Riconosciamo con gratitudine il sostegno del programma Ceramica nella divisione di materiali di ricerca della US National Science Foundation, con la concessione n. DMR-1006515 (program manager, il dottor Lynnette D. Madsen).

1. Preparazione di un elettrodo di lavoro <ol><li> Preparare una miscela di ~ 6 wt. % Di polivinilidene fluoruro (PVDF) legante in N-metil-2-pirrolidone (NMP). </li><li> Pesare 80 wt. % Materiale attivo (LiCoO 2 in questo caso) e 10 wt. % C nero (acetilene, + 99,9%) e poi miscelare in un vortice per 1 min. </li><li> Aggiungere NMP-legante miscela tale che il legante costituisce il 10 wt. % Del peso totale della miscela. </li><li> Trasferire la suddetta miscela in una piccola fiala di vetro e di miscela nel miscelatore a vortice di giri massimo per circa 30 min. Due palle di ossido di zirconio del diametro di 5 mm può essere utilizzata come supporto per una migliore miscelazione. Se necessario, aggiungere più NMP per ottenere slurry di consistenza richiesta. </li><li> Stendere un foglio metallico di collettore di corrente (tipicamente, alluminio per il catodo e l&#39;anodo di rame per) su di una lastra di vetro. L&#39;uso di acetone e di garantire che non vi siano bolle d&#39;aria tra la pellicola e la lastra di vetro. Utilizzare due strati di nastro adesivo in modo da formare una traccia e defnare la regione da rivestire. </li><li> Applicare la sospensione al foglio metallico con una spatola in acciaio inossidabile e diffondere uniformemente lo slurry sulla pista usando una lama di rasoio. </li><li> Essiccare il rivestimento in aria o sotto vuoto a ~ 90-120 ° C per circa 2-8 ore (che dovrebbe essere regolato dipende dal materiale utilizzato e legante). </li><li> Posizionare la lamina rivestita di metallo tra due piastre di acciaio (e due documenti di pesatura per proteggere il rivestimento) e stampa sotto un carico di ~ 3000 £ utilizzando una pressa idraulica. </li><li> Punch la pellicola essiccata in metallo verniciato in dischi di 8 mm di diametro (preferibilmente all&#39;interno di un vano portaoggetti). Pesare i catodi e avvolgere prima del trasferimento nel vano portaoggetti. </li><li> Perforare il foglio metallico rivestito con lo stesso materiale in dischi di diametro di 8 mm e peso tali dischi. </li></ol> 2. Preparazione di elettroliti <ol><li> Poiché l&#39;elettrolita è fotosensibile, memorizzare l&#39;elettrolita (1M LiPF 6 in EC: DMC: DEC in questo caso) in un bottl Nalgenee avvolto da un foglio di alluminio. </li></ol> 3. Preparazione di un controelettrodo (lamina di litio in questo caso) <ol><li> Pulire la superficie del foglio di litio con una spazzola in nylon / acciaio inox bisturi fino ad una superficie lucida argentata appare (all&#39;interno di un vano portaoggetti argon). </li><li> Punch il foglio di litio in dischi di diametro di ½ pollice (all&#39;interno di un vano portaoggetti argon). </li></ol> 4. Coin cella di assemblaggio <ol><li> Figura 2 mostra una schematica del complesso a bottone. </li><li> Punch Celgard C480 membrane in dischi di 19 mm di diametro separatori e li usano come. </li><li> Trasferimento casi a bottone (CR2032), molle e distanziali (acquistati da MTI Corp.), i separatori e gli elettrodi di lavoro nel vano portaoggetti (dopo lavaggio dello scambiatore di cinque volte con argon). </li><li> Montare le batterie a bottone nel vano portaoggetti. </li><li> Aggiungere due gocce di elettrolita al tazza cella e posizionare l&#39;elettrodo di lavoro su di esso. Aggiungi un altro tregocce di elettrolita e posto due separatori con due gocce di elettrolita tra loro. Aggiungere due gocce più dell&#39;elettrolita prima di posizionare il controelettrodo litio su di esso. Mettere due distanziali in acciaio inox e una