Pub Date : 2024-07-09DOI: 10.1149/1945-7111/ad60f9
Marwa Marwa, Mohammad aboelhamd, R. H. Obaydo, Dania Nashed, C. Nessim
This study presents a sustainable electrochemical investigation of pramipexole (PRA) in pharmaceuticals and human plasma, using cyclic and differential pulse voltammetry. Key parameters, including potential range, buffer pH, accumulation period, and scan rate were optimized, establishing efficient voltammetric methods for PRA analysis. The analytical range was 0.60 – 12.00 μg/mL, with a detection limit of 0.14 μg/mL and a correlation coefficient of 0.9998. Recovery rates for PRA ranged from 98.60 ± 0.26% to 101.33 ± 0.38%, validating the methodology's applicability in human plasma with an average recovery of 99.25 ± 0.45%. The study highlights the environmental sustainability of the developed voltammetric electrode, evaluated through SWOT analysis, and assesses the greennees impact using tools like Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical greenness (AGREE) and Analytical greenness for sample preparation (AGREEprep). Significantly, this work aligns with numerous United Nations Sustainable Development Goals (UN-SDGs), specifically goals 3, 4, 5, 7, 9, 11, 12, 13, 14, 15, and 17, illustrating our commitment to sustainable pharmaceutical research. The sustainability of the method was further quantified using the newly introduced Need, Quality, Sustainability (NQS) index, demonstrating significant alignment with sustainable analytical practices.
{"title":"Bridging Pharma and Sustainability: Green Electrochemical Analysis of Antiparkinsonian Drug in Pharmaceuticals and Plasma, Aligned with United Nations Goals via the NQS Index","authors":"Marwa Marwa, Mohammad aboelhamd, R. H. Obaydo, Dania Nashed, C. Nessim","doi":"10.1149/1945-7111/ad60f9","DOIUrl":"https://doi.org/10.1149/1945-7111/ad60f9","url":null,"abstract":"\u0000 This study presents a sustainable electrochemical investigation of pramipexole (PRA) in pharmaceuticals and human plasma, using cyclic and differential pulse voltammetry. Key parameters, including potential range, buffer pH, accumulation period, and scan rate were optimized, establishing efficient voltammetric methods for PRA analysis. The analytical range was 0.60 – 12.00 μg/mL, with a detection limit of 0.14 μg/mL and a correlation coefficient of 0.9998. Recovery rates for PRA ranged from 98.60 ± 0.26% to 101.33 ± 0.38%, validating the methodology's applicability in human plasma with an average recovery of 99.25 ± 0.45%. The study highlights the environmental sustainability of the developed voltammetric electrode, evaluated through SWOT analysis, and assesses the greennees impact using tools like Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical greenness (AGREE) and Analytical greenness for sample preparation (AGREEprep). Significantly, this work aligns with numerous United Nations Sustainable Development Goals (UN-SDGs), specifically goals 3, 4, 5, 7, 9, 11, 12, 13, 14, 15, and 17, illustrating our commitment to sustainable pharmaceutical research. The sustainability of the method was further quantified using the newly introduced Need, Quality, Sustainability (NQS) index, demonstrating significant alignment with sustainable analytical practices.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141663859","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}
Pub Date : 2024-07-09DOI: 10.1149/1945-7111/ad6074
Mohammad Taghi Tourchi Moghadam, Karolina Cysewska
This study explores the influence of deposition charge during fabrication of poly(3,4-ethylenedioxythiophene) doped with polystyrene sulfonate (PEDOT:PSS) on its electrical interface parameters. For this purpose, PEDOT:PSS was fabricated under state-of-the-art conditions desirable for neural bioelectrodes on commercial platinum electrodes with the electrodeposition time limited by different charges (1, 3, 6, 9 mC). Further, the electrodes were characterized regarding their electrical interface such as interfacial impedance, potential window, double-layer capacitance, charge storage capacity, and current injection limit under simulated body conditions. The work showed whether and to what extent the change of deposition charge affected the electrical interface parameters of PEDOT:PSS-based platinum electrodes. The electrodes polymerized with 9 mC exhibited a significant increase in specific capacitance, indicating enhanced charge storage capacity. Additionally, this sample demonstrated lower resistance in phosphate-buffered saline, suggesting improved conductivity.
