTROCHEMISTRY Pub Date : 2025-12-05 DOI: 10.1016/j.ijoes.2025.101262
Keqiang Ding , Xiaoxuan Liang , Ying Bai , Yiqing Chen , Jiawen Bao , Qian Zhao , Mengqing Niu , Wanting Shi , Hui Wang
<div><div>For the first time, a novel kind of alkaline hydrogen evolution reaction (HER) catalyst, namely, a flaky graphite (denoted as FG) and nickelous oxide (NiO) composite material supported platinum (Pt) catalyst (denoted as Pt/FG-NiO), is prepared via an air calcination-assisted hydrothermal method, in which the commercial graphite, one kind of nickel-containing substance (nickel acetate tetrahydrate (Ni(CH<sub>3</sub>COO)<sub>2</sub>·4 H<sub>2</sub>O) or nickel acetylacetonate (C<sub>10</sub>H<sub>14</sub>NiO<sub>4</sub>) or nickel oxalate dehydrate (NiC<sub>2</sub>O<sub>4</sub>·2 H<sub>2</sub>O)) and chloroplatinic acid hexahydrate (H<sub>2</sub>PtCl<sub>6</sub>·6 H<sub>2</sub>O) are utilized as the starting materials. In this work, firstly, three precursors are synthesized through calcining the mixture having the commercial graphite and one kind of nickel-containing substance in air at 550℃ for 1 h, namely, precursor p<sub>1</sub>, p<sub>2</sub> and p<sub>3</sub> are respectively prepared using Ni(CH<sub>3</sub>COO)<sub>2</sub>·4 H<sub>2</sub>O, C<sub>10</sub>H<sub>14</sub>NiO<sub>4</sub> and NiC<sub>2</sub>O<sub>4</sub>·2 H<sub>2</sub>O. Subsequently, the resulting precursor p<sub>1</sub>, p<sub>2</sub> and p<sub>3</sub> are subjected to the hydrothermal treatment in the presence of chloroplatinic acid solution, respectively, generating catalyst c<sub>1</sub>, c<sub>2</sub> and c<sub>3</sub>. As demonstrated by XRD and XPS results, graphite, NiO and metallic Pt are the major substances of all fabricated catalysts. More importantly, all prepared catalysts, especially catalyst c<sub>1</sub>, showed an excellent electrocatalytic activity towards alkaline HER. For example, the overpotential value to attain a HER current density of 10 mA cm<sup>−2</sup> on catalyst c<sub>1</sub> is as lower as 39.6 mV, being rather lower than that of catalyst c<sub>2</sub> (52.2 mV) and c<sub>3</sub> (57.2 mV). To be noted, the value of 39.6 mV for catalyst c<sub>1</sub> is very close to that of the commercial platinum/carbon (Pt/C) catalyst (37.9 mV). The Tafel slope values of catalyst c<sub>1</sub>, c<sub>2</sub>, c<sub>3</sub> and Pt/C for HER are about 41.3, 52.4, 59.0 and 49.5 mV dec<sup>−1</sup>, respectively. In the chronoamperometry (CA) test, the HER current density measured on catalyst c<sub>1</sub> is about 7.81 mA cm<sup>−2</sup> after 10 h, being much higher than that of catalyst c<sub>2</sub> (2.15 mA cm<sup>−2</sup>), c<sub>3</sub> (2.73 mA cm<sup>−2</sup>) and the commercial Pt/C (5.63 mA cm<sup>−2</sup>). After a thorough characterization, the greatly decreased R<sub>ct</sub> and the larger ECSA value are analyzed to be the main reasons giving catalyst c<sub>1</sub> an outstanding HER electrocatalytic activity. Showing the preparation of a novel HER catalyst of Pt/FG-NiO as well as its satisfied HER electrocatalytic performance are the main contributions of the present work, which is very beneficial to the development of Ni and Pt based alka
