Agradecemos el apoyo del programa de Cerámica en la División de Investigación de Materiales de los EE.UU. National Science Foundation, bajo la subvención no. DMR-1006515 (director del programa, el Dr. D. Lynnette Madsen).

1. Preparación de un electrodo de trabajo <ol><li> Preparar una mezcla de ~ 6 en peso. % De fluoruro de polivinilideno (PVDF) aglutinante en N-metil-2-pirrolidona (NMP). </li><li> Pesar 80 en peso. % De materia activa (LiCoO 2 en este caso) y el peso 10. % C negro (acetileno, un 99,9% +) y luego los mezcla en un vórtex durante 1 min. </li><li> Añadir NMP-aglutinante tal mezcla que constituye el aglutinante 10 en peso. % Del peso total de la mezcla. </li><li> Transferir la mezcla anterior en un pequeño frasco de vidrio y se mezcla en el mezclador de vórtice al régimen máximo durante aproximadamente 30 min. Dos bolas de circonia de 5 mm de diámetro pueden ser utilizados como medios para un mejor mezclado. Si es necesario, añadir más NMP para obtener pasta de consistencia requerida. </li><li> Extender una lámina metálica de la corriente de colector (típicamente, el aluminio para el cátodo y el ánodo de cobre para) sobre una placa de vidrio. Use acetona y asegurarse de que no hay burbujas de aire entre la lámina y la placa de vidrio. El uso de dos capas de cinta adhesiva para formar una pista y defINE región que va a revestirse. </li><li> Aplicar la suspensión a la lámina de metal utilizando una espátula de acero inoxidable y se extendió uniformemente sobre la suspensión a la pista utilizando una cuchilla de afeitar. </li><li> Secar la capa en el aire o vacío a ~ 90-120 ° C durante aproximadamente 2-8 horas (que debe ser ajustado en función del material y aglutinante utilizado). </li><li> Colocar la lámina metálica recubierta entre dos placas de acero (y dos documentos de pesaje para proteger el recubrimiento) y la prensa bajo una carga de ~ 3000 libras utilizando una prensa hidráulica. </li><li> Perforar la lámina metálica revestida seca en los discos de 8 mm de diámetro (de preferencia dentro de una caja con guantes). Pesar los cátodos y se envuelven antes de la transferencia en la guantera. </li><li> Perfore la lámina metálica recubierta del mismo material en discos de 8 mm de diámetro y pesa estos discos. </li></ol> 2. Preparación de Electrolito <ol><li> A medida que el electrolito es fotosensible, almacenar el electrolito (1M LiPF 6 en CE: DMC: diciembre en este caso) en un bottl Nalgenee envuelto por una lámina de aluminio. </li></ol> 3. Preparación de un contra-electrodo (lámina de litio en este caso) <ol><li> Limpiar la superficie de la lámina de litio usando un cepillo de nylon / acero bisturí de acero hasta una superficie plateada brillante aparece (dentro de una guantera argón). </li><li> Perfore el papel aluminio de litio en los discos de ½ pulgada de diámetro (dentro de una caja de guantes de argón). </li></ol> 4. Moneda de la Asamblea de la célula <ol><li> La figura 2 muestra un esquema del conjunto celular moneda. </li><li> Golpe Celgard C480 membranas en los discos de 19 mm de diámetro en los separadores y los utilizan como. </li><li> Traslado de los casos de células de la moneda (CR2032), muelles y separadores (comprado a MTI Corp.), separadores y los electrodos de trabajo en la guantera (después de la limpieza del intercambiador de cinco veces con argón). </li><li> Montar las células de la moneda en la guantera. </li><li> Añadir dos gotas del electrolito en la célula a la taza y colocar el electrodo de trabajo en ella. Añadir otros tresgotas del electrolito y el lugar dos separadores con dos gotas de electrolito entre ellos. Añadir dos gotas más de la electrolito antes de colocar el contra-electrodo de litio en ella. Coloque dos espaciadores de acero inoxidable y un resorte en el disco de litio. </li><li> Cerca de la celda utilizando