本研究探讨了掺杂聚苯乙烯磺酸盐的聚（3,4-亚乙二氧基噻吩）（PEDOT:PSS）在制造过程中沉积电荷对其电学界面参数的影响。为此，PEDOT:PSS 是在最先进的神经生物电极制造条件下在商用铂电极上制造的，电沉积时间受不同电荷（1、3、6、9 mC）的限制。此外，还对电极的电界面进行了表征，如界面阻抗、电位窗口、双层电容、电荷存储容量以及模拟人体条件下的电流注入极限。研究结果表明了沉积电荷的变化是否以及在多大程度上影响了基于 PEDOT:PSS 的铂电极的电界面参数。聚合度为 9 mC 的电极的比电容显著增加，表明电荷存储能力增强。此外，该样品在磷酸盐缓冲盐水中的电阻较低，表明其导电性有所提高。
{"title":"Electrical Interface Parameters of PEDOT:PSS: Effect of Electrodeposition Charge Evaluated Under Body Conditions for Neural Electrode Applications","authors":"Mohammad Taghi Tourchi Moghadam, Karolina Cysewska","doi":"10.1149/1945-7111/ad6074","DOIUrl":"https://doi.org/10.1149/1945-7111/ad6074","url":null,"abstract":"\u0000 This study explores the influence of deposition charge during fabrication of poly(3,4-ethylenedioxythiophene) doped with polystyrene sulfonate (PEDOT:PSS) on its electrical interface parameters. For this purpose, PEDOT:PSS was fabricated under state-of-the-art conditions desirable for neural bioelectrodes on commercial platinum electrodes with the electrodeposition time limited by different charges (1, 3, 6, 9 mC). Further, the electrodes were characterized regarding their electrical interface such as interfacial impedance, potential window, double-layer capacitance, charge storage capacity, and current injection limit under simulated body conditions. The work showed whether and to what extent the change of deposition charge affected the electrical interface parameters of PEDOT:PSS-based platinum electrodes. The electrodes polymerized with 9 mC exhibited a significant increase in specific capacitance, indicating enhanced charge storage capacity. Additionally, this sample demonstrated lower resistance in phosphate-buffered saline, suggesting improved conductivity.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141663370","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}
Pub Date : 2024-07-08DOI: 10.1149/1945-7111/ad6037
Ho Lun Chan, E. Romanovskaia, Sean Mills, Minsung Hong, V. Romanovski, Nathan Bieberdorf, Chaitanya Peddeti, Andy Minor, Peter Hosemann, Mark Asta, John R. Scully
In this work, the dealloying corrosion behavior of the FCC Ni20Cr (wt.%) in molten LiF-NaF-KF (FLiNaK) salts at 600 °C under varying applied potentials was investigated. Using in-operando electrochemical techniques and a multi-modal suite of characterization methods, we connect electrochemical potential, thermodynamic stability, and electro-dissolution kinetics to the corrosion morphologies. Notably, under certain potential regimes, a micro-scale bicontinuous structure, characterized by a network of interconnected ligaments and pores with the composition of the more noble (MN) element, becomes prominent. At other potentials both MN and less noble (LN) elements dealloy but at different rates. The dealloying process consists of bulk and grain boundary diffusion of Cr to the metal/salt interface, interphase Cr oxidation, accompanied by surface diffusion of Ni to interconnected ligaments. This process is predominately controlled by charge transfer, resulting in the formation of Cr(II) and Cr(III) species at a constant rate of attack for a period of 10,000 seconds. At higher potentials, the bicontinuous porous structure undergoes further surface coarsening. Concurrently, Cr(II), Cr(III), and Ni(II) begin to dissolve, with the dissolution of Ni occurring at a significantly slower rate. When solid state transport of Cr is exceeded by the interfacial rates, dealloying depths are limited.