molla sul disco di litio. </li><li> Chiudere il cellulare usando il tappo di cella e crimpare 3-4 volte con la macchina compatta crimpatura (acquistato da MTI Corp.). </li><li> Dopo aver assemblato le celle, maneggiare le cellule finiti utilizzando una pinzetta di plastica (per evitare corto circuiti). </li><li> Pulire l&#39;elettrolita in eccesso che fuoriesce dai lati della cella utilizzando un tovagliolo di carta. </li><li> La cella è pronto per il collaudo e può essere estratto il vano portaoggetti. </li></ol> 5. Coin cella Testing <ol><li> Mantenere la cella moneta collegato alla batteria tester in tensione a circuito aperto (OCV) modalità per un&#39;ora appena è pronto. </li><li> Definire finestra tensione per testare la cella in base al materiale attivo utilizzato in elettrodo di lavoro. </li><li> Calcolare la lacapacità teorica per la cella utilizzando i calcoli mostrati sotto. </li></ol> Peso del disco elettrodo con la corrente di collettore = W EO Peso del disco rivestito corrente di collettore dello stesso diametro = W CC Peso del materiale di elettrodo, W EM, è dato dal <img alt="Equazione 1" src="/files/ftp_upload/4104/4104eq1.jpg" /> Peso del materiale attivo nell&#39;elettrodo, W AM, è dato dal <img alt="Equazione 2" src="/files/ftp_upload/4104/4104eq2.jpg" /> Capacità teorica per il disco elettrodo, C ED, è dato dal <img alt="Equazione 3" src="/files/ftp_upload/4104/4104eq3.jpg" /> dove C è la s teoricopecifici capacità del materiale attivo. <ol start="4"><li> Verificare la cella moneta per cicli di carica-scarica a richiesta C-rate. </li></ol> 6. Risultati rappresentativi Come esempio, una cellula moneta è stata costruita usando LiCoO 2 come materiale attivo per l&#39;elettrodo di lavoro. Dopo la costruzione, la cella è stato testato a C / 5 velocità. Il profilo ottenuto è mostrato nella Figura 3. La finestra di tensione è stato impostato per essere tra 3 e 4,3 V per questa cella moneta. La capacità è 155 mAh / g per il primo ciclo di carica e 140 mAh / g per il primo ciclo di scarico. <img alt="Figura 1" src="/files/ftp_upload/4104/4104fig1.jpg" /> Figura 1. Diagramma di flusso della procedura di costruzione moneta cella. In primo luogo, un elettrodo di lavoro viene preparato dalla polvere del materiale attivo. Poi, un elettrodo contatore viene preparato da una lamina di litio pulito ed i separatori sono perforato. Infine, una cellula èassemblati all&#39;interno di un vano portaoggetti argon. <img alt="Figura 2" src="/files/ftp_upload/4104/4104fig2.jpg" /> Figura 2. Schematica di un processo di assemblaggio delle cellule moneta che mostra tutti i componenti nell&#39;ordine in cui sono collocati all&#39;interno della cassa a bottone. <img alt="Figura 3" src="/files/ftp_upload/4104/4104fig3.jpg" /> Figura 3. Risultati rappresentativi ottenuto da una cellula moneta costruito utilizzando un elettrodo di lavoro composto da LiCoO 2 ed un elettrodo di litio lamina contatore. Il grafico mostra la prima carica e le curve di scarico prime per la cella moneta che è stata caricata e scaricata in C / 5 velocità. <img alt="Figura 4" src="/files/ftp_upload/4104/4104fig4.jpg" /> Figura 4. Confronto di rivestimenti positivi e negativi dopo che sono stati essiccati. Un rivestimento di cracking risulta tipicamente da liquame che ha eccesso di NMP e un rivestimento poroso risulta tipicamente da slurry che ha insufficiente NMP. <img alt="Figura 5" src="/files/ftp_upload/4104/4104fig5.jpg" /> Figura 5. Confronto di una cella moneta ben serrati e una cella moneta mal aggraffato, insieme a un non crimpate cella. Tipicamente, una cellula moneta mal serrati spacca dopo poche ore in ambiente a causa il rigonfiamento della lamina di litio dopo reazione con l&#39;umidità.