la tapa de la celda y el engarce de 3-4 veces usando la máquina de prensado compacta (comprado a MTI Corp.). </li><li> Después de montar las células, manejar las células terminados utilizando pinzas de plástico (para evitar cortocircuitos). </li><li> Limpiar el exceso de electrolito fugas desde los lados de la celda utilizando una servilleta de papel. </li><li> La célula está listo para el ensayo y se puede sacar de la guantera. </li></ol> 5. Prueba de la moneda de la célula <ol><li> Mantener la celda de moneda conectado al medidor de batería en la tensión de circuito abierto (OCV) el modo durante una hora, tan pronto como esté listo. </li><li> Definir ventana de tensión para probar la celda basado en el material activo utilizado en electrodo de trabajo. </li><li> Calcular la de lacapacidad teórico para la celda utilizando los cálculos que se muestran a continuación. </li></ol> Peso del disco electrodo con la corriente de colector = W EO Peso del disco colector de corriente sin revestir del mismo diámetro = W CC Peso de material de electrodo, W EM, está dada por <img alt="Ecuación 1" src="/files/ftp_upload/4104/4104eq1.jpg" /> Peso de material activo en el electrodo, W AM, se da por <img alt="Ecuación 2" src="/files/ftp_upload/4104/4104eq2.jpg" /> La capacidad teórica para el disco de electrodo, C ED, está dada por <img alt="Ecuación 3" src="/files/ftp_upload/4104/4104eq3.jpg" /> donde C es la teórica scapacidad ESPECÍFICA del material activo. <ol start="4"><li> Prueba de la célula de la moneda a los ciclos de carga-descarga en la C-tasa requerida. </li></ol> 6. Los resultados representativos Como un ejemplo, una célula de la moneda se construyó utilizando LiCoO 2 como el material activo para el electrodo de trabajo. Después de la construcción, la célula se ensayó en la C / 5 tasa. El perfil obtenido se muestra en la Figura 3. La ventana de tensión se fija para ser entre 3 y 4,3 V de esta célula de la moneda. La capacidad fue de 155 mAh / g para el ciclo de carga primero y 140 mAh / g para el ciclo de descarga primero. <img alt="Figura 1" src="/files/ftp_upload/4104/4104fig1.jpg" /> Figura 1. Diagrama de flujo del procedimiento de moneda construcción celular. En primer lugar, un electrodo de trabajo se preparó a partir del polvo del material activo. Entonces, un contra-electrodo se preparó a partir de una lámina de litio limpio y los separadores se troquelan. Finalmente, una célula esensamblada dentro de una caja de guantes de argón. <img alt="Figura 2" src="/files/ftp_upload/4104/4104fig2.jpg" /> Figura 2. Esquemática de un proceso de moneda conjunto celular que muestra todos los componentes en el orden en que se colocan dentro de la carcasa de la celda moneda. <img alt="Figura 3" src="/files/ftp_upload/4104/4104fig3.jpg" /> Figura 3. Los resultados representativos obtenido a partir de una célula de la moneda construido utilizando un electrodo de trabajo hecha de LiCoO 2 y un electrodo de lámina de litio contador. La gráfica muestra la primera carga y la descarga de las primeras curvas de la célula de la moneda que se ha cargado y descargado en C / 5 la tasa. <img alt="Figura 4" src="/files/ftp_upload/4104/4104fig4.jpg" /> Figura 4. Comparación de los recubrimientos de buenas y malas después de que han sido secados. Un recubrimiento agrietado típicamente resulta de suspensión que tiene exceso de NMP y un revestimiento poroso típicamente resulta de slurry que tiene insuficiente NMP. <img alt="Figura 5" src="/files/ftp_upload/4104/4104fig5.jpg" /> Figura 5. Comparación de una celda de moneda bien engarzado y una celda de moneda mal engarzado, junto con una célula no-ondulado. Típicamente, una célula de la moneda mal engarzado divide abierta después de unas pocas horas en ambiente debido a la hinchazón de lámina de litio después de la reacción con la humedad.