{"title":"Morphological Evolution and Dealloying During Corrosion of Ni20Cr in Molten FLiNaK Salt","authors":"Ho Lun Chan, E. Romanovskaia, Sean Mills, Minsung Hong, V. Romanovski, Nathan Bieberdorf, Chaitanya Peddeti, Andy Minor, Peter Hosemann, Mark Asta, John R. Scully","doi":"10.1149/1945-7111/ad6037","DOIUrl":"https://doi.org/10.1149/1945-7111/ad6037","url":null,"abstract":"\u0000 In this work, the dealloying corrosion behavior of the FCC Ni20Cr (wt.%) in molten LiF-NaF-KF (FLiNaK) salts at 600 °C under varying applied potentials was investigated. Using in-operando electrochemical techniques and a multi-modal suite of characterization methods, we connect electrochemical potential, thermodynamic stability, and electro-dissolution kinetics to the corrosion morphologies. Notably, under certain potential regimes, a micro-scale bicontinuous structure, characterized by a network of interconnected ligaments and pores with the composition of the more noble (MN) element, becomes prominent. At other potentials both MN and less noble (LN) elements dealloy but at different rates. The dealloying process consists of bulk and grain boundary diffusion of Cr to the metal/salt interface, interphase Cr oxidation, accompanied by surface diffusion of Ni to interconnected ligaments. This process is predominately controlled by charge transfer, resulting in the formation of Cr(II) and Cr(III) species at a constant rate of attack for a period of 10,000 seconds. At higher potentials, the bicontinuous porous structure undergoes further surface coarsening. Concurrently, Cr(II), Cr(III), and Ni(II) begin to dissolve, with the dissolution of Ni occurring at a significantly slower rate. When solid state transport of Cr is exceeded by the interfacial rates, dealloying depths are limited.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141667729","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}
Pub Date : 2024-07-08DOI: 10.1149/1945-7111/ad603b
Shanxin Xiong, Juan Wu, Min Chen, Kerui Zhang, Ke Fang, Yukun Zhang, Xiaoqin Wang, Chunxia Hua, Jia Chu, Runlan Zhang, Chenxu Wang, Ming Gong, Hong Wang, Bohua Wu
The stacking between layers of a two-dimensional covalent organic framework (COF) leads to overlapping π orbitals, which enables charge carriers to be transported quickly through these pre-designed π orbitals. The two-dimensional COF featuring donor-acceptor interactions represents a straightforward approach for fabricating a high-performance organic electrochromic device. In this paper, N, N, N', N'-tetrad(4-aminophenyl)-1,4-phenylenediamine (TPDA) with electron-rich structure and 2,2'-bipyridine-5,5'-dialdehyde (BPDA) with strong electron absorption ability were used as the construction unit. COFTPDA-BPDA electrochromic materials with donor-acceptor structure were synthesized by Schiff base reaction, which can achieve reversible switching from red to dark gray. The color/fade time of the film at 474 nm wavelength is 6.8 s/11.9 s. The contrast retention rate of the film can reach 97.6% after 20 potential cycles, the memory time is as long as 4278 s. The present study demonstrates that constructing a donor-acceptor (D-A) structural unit with conjugated triphenylamine as the electron donor linked to bipyridine electron-withdrawing groups enhances charge transfer and redox reactions. With the success of this design strategy, the construction of the D-A structure is an important methodology for improving the electrochromic properties of materials.
{"title":"Construction and Electrochromic Properties of Two-Dimensional Covalent Organic Frameworks with Donor-Acceptor Structures of Triphenylamine and Bipyridine","authors":"Shanxin Xiong, Juan Wu, Min Chen, Kerui Zhang, Ke Fang, Yukun Zhang, Xiaoqin Wang, Chunxia Hua, Jia Chu, Runlan Zhang, Chenxu Wang, Ming Gong, Hong Wang, Bohua Wu","doi":"10.1149/1945-7111/ad603b","DOIUrl":"https://doi.org/10.1149/1945-7111/ad603b","url":null,"abstract":"\u0000 The stacking between layers of a two-dimensional covalent organic framework (COF) leads to overlapping π orbitals, which enables charge carriers to be transported quickly through these pre-designed π orbitals. The two-dimensional COF featuring donor-acceptor interactions represents a straightforward approach for fabricating a high-performance organic electrochromic device. In this paper, N, N, N', N'-tetrad(4-aminophenyl)-1,4-phenylenediamine (TPDA) with electron-rich structure and 2,2'-bipyridine-5,5'-dialdehyde (BPDA) with strong electron absorption ability were used as the construction unit. COFTPDA-BPDA electrochromic materials with donor-acceptor structure were synthesized by Schiff base reaction, which can achieve reversible switching from red to dark gray. The color/fade time of the film at 474 nm wavelength is 6.8 s/11.9 s. The contrast retention rate of the film can reach 97.6% after 20 potential cycles, the memory time is as long as 4278 s. The present study demonstrates that constructing a donor-acceptor (D-A) structural unit with conjugated triphenylamine as the electron donor linked to bipyridine electron-withdrawing groups enhances charge transfer and redox reactions. With the success of this design strategy, the construction of the D-A structure is an important methodology for improving the electrochromic properties of materials.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141669136","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}