本文首次采用空气助烧水热法制备了一种新型碱性析氢反应(HER)催化剂,即片状石墨(FG)和氧化镍(NiO)复合材料负载铂(Pt)催化剂(Pt /FG-NiO)。以四水合乙酸镍(Ni(CH3COO)2·4 H2O)或乙酰丙酮镍(C10H14NiO4)或脱水草酸镍(NiC2O4·2 H2O)和六水合氯铂酸(H2PtCl6·6 H2O)为原料。本研究首先将商品石墨与一种含镍物质的混合物在550℃空气中煅烧1 h,合成了3种前驱体,分别用Ni(CH3COO)2·4 H2O、C10H14NiO4和NiC2O4·2 H2O制备前驱体p1、p2和p3。随后,将得到的前驱体p1、p2和p3分别在氯铂酸溶液存在下进行水热处理,生成催化剂c1、c2和c3。XRD和XPS结果表明,石墨、NiO和金属Pt是所有催化剂的主要成分。更重要的是,所有制备的催化剂,特别是c1催化剂,对碱性HER都表现出优异的电催化活性。例如,催化剂c1上达到HER电流密度为10 mA cm−2的过电位值低至39.6 mV,远低于催化剂c2(52.2 mV)和c3(57.2 mV)。值得注意的是,催化剂c1的39.6 mV与商业铂/碳(Pt/C)催化剂(37.9 mV)的值非常接近。催化剂c1、c2、c3和Pt/C对HER的Tafel斜率分别约为41.3、52.4、59.0和49.5 mV dec−1。计时电流法(CA)测试,她的电流密度测量催化剂c1是关于7.81马  厘米−2 10 h后,比这更高的催化剂c2(2.15马  厘米−2),c3(2.73马  厘米−2)和商业Pt / C(5.63马  厘米−2)。经过深入的表征,分析了Rct的大幅降低和ECSA值的增大是c1催化剂具有优异HER电催化活性的主要原因。本文的主要贡献是制备了一种新型的Pt/FG-NiO she催化剂,并取得了令人满意的HER电催化性能,这对Ni和Pt基碱性HER催化剂的发展是非常有益的。
{"title":"Pt/flaky graphite–NiO composite electrocatalyst for the alkaline hydrogen evolution reaction","authors":"Keqiang Ding ,&nbsp;Xiaoxuan Liang ,&nbsp;Ying Bai ,&nbsp;Yiqing Chen ,&nbsp;Jiawen Bao ,&nbsp;Qian Zhao ,&nbsp;Mengqing Niu ,&nbsp;Wanting Shi ,&nbsp;Hui Wang","doi":"10.1016/j.ijoes.2025.101262","DOIUrl":"10.1016/j.ijoes.2025.101262","url":null,"abstract":"&lt;div&gt;&lt;div&gt;For the first time, a novel kind of alkaline hydrogen evolution reaction (HER) catalyst, namely, a flaky graphite (denoted as FG) and nickelous oxide (NiO) composite material supported platinum (Pt) catalyst (denoted as Pt/FG-NiO), is prepared via an air calcination-assisted hydrothermal method, in which the commercial graphite, one kind of nickel-containing substance (nickel acetate tetrahydrate (Ni(CH&lt;sub&gt;3&lt;/sub&gt;COO)&lt;sub&gt;2&lt;/sub&gt;·4 H&lt;sub&gt;2&lt;/sub&gt;O) or nickel acetylacetonate (C&lt;sub&gt;10&lt;/sub&gt;H&lt;sub&gt;14&lt;/sub&gt;NiO&lt;sub&gt;4&lt;/sub&gt;) or nickel oxalate dehydrate (NiC&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;4&lt;/sub&gt;·2 H&lt;sub&gt;2&lt;/sub&gt;O)) and chloroplatinic acid hexahydrate (H&lt;sub&gt;2&lt;/sub&gt;PtCl&lt;sub&gt;6&lt;/sub&gt;·6 H&lt;sub&gt;2&lt;/sub&gt;O) are utilized as the starting materials. In this work, firstly, three precursors are synthesized through calcining the mixture having the commercial graphite and one kind of nickel-containing substance in air at 550℃ for 1 h, namely, precursor p&lt;sub&gt;1&lt;/sub&gt;, p&lt;sub&gt;2&lt;/sub&gt; and p&lt;sub&gt;3&lt;/sub&gt; are respectively prepared using Ni(CH&lt;sub&gt;3&lt;/sub&gt;COO)&lt;sub&gt;2&lt;/sub&gt;·4 