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No hay conflictos de interés declarado.

En nuestra experiencia, el paso más crítico en la preparación del electrodo de trabajo está haciendo lechadas buenos con consistencia. Como se muestra en la Figura 4, el exceso de NMP en la suspensión puede resultar en un revestimiento agrietado, mientras insuficiente NMP puede resultar en un revestimiento poroso. En el trabajo presentado aquí, CR2032 celda de moneda de los casos que son de 20 mm de diámetro se utilizan. Cabe señalar que los casos de monedas de células de diferentes tamaños se...

<table border="1"><tbody><tr><td> Nombre del reactivo </td><td> Empresa </td><td> Número de catálogo </td></tr><tr><td> Poli (fluoruro de vinilideno) </td><td> Sigma-Aldrich </td><td> 182702 </td></tr><tr><td> 1-metil-2-pirrolidinona, 99,5% </td><td> Alfa Aesar </td><td> 31903 </td></tr><tr><td> LiCoO 2 </td><td> Alfa Aesar </td><td> 42090 </td></tr><tr><td> El negro de carbón, acetileno, 99,9% más </td><td> Alfa Aesar </td><td> 39724 </td></tr><tr><td> LiPF 6 de la CE: DMC: diciembre </td><td> MTI Corporación </td><td> EQ-Be-LiPF6 </td></tr><tr><td> Celgard separador </td><td> Celgard </td><td> C480 </td></tr><tr><td> Mezclador Vortex analógica </td><td> VWR </td><td> 58816-121 </td></tr><tr><td> Horno al vacío </td><td></td><td></td></tr><tr><td> Vacíobomba </td><td></td><td></td></tr><tr><td> Prensa hidráulica </td><td></td><td></td></tr><tr><td> Moneda caso de la célula </td><td> MTI Corporación </td><td> EQ-CR2032-CASE-304 </td></tr><tr><td> La primavera y el espaciador </td><td> MTI Corporación </td><td> EQ-CR20SprSpa-304 </td></tr><tr><td> Guantera </td><td> mBraun </td><td> UNILAB </td></tr><tr><td> Batería probador </td><td> Arbin Instruments </td><td> BT2143 </td></tr></tbody></table>

construction and testing of coin cells of lithium ion batteries

Las baterías recargables de iones de litio tienen amplias aplicaciones en la electrónica, donde los clientes siempre exigen más capacidad y mayor vida útil. Baterías de ión litio también se han considerado para ser utilizado en vehículos eléctricos e híbridos 1 o sistemas de la red eléctrica, incluso de estabilización 2. Todas estas aplicaciones simular un aumento dramático en la investigación y el desarrollo de materiales de la batería 3-7, incluyendo nuevos materiales 3,8, el dopaje 9, nanoestructuración 10-13, revestimientos o modificaciones de superficies 14-17 y aglutinantes novedosos 18. En consecuencia, un número creciente de físicos, químicos y científicos de los materiales recientemente han incursionado en esta área. Las células de la moneda son ampliamente utilizados en los laboratorios de investigación para poner a prueba los nuevos materiales de la batería, e incluso para la investigación y desarrollo que las aplicaciones de destino a gran escala y de alta potencia, las células pequeñas de monedas se utilizan a menudo para poner a prueba las capacidades y competencias de velocidad delos nuevos materiales en la etapa inicial. En 2010, comenzó la National Science Foundation (NSF), patrocinado proyecto de investigación para investigar la superficie de adsorción y el desorden en los materiales de la batería (subvención no. DMR-1006515). En la etapa inicial de este proyecto, hemos luchado para aprender las técnicas de montaje y prueba de las células de la moneda, que no se puede lograr sin la ayuda de numerosos otros investigadores de otras universidades (a través de llamadas frecuentes, los intercambios de correo electrónico y dos visitas de campo). Por lo tanto, creemos que es beneficioso para documentar, tanto por texto y vídeo, un protocolo de montaje y prueba de una célula de la moneda, lo que ayudará a otros nuevos investigadores en este campo. Este esfuerzo representa el &quot;mayor impacto&quot;, las actividades de nuestro proyecto de la NSF, y también ayudará a educar e inspirar a los estudiantes. En este artículo de vídeo, se documenta un protocolo para montar una pila de botón CR2032 con una LiCoO 2 electrodo de trabajo, un electrodo contador de Li,y (la mayoría de uso general) de fluoruro de polivinilideno (PVDF) aglutinante. Para asegurarse de nuevos estudiantes a repetir fácilmente el protocolo, seguimos el protocolo lo más específico y explícito posible. Sin embargo, es importante señalar que en específico de investigación y trabajo de desarrollo, muchos parámetros adoptado aquí se puede variar. En primer lugar, se puede hacer que las células de monedas de diferentes tamaños y probar el electrodo de trabajo frente a un electrodo contador que no sea Li. En segundo lugar, las cantidades de C negro y aglutinante añadido en los electrodos de trabajo son a menudo variar para adaptarse a la finalidad particular de la investigación, por ejemplo, grandes cantidades de negro C o incluso polvo inerte se añadieron al electrodo de trabajo para probar la &quot;intrínseca&quot; rendimiento de 14 materiales de cátodo. En tercer lugar, aglutinantes mejores (que no sea PVDF) también han desarrollado y utilizado 18. Finalmente, otros tipos de electrolitos (en lugar de LiPF 6) también se pueden utilizar, de hecho, ciertos materiales de alto voltaje de los electrodos se requieren los usos de Electrol especialytes 7.

Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

Construction and Testing of Coin Cells of Lithium Ion Batteries

Un protocolo para construir y poner a prueba las células de la moneda de baterías de iones de litio se describe. Los procedimientos específicos de toma de un electrodo de trabajo, la preparación de un contra-electrodo, montaje de una celda dentro de una caja de guantes y probar la celda se presentan.

Construcción y verificación de las células de la moneda de baterías de ion de litio

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

construction-and-testing-of-coin-cells-of-lithium-ion-batteries

Research

JoVE Journal

Engineering

31.1K vistas.  Clemson University. Un protocolo para construir y poner a prueba las células de la moneda de baterías de iones de litio se describe. Los procedimientos específicos de toma de un electrodo de trabajo, la preparación de un contra-electrodo, montaje de una celda dentro de una caja de guantes y probar la celda se presentan.

Video: Construction and Testing of Coin Cells of Lithium Ion Batteries

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

Caracterización de los materiales de los electrodos de ión de litio y baterías de ión sodio utilizando técnicas de Radiación Sincrotrón

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Investigación

Ingeniería

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

In Situ de neutrones polvo Difracción Uso de baterías de litio-ion por encargo

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

Análisis de Falla en Baterías Utilizando Microtomografía duro de rayos X a base de Sincrotrón

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

Especiación y biodisponibilidad mediciones de plutonio Ambiental Uso de Difusión en Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational analysis. Testing of lithium-ion batteries in an academic setting has taken on several forms, but at the most basic level lies the coin cell construction. In traditional LIB electrode preparation, a multi-phase slurry composed of active material, binder, and conductive additive is cast out onto a substrate. An electrode disc can then be punched from the dried sheet and used in the construction of a coin cell for electrochemical evaluation. Utilization of the potential of the active material in a battery is critically dependent on the microstructure of the electrode, as an appropriate distribution of the primary components are crucial to ensuring optimal electrical conductivity, porosity, and tortuosity, such that electrochemical and transport interaction is optimized. Processing steps ranging from the combination of dry powder, wet mixing, and drying can all critically affect multi-phase interactions that influence the microstructure formation. Electrochemical probing necessitates the construction of electrodes and coin cells with the utmost care and precision. This paper aims at providing a step-by-step guide of non-aqueous electrode processing and coin cell construction for lithium-ion batteries within an academic setting and with emphasis on deciphering the influence of drying and calendaring.

Non-aqueous electrode processing is central to the construction of coin cells and the evaluation of new electrode chemistries for lithium-ion batteries. A step-by-step guide to the basic practices needed as an electrochemical engineer working with batteries in an academic experimental setting is furnished.

Procesamiento de electrodos no acuoso y Construcción de células de iones de litio de la moneda

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

Síntesis de líquidos iónicos electrolitos basados, Montaje de baterías de ion-litio, y mediciones de rendimiento a temperaturas elevadas

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

Ion enfocado viga fabricación de Nanobatteries LiPON basado en estado sólido-ion de litio para la prueba In Situ

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

Moneda de tres electrodos célula preparación y análisis de electrodeposición para baterías de iones de litio

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

Expresión de la solución de poro del cemento y el análisis de su composición química y resistencia mediante fluorescencia de rayos x

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

Preparación de las células del líquido de grafeno para la observación de Material de batería de iones de litio

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...