Pub Date : 2024-07-08DOI: 10.1149/1945-7111/ad6038
Afsana Khan, Sonia Bansal
Flexible humidity sensors play a critical role in medical diagnostics and industrial control systems. In this study, a low-cost flexible humidity sensor is presented. The humidity sensor is developed by printing silver interdigitated electrodes (IDE) on a polyethylene terephthalate (PET) substrate using an Epson Stylus C88+ inkjet printer. The sensing layer of the humidity sensor was fabricated using graphene oxide (GO) ink, which is deposited onto the electrodes using an aerosol deposition technique. The GO humidity sensor achieves excellent sensing performance over a wide range of humidity levels from 11% to 97% RH range, with a fast response time of 2 seconds and recovery time of 17 seconds. The sensor also exhibits ultra-high sensitivity (243 kΩ/%RH), low hysteresis (2.16%), excellent repeatability, long-term stability, and high flexibility (tested at bending radiuses of 4 cm, 3.5 cm, 3 cm, and 2.5 cm). The humidity sensing mechanism of the proposed GO humidity sensor was also discussed. Furthermore, the sensor exhibited excellent capabilities in monitoring human respiration, distinguishing between nose and mouth breathing, detecting finger movements without physical contact, and even recognising basic spoken words. These features of the sensor possess significant potential for various applications in human healthcare.
{"title":"Low-Cost Flexible Graphene Oxide Humidity Sensor Fabricated Using Inkjet Printing and Aerosol Deposition","authors":"Afsana Khan, Sonia Bansal","doi":"10.1149/1945-7111/ad6038","DOIUrl":"https://doi.org/10.1149/1945-7111/ad6038","url":null,"abstract":"\u0000 Flexible humidity sensors play a critical role in medical diagnostics and industrial control systems. In this study, a low-cost flexible humidity sensor is presented. The humidity sensor is developed by printing silver interdigitated electrodes (IDE) on a polyethylene terephthalate (PET) substrate using an Epson Stylus C88+ inkjet printer. The sensing layer of the humidity sensor was fabricated using graphene oxide (GO) ink, which is deposited onto the electrodes using an aerosol deposition technique. The GO humidity sensor achieves excellent sensing performance over a wide range of humidity levels from 11% to 97% RH range, with a fast response time of 2 seconds and recovery time of 17 seconds. The sensor also exhibits ultra-high sensitivity (243 kΩ/%RH), low hysteresis (2.16%), excellent repeatability, long-term stability, and high flexibility (tested at bending radiuses of 4 cm, 3.5 cm, 3 cm, and 2.5 cm). The humidity sensing mechanism of the proposed GO humidity sensor was also discussed. Furthermore, the sensor exhibited excellent capabilities in monitoring human respiration, distinguishing between nose and mouth breathing, detecting finger movements without physical contact, and even recognising basic spoken words. These features of the sensor possess significant potential for various applications in human healthcare.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141667607","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}
Electroless plating is a commonly used method to enhance the corrosion resistance, wear resistance, and decorative performance of aluminum alloys. However, in electroless plating processes, it is customary to maintain the solution temperature at levels exceeding 85°C, a critical condition that ensures a sufficiently rapid deposition rate and thereby fosters the formation of high-performance coatings. Conventional immersion pretreatments with zinc and palladium result in lower deposition rates at low temperatures. This study shows that a copper immersion layer with microporous channels can facilitate the electroless plating process for aluminum alloys at lower temperatures. Through a redox reaction in a Cu2+-containing solution at 70°C, a copper immersion layer with a microporous structure could be created on an aluminum alloy. The microporous channels between the copper immersion layer and the aluminum alloy create electrochemical corrosion cells in the plating solution, accelerating the electroless plating process. The Ni-P coating obtained after pretreatment by copper immersion has a higher hardness (578 HV) and a lower corrosion current density (0.55 μA/cm2). This work provides a practical method to rapidly fabricate high-performance Ni-P coatings at intermediate temperatures (70-75°C).