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Non ci sono conflitti di interesse dichiarati.

Nella nostra esperienza, la fase più critica nella preparazione dell&#39;elettrodo di lavoro sta facendo impasti con buone consistenza. Come mostrato in Figura 4, NMP eccesso nello slurry può risultare in un rivestimento cracking, mentre insufficiente NMP può risultare in un rivestimento poroso. Nel lavoro presentato qui, CR2032 casi a bottone che sono 20 mm di diametro vengono utilizzati. Va notato che i casi monete cellule di diverse dimensioni possono essere utilizzati, quando le dimensioni degli ...

<table border="1"><tbody><tr><td> Nome del reattivo </td><td> Azienda </td><td> Numero di catalogo </td></tr><tr><td> Poli (vinilidene fluoruro) </td><td> Sigma-Aldrich </td><td> 182702 </td></tr><tr><td> 1-metil-2-pirrolidinone, 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> Nerofumo, acetilene, + 99,9% </td><td> Alfa Aesar </td><td> 39724 </td></tr><tr><td> LiPF 6 in EC: DMC: DEC </td><td> MTI Corporation </td><td> EQ-Be-LiPF6 </td></tr><tr><td> Celgard separatore </td><td> Celgard </td><td> C480 </td></tr><tr><td> Vortex Mixer analogico </td><td> VWR </td><td> 58816-121 </td></tr><tr><td> Vacuum forno </td><td></td><td></td></tr><tr><td> Vuotopompa </td><td></td><td></td></tr><tr><td> Pressa idraulica </td><td></td><td></td></tr><tr><td> Coin cell caso </td><td> MTI Corporation </td><td> EQ-CR2032-CASE-304 </td></tr><tr><td> Primavera e distanziale </td><td> MTI Corporation </td><td> EQ-CR20SprSpa-304 </td></tr><tr><td> Glovebox </td><td> mBraun </td><td> UNILAB </td></tr><tr><td> Batteria tester </td><td> Arbin Instruments </td><td> BT2143 </td></tr></tbody></table>