H&lt;sub&gt;2&lt;/sub&gt;O, C&lt;sub&gt;10&lt;/sub&gt;H&lt;sub&gt;14&lt;/sub&gt;NiO&lt;sub&gt;4&lt;/sub&gt; and NiC&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;4&lt;/sub&gt;·2 H&lt;sub&gt;2&lt;/sub&gt;O. Subsequently, the resulting precursor p&lt;sub&gt;1&lt;/sub&gt;, p&lt;sub&gt;2&lt;/sub&gt; and p&lt;sub&gt;3&lt;/sub&gt; are subjected to the hydrothermal treatment in the presence of chloroplatinic acid solution, respectively, generating catalyst c&lt;sub&gt;1&lt;/sub&gt;, c&lt;sub&gt;2&lt;/sub&gt; and c&lt;sub&gt;3&lt;/sub&gt;. As demonstrated by XRD and XPS results, graphite, NiO and metallic Pt are the major substances of all fabricated catalysts. More importantly, all prepared catalysts, especially catalyst c&lt;sub&gt;1&lt;/sub&gt;, showed an excellent electrocatalytic activity towards alkaline HER. For example, the overpotential value to attain a HER current density of 10 mA cm&lt;sup&gt;−2&lt;/sup&gt; on catalyst c&lt;sub&gt;1&lt;/sub&gt; is as lower as 39.6 mV, being rather lower than that of catalyst c&lt;sub&gt;2&lt;/sub&gt; (52.2 mV) and c&lt;sub&gt;3&lt;/sub&gt; (57.2 mV). To be noted, the value of 39.6 mV for catalyst c&lt;sub&gt;1&lt;/sub&gt; is very close to that of the commercial platinum/carbon (Pt/C) catalyst (37.9 mV). The Tafel slope values of catalyst c&lt;sub&gt;1&lt;/sub&gt;, c&lt;sub&gt;2&lt;/sub&gt;, c&lt;sub&gt;3&lt;/sub&gt; and Pt/C for HER are about 41.3, 52.4, 59.0 and 49.5 mV dec&lt;sup&gt;−1&lt;/sup&gt;, respectively. In the chronoamperometry (CA) test, the HER current density measured on catalyst c&lt;sub&gt;1&lt;/sub&gt; is about 7.81 mA cm&lt;sup&gt;−2&lt;/sup&gt; after 10 h, being much higher than that of catalyst c&lt;sub&gt;2&lt;/sub&gt; (2.15 mA cm&lt;sup&gt;−2&lt;/sup&gt;), c&lt;sub&gt;3&lt;/sub&gt; (2.73 mA cm&lt;sup&gt;−2&lt;/sup&gt;) and the commercial Pt/C (5.63 mA cm&lt;sup&gt;−2&lt;/sup&gt;). After a thorough characterization, the greatly decreased R&lt;sub&gt;ct&lt;/sub&gt; and the larger ECSA value are analyzed to be the main reasons giving catalyst c&lt;sub&gt;1&lt;/sub&gt; an outstanding HER electrocatalytic activity. Showing the preparation of a novel HER catalyst of Pt/FG-NiO as well as its satisfied HER electrocatalytic performance are the main contributions of the present work, which is very beneficial to the development of Ni and Pt based alka","PeriodicalId":13872,"journal":{"name":"International Journal of Electrochemical Science","volume":"21 1","pages":"Article 101262"},"PeriodicalIF":2.4,"publicationDate":"2025-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145786960","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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International Journal of Electrochemical Science
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