{"title":"A Microporous Channel Copper Immersion Layer Promotes the Rapid Ni-P Electroless Plating Process on Aluminum Alloys at Medium and Low Temperatures","authors":"Dongdong Zhu, Qinghui Wang, Jiale Sun, Liying Wang, Xijia Yang, Xuesong Li","doi":"10.1149/1945-7111/ad6039","DOIUrl":"https://doi.org/10.1149/1945-7111/ad6039","url":null,"abstract":"\u0000 Electroless plating is a commonly used method to enhance the corrosion resistance, wear resistance, and decorative performance of aluminum alloys. However, in electroless plating processes, it is customary to maintain the solution temperature at levels exceeding 85°C, a critical condition that ensures a sufficiently rapid deposition rate and thereby fosters the formation of high-performance coatings. Conventional immersion pretreatments with zinc and palladium result in lower deposition rates at low temperatures. This study shows that a copper immersion layer with microporous channels can facilitate the electroless plating process for aluminum alloys at lower temperatures. Through a redox reaction in a Cu2+-containing solution at 70°C, a copper immersion layer with a microporous structure could be created on an aluminum alloy. The microporous channels between the copper immersion layer and the aluminum alloy create electrochemical corrosion cells in the plating solution, accelerating the electroless plating process. The Ni-P coating obtained after pretreatment by copper immersion has a higher hardness (578 HV) and a lower corrosion current density (0.55 μA/cm2). This work provides a practical method to rapidly fabricate high-performance Ni-P coatings at intermediate temperatures (70-75°C).","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141667817","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}
Pub Date : 2024-07-08DOI: 10.1149/1945-7111/ad603c
S. Tao, Fengqi Zhang, Jianping Peng, Ruiting Ma, Wu Zhang
Selective and efficient electrochemical analytical methods for the depositing process of metal aluminum are significant and necessary. The electrochemical measurement methods are based on the means of cyclic voltammetry, square wave voltammetry and constant potential electrolysis. The above methods are even never used to analyze the depositing process of metal aluminum in NaF-NaCl-Al2O3 and NaF-NaCl-NaAlO2 molten salt. Cyclic voltammetry analysis showed that Al3+ ions were reduced to metal aluminum through two consecutive steps. From the analysis of square wave voltammetry curve, the main reaction on the electrode was the reduction of metal sodium in the NaF-NaCl system, and the electron transfer number of the reaction was 0.80. With the addition of NaAlO2 and Al2O3 in the electrolyte, the electron transfer numbers of the two reduction steps were about 3.0. The process of reduction of Al3+ ions to aluminum was further proved by the analysis of the electrolysis curve at constant potential. The diffusion rate of Al3+ions and the rate of Al3+ reduction reaction increased with the addition of NaAlO2 and Al2O3 and the change of the potential.
{"title":"Cathode Electrochemical Behavior of Aluminum Electrolysis in NaF-NaCl Based Molten Salt","authors":"S. Tao, Fengqi Zhang, Jianping Peng, Ruiting Ma, Wu Zhang","doi":"10.1149/1945-7111/ad603c","DOIUrl":"https://doi.org/10.1149/1945-7111/ad603c","url":null,"abstract":"\u0000 Selective and efficient electrochemical analytical methods for the depositing process of metal aluminum are significant and necessary. The electrochemical measurement methods are based on the means of cyclic voltammetry, square wave voltammetry and constant potential electrolysis. The above methods are even never used to analyze the depositing process of metal aluminum in NaF-NaCl-Al2O3 and NaF-NaCl-NaAlO2 molten salt. Cyclic voltammetry analysis showed that Al3+ ions were reduced to metal aluminum through two consecutive steps. From the analysis of square wave voltammetry curve, the main reaction on the electrode was the reduction of metal sodium in the NaF-NaCl system, and the electron transfer number of the reaction was 0.80. With the addition of NaAlO2 and Al2O3 in the electrolyte, the electron transfer numbers of the two reduction steps were about 3.0. The process of reduction of Al3+ ions to aluminum was further proved by the analysis of the electrolysis curve at constant potential. The diffusion rate of Al3+ions and the rate of Al3+ reduction reaction increased with the addition of NaAlO2 and Al2O3 and the change of the potential.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141669753","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}
Pub Date : 2024-07-04DOI: 10.1149/1945-7111/ad5f21
Elahe Moazzen, J. Mujtaba, Bruce Buchholz, Dieter Isheim, Norman Luu, David Rowell, Xiaobing Hu, Trung Ha, M. Hersam, Scott A Barnett
Atom probe tomography (APT) can yield three-dimensional tomographic images at atomic-scale resolution and low-AMU elements such as Li are readily observed, making it a powerful tool for exploring battery materials interfaces. However, it is difficult to prepare APT specimen tips containing the interface of interest starting with typical particle-based battery electrodes. Here we demonstrate a methodology for reliable APT imaging of battery interfaces in which a thin film electrode geometry is used to provide well-controlled planar interfaces that are ideal for APT sample preparation and imaging. LiFePO4 (LFP) thin film electrodes, synthesized using pulsed laser deposition (PLD), were studied as an example system, with standard Li-salt electrolytes. For the results to be applicable to conventional particulate electrodes, it is important to obtain representative thin film structure and electrochemical characteristics. Thus, the effects of PLD conditions including substrate temperature, substrate crystallinity, target composition, and deposition time (number of laser pulses) on the thin film's crystallographic texture, morphology, and electrochemical performance were studied. Optimized LFP film showed good crystallinity with low-C-rate capacity of ~ 90 mAh g-1. Initial APT three-dimensional imaging of the LFP/electrolyte interface shows an ~ 10 nm cathode-electrolyte interphase layer that is enriched in F and Li.
