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Method Article
* Wspomniani autorzy wnieśli do projektu równy wkład.
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.
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.
Although the origin of lithium-batteries can be traced arbitrarily far back into the past, the large-scale production and commercialization of many of today's commonly found lithium-ion batteries began in the 1980s. Many of the materials developed during this era, one example being Lithium Cobalt Oxide (LiCoO2), are still commonly found in use today1. Many current studies have been focused towards the development of various other metal oxide structures, with some emphasis placed towards reducing or eliminating the use of cobalt in place of other lower cost and more environmentally benign metals, such as manganese or nickel
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1. Reference Electrode and Separator Preparation
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Typical results for the voltage and potential profiles for the three-electrode cell can be seen in Figure 7. In an ideal setup, the full cell voltage should be identical to that produced from a two-electrode cell using the same electrode couple. This is one method to determine whether the insertion of the reference electrode modifies the performance of the cell. If there is a significant difference between the two- and three-electrode full cell performance (f.......
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Cell crimping pressure plays an important part in the success rate of both the preparation and working cells. If the cell is crimped at too high a pressure (>800 psi), the reference electrode can become shorted with the cell cap due to the reference wire position in-between the cap and the gasket. Note that the wire crossing this interface is a requirement in order to connect the reference electrode reading to an external measurement device. If the cell pressure is too low (<700 psi), the cell can have issues wit.......
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The authors have nothing to disclose.
Financial support from the Texas Instruments (TI) University Research Partnership program is gratefully acknowledged. The authors also gratefully acknowledge the assistance of Chien-Fan Chen from the Energy and Transport Sciences Laboratory, Mechanical Engineering, Texas A&M University, during the initial stage of this work.
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Name | Company | Catalog Number | Comments |
Agate Mortar and Pestle | VWR | 89037-492 | 5 in diameter |
Die Set | Mayhew | 66000 | |
Laboratory Press | MTI | YLJ-12 | |
Analytical Scale | Ohaus | Adventurer AX | |
High-Shear Mixing Device | IKA | 3645000 | |
Argon-filled Glovebox | MBraun | LABstar | |
Hydraulic Crimper | MTI | MSK-110 | |
Battery Cycler | Arbin Instruments | BT2000 | |
Potentiostat/Galvanostat/EIS | Bio-Logic | VMP3 | |
Vacuum Oven and Pump | MTI | - | |
Copper Wire | Remington | PN155 | 32 AWG |
Glass Balls | McMasterr-Carr | 8996K25 | 6 mm borosilicate glass balls |
Stirring Tube | IKA | 3703000 | 20 ml |
Celgard 2500 Separator | MTI | EQ-bsf-0025-60C | 25 μm thick; Polypropylene |
Stainless Steel CR2032 Coin Cell Kit | Pred Materials | Coin cell kit includes: case, cap, PP gasket | |
Stainless Steel Spacer | Pred Materials | 15.5 mm diameter × 0.5 mm thickness | |
Stainless Steel Wave Spring | Pred Materials | 15.0 mm diameter × 1.4 mm height | |
Li-ion Battery Anode - Graphite | MTI | bc-cf-241-ss-005 | Cu Foil Single Side Coated by CMS Graphite (241mm L x 200mm W x 50μm Thickness) |
Li-ion Battery Cathode - LiCoO2 | MTI | bc-af-241co-ss-55 | Al Foil Single Side Coated by LiCoO2 (241mm L x 200mm W x 55μm Thickness) |
Polyvinylidene Difluoride (PVDF) | Kynar | Flex 2801 | |
N-Methyl-2-Pyrrolidinone Anhydrous (NMP), 99.5% | Sigma Aldrich | 328634 | |
CNERGY Super C-65 | Timcal | ||
Electrolyte (1.0 M LiPF6 in EC/DEC, 1:1 by vol.) | BASF | 50316366 | |
Lithium Titanate (Li4Ti5O12) | Sigma Aldrich | 702277 | |
KS6 Synthetic Graphite | Timcal | ||
Lithium Metal Ribbon | Sigma Aldrich | 320080 | 0.75 mm thickness |
Epoxy Multipurpose | Loctite | ||
Electrical Tape | Scotch 3M Super 88 | ||
Isopropyl Alcohol (IPA), ACS reagent, ≥99.5% | Sigma Aldrich | 190764 |
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