construction and testing of coin cells of lithium ion batteries

Le batterie ricaricabili agli ioni di litio hanno applicazioni ampie in elettronica, in cui i clienti richiedono sempre più capacità e una maggiore durata. Batterie agli ioni di litio sono stati considerati per essere utilizzato in veicoli elettrici ibridi e 1 o addirittura elettrici sistemi di stabilizzazione della griglia 2. Tutte queste applicazioni simulare un drammatico aumento nella ricerca e nello sviluppo di materiali batteria 3-7, compresi i materiali nuovi 3,8, il doping 9, nanostrutturazione 10-13, rivestimenti o modificazioni superficiali 14-17 e 18 nuovi leganti. Di conseguenza, un numero crescente di fisici, chimici e scienziati dei materiali hanno recentemente avventurato in questa zona. Pile sono ampiamente utilizzati nei laboratori di ricerca per testare i materiali della nuova batteria, anche per la ricerca e sviluppo che le applicazioni di destinazione su larga scala e ad alta potenza, batterie a bottone di piccole dimensioni sono spesso usati per testare le capacità e le capacità di tasso dinuovi materiali nella fase iniziale. Nel 2010, abbiamo iniziato un National Science Foundation (NSF), patrocinata progetto di ricerca per studiare la superficie di assorbimento e disordinando in materiali della batteria (concessione n. DMR-1006515). Nella fase iniziale di questo progetto, abbiamo lottato per apprendere le tecniche di assemblaggio e collaudo batterie a bottone, che non possono essere raggiunti senza l&#39;aiuto di numerosi altri ricercatori in altre Università (attraverso chiamate frequenti, scambi e-mail e due visite in loco). Pertanto, riteniamo che sia utile per documentare, per testo e video, un protocollo di assemblaggio e collaudo di una cella moneta, che aiuterà gli altri nuovi ricercatori in questo campo. Questo sforzo rappresenta i &quot;più ampia&quot; Impact attività del nostro progetto NSF, ed aiuterà anche ad educare e ispirare gli studenti. In questo articolo video, documentare un protocollo di montare una batteria CR2032 moneta con un elettrodo di 2 LiCoO di lavoro, un elettrodo contatore Li,e (la maggior parte comunemente usato) polivinilidenfluoruro (PVDF) legante. Al fine di garantire nuovi discenti per ripetere facilmente il protocollo, manteniamo il protocollo il più specifico ed esplicito possibile. Tuttavia, è importante notare che nella ricerca e sviluppo specifico, molti parametri adottato qui può essere variata. In primo luogo, si possono rendere le cellule monete di diverse dimensioni e testare l&#39;elettrodo di lavoro contro un contro elettrodo diverso Li. In secondo luogo, le quantità di nero e C legante aggiunto in gli elettrodi di lavoro sono spesso adattate alle particolare scopo di ricerca, ad esempio, grandi quantità di C nero o addirittura polvere inerte sono stati aggiunti l&#39;elettrodo di lavoro per verificare l&#39;efficacia &quot;intrinseca&quot; di materiali catodici 14. Terzo, leganti meglio, diversi PVDF) hanno sviluppato e utilizzato 18. Infine, altri tipi di elettroliti (invece di LiPF 6) può anche essere utilizzato, infatti, alcuni alta tensione materiali elettrodici richiederà gli usi di electrol specialeYtes 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 protocollo per costruire e testare batterie a bottone di batterie agli ioni di litio viene descritto. Le specifiche procedure di realizzazione di un elettrodo di lavoro, preparando un controelettrodo, assemblando una cella all&#39;interno di un portaoggetti e verifica della cella sono presentati.

Costruzione e collaudo di Pile Batterie agli ioni di 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

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Engineering

31.2K Views.  Clemson University. Un protocollo per costruire e testare batterie a bottone di batterie agli ioni di litio viene descritto. Le specifiche procedure di realizzazione di un elettrodo di lavoro, preparando un controelettrodo, assemblando una cella all'interno di un portaoggetti e verifica della cella sono presentati.

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

Caratterizzazione di materiali per elettrodi per batterie agli ioni sodio e ioni di litio utilizzando tecniche Synchrotron Radiation

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

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Ingegneria

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 Neutron polvere diffrazione Utilizzo su misura agli ioni di litio batterie

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.

Failure Analysis delle batterie a base di sincrotrone Utilizzando raggi X duri microtomografia

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.

Speciazione e di biodisponibilità Misure di plutonio ambientale Uso Diffusione in film sottili

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.

Non acquoso Processing elettrodi e Costruzione di celle agli ioni di litio Coin

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.

Sintesi di ionici liquido a base di elettroliti, Assemblea delle batterie agli ioni di litio, e le misure di prestazioni ad alta temperatura

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.

Focused Ion Beam fabbricazione di Nanobatteries basati su LiPON litio allo stato solido per test 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.

Preparazione delle cellule di tre elettrodi moneta e Analitica di elettrodeposizione per batterie agli ioni di 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.

Espressione di soluzione cementizia poro e l'analisi della sua composizione chimica e la resistività mediante fluorescenza a raggi 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.

Preparazione delle cellule di Graphene liquido per l'osservazione di materiale batteria agli ioni di litio

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