原子探针层析成像（APT）可以产生原子级分辨率的三维层析成像，而且很容易观察到锂等低AMU元素，因此是探索电池材料界面的有力工具。然而，从典型的颗粒型电池电极开始，很难制备出含有相关界面的 APT 试样尖端。在这里，我们展示了一种对电池界面进行可靠 APT 成像的方法，其中薄膜电极的几何形状可提供良好控制的平面界面，非常适合 APT 样品制备和成像。我们以使用脉冲激光沉积（PLD）合成的磷酸铁锂（LFP）薄膜电极为例，研究了标准锂盐电解质系统。为了使研究结果适用于传统的微粒电极，必须获得具有代表性的薄膜结构和电化学特性。因此，我们研究了 PLD 条件（包括基底温度、基底结晶度、目标成分和沉积时间（激光脉冲数））对薄膜结晶纹理、形态和电化学性能的影响。优化后的 LFP 薄膜显示出良好的结晶度，低 C 速率容量约为 90 mAh g-1。LFP/ 电解质界面的初步 APT 三维成像显示，阴极-电解质相间层约为 10 nm，富含 F 和 Li。
{"title":"Atom Probe Tomography of the LiFePO4-Electrolyte Interface Enabled By Thin Film Electrodes","authors":"Elahe Moazzen, J. Mujtaba, Bruce Buchholz, Dieter Isheim, Norman Luu, David Rowell, Xiaobing Hu, Trung Ha, M. Hersam, Scott A Barnett","doi":"10.1149/1945-7111/ad5f21","DOIUrl":"https://doi.org/10.1149/1945-7111/ad5f21","url":null,"abstract":"\u0000 Atom probe tomography (APT) can yield three-dimensional tomographic images at atomic-scale resolution and low-AMU elements such as Li are readily observed, making it a powerful tool for exploring battery materials interfaces. However, it is difficult to prepare APT specimen tips containing the interface of interest starting with typical particle-based battery electrodes. Here we demonstrate a methodology for reliable APT imaging of battery interfaces in which a thin film electrode geometry is used to provide well-controlled planar interfaces that are ideal for APT sample preparation and imaging. LiFePO4 (LFP) thin film electrodes, synthesized using pulsed laser deposition (PLD), were studied as an example system, with standard Li-salt electrolytes. For the results to be applicable to conventional particulate electrodes, it is important to obtain representative thin film structure and electrochemical characteristics. Thus, the effects of PLD conditions including substrate temperature, substrate crystallinity, target composition, and deposition time (number of laser pulses) on the thin film's crystallographic texture, morphology, and electrochemical performance were studied. Optimized LFP film showed good crystallinity with low-C-rate capacity of ~ 90 mAh g-1. Initial APT three-dimensional imaging of the LFP/electrolyte interface shows an ~ 10 nm cathode-electrolyte interphase layer that is enriched in F and Li.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141680064","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}
Pub Date : 2024-07-03DOI: 10.1149/1945-7111/ad5ef9
Yan Ying Lee, Hoon Seng Chan, Julian Ulrich, A. Weber, Ulrike Krewer
This study presents an in-depth analysis of the cathode and anode of a commercial 18650 lithium-ion battery by comparing their dynamic behaviors systematically with that of two additional experimental cell setups: (i) full-cell in a three-electrode setup and (ii) symmetrical cathode and anode cells. The analysis involves subjecting the cells to electrochemical impedance spectroscopy, distribution of relaxation times, and nonlinear frequency response analysis at different state-of-charges. Our findings highlight the importance of analyzing the electrodes in all three setups. The impedance and nonlinear frequency response features of the full-cell are also observed in the electrode-resolved cells. Symmetrical cells exhibit stronger impedance and nonlinear responses compared to the commercial cell and the cell with reference electrode, yet they allow identifying contributions of the single cells without artifacts from inductive loops caused by the reference electrode. By correlating nonlinear signals and characteristic peaks across different cell setups, cathode and anode processes and their respective characteristic frequencies can be clearly identified.
{"title":"Full-, Half-, and Symmetrical Cell Analysis of Lithium-Ion Battery Using Impedance and Nonlinear Frequency Response","authors":"Yan Ying Lee, Hoon Seng Chan, Julian Ulrich, A. Weber, Ulrike Krewer","doi":"10.1149/1945-7111/ad5ef9","DOIUrl":"https://doi.org/10.1149/1945-7111/ad5ef9","url":null,"abstract":"\u0000 This study presents an in-depth analysis of the cathode and anode of a commercial 18650 lithium-ion battery by comparing their dynamic behaviors systematically with that of two additional experimental cell setups: (i) full-cell in a three-electrode setup and (ii) symmetrical cathode and anode cells. The analysis involves subjecting the cells to electrochemical impedance spectroscopy, distribution of relaxation times, and nonlinear frequency response analysis at different state-of-charges. Our findings highlight the importance of analyzing the electrodes in all three setups. The impedance and nonlinear frequency response features of the full-cell are also observed in the electrode-resolved cells. Symmetrical cells exhibit stronger impedance and nonlinear responses compared to the commercial cell and the cell with reference electrode, yet they allow identifying contributions of the single cells without artifacts from inductive loops caused by the reference electrode. By correlating nonlinear signals and characteristic peaks across different cell setups, cathode and anode processes and their respective characteristic frequencies can be clearly identified.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141680332","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}
Pub Date : 2024-07-03DOI: 10.1149/1945-7111/ad5efd
Ying Sun, T. Kadyk, A.A. Kulikovsky, M. Eikerling
We report a physics--based model for the electrochemical impedance of a PEM fuel cell cathode. The model takes into account the transient behavior of oxygen and proton transport in the cathode catalyst layer caused by variation of the liquid saturation with cell current. Transients of the catalyst layer oxygen diffusivity result in a second capacitive arc in the Nyquist spectrum, while proton conductivity transients lead to formation of an inductive loop. In the range of capillary pressures $p_c$ in which the liquid saturation in the catalyst layer is independent of $p_c$, the loop does not form. Stability analysis of a reduced system of equations reveals that the static solution with inductive loop is unstable with respect to spatial perturbations, implying that the post--oscillatory steady state is impossible to reach. Possible scenarios of instability development are discussed.
{"title":"The Effect of Liquid Saturation Transients on PEM Fuel Cell Impedance: Inductive Loop and Instability of Catalyst Layer Operation","authors":"Ying Sun, T. Kadyk, A.A. Kulikovsky, M. Eikerling","doi":"10.1149/1945-7111/ad5efd","DOIUrl":"https://doi.org/10.1149/1945-7111/ad5efd","url":null,"abstract":"\u0000 We report a physics--based model for the electrochemical impedance of a PEM fuel cell cathode. The model takes into account the transient behavior of oxygen and proton transport in the cathode catalyst layer caused by variation of the liquid saturation with cell current. Transients of the catalyst layer oxygen diffusivity result in a second capacitive arc in the Nyquist spectrum, while proton conductivity transients lead to formation of an inductive loop. In the range of capillary pressures $p_c$ in which the liquid saturation in the catalyst layer is independent of $p_c$, the loop does not form. Stability analysis of a reduced system of equations reveals that the static solution with inductive loop is unstable with respect to spatial perturbations, implying that the post--oscillatory steady state is impossible to reach. Possible scenarios of instability development are discussed.","PeriodicalId":509718,"journal":{"name":"Journal of The Electrochemical Society","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141682317","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}
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