Name: three-electrode coin cell preparation and electrodeposition analytics for lithium-ion batteries
Uploaded: 2018-05-22T15:00:00.000+00:00
Duration: 10 min 41 s
Description: Watch this Scientific Journal Video about Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries at JoVE.com

텍사스 인스트루먼트 (TI) 대학 연구 협력 프로그램에서 재정 지원은 기꺼이 인정 했다. 저자는 또한 기꺼이이 작품의 초기 단계에서 에너지와 수송 과학 실험실, 기계 공학, 텍사스 A에서 Chien-팬 첸의 도움 & M 대학 인정합니다.

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	<li>Whittingham, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+batteries+and+cathode+materials.">Lithium batteries and cathode materials.</a> Chemical Reviews. 104 (10), 4271-4301 (2004).</li><li>Schipper, F., Aurbach, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Brief+Review:+Past,+Present+and+Future+of+Lithium+Ion+Batteries.">A Brief Review: Past, Present and Future of Lithium Ion Batteries.</a> Russian Journal of Electrochemistry. 52 (12), 1095-1121 (2016).</li><li>Stein, M., Chen, C. F., Robles, D. J., Rhodes, C., Mukherjee, P. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Non-aqueous+Electrode+Processing+and+Construction+of+Lithium-ion+Coin+Cells.">Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells.</a> Journal of Visualized Experiments. (108), e53490 (2016).</li><li>Juarez-Robles, D., Chen, C. F., Barsoukov, Y., Mukherjee, P. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Impedance+Evolution+Characteristics+in+Lithium-Ion+Batteries.">Impedance Evolution Characteristics in Lithium-Ion Batteries.</a> Journal of the Electrochemical Society. 164 (4), 837-847 (2017).</li><li>Wu, Q. W., Lu, W. Q., Prakash, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+a+commercial+size+cylindrical+Li-ion+cell+with+a+reference+electrode.">Characterization of a commercial size cylindrical Li-ion cell with a reference electrode.</a> Journal of Power Sources. 88 (2), 237-242 (2000).</li><li>Wu, M. S., Chiang, P. C. J., Lin, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+investigations+on+advanced+lithium-ion+batteries+by+three-electrode+measurements.">Electrochemical investigations on advanced lithium-ion batteries by three-electrode measurements.</a> Journal of the Electrochemical Society. 152 (1), 47-52 (2005).</li><li>Jansen, A. N., Dees, D. W., Abraham, D. P., Amine, K., Henriksen, G. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Low-temperature+study+of+lithium-ion+cells+using+a+LiySn+micro-reference+electrode.">Low-temperature study of lithium-ion cells using a LiySn micro-reference electrode.</a> Journal of Power Sources. 174 (2), 373-379 (2007).</li><li>Belt, J. R., Bernardi, D. M., Utgikar, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+and+Use+of+a+Lithium-Metal+Reference+Electrode+in+Aging+Studies+of+Lithium-Ion+Batteries.">Development and Use of a Lithium-Metal Reference Electrode in Aging Studies of Lithium-Ion Batteries.</a> Journal of the Electrochemical Society. 161 (6), 1116-1126 (2014).</li><li>McTurk, E., Birkl, C. R., Roberts, M. R., Howey, D. A., Bruce, P. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Minimally+Invasive+Insertion+of+Reference+Electrodes+into+Commercial+Lithium-Ion+Pouch+Cells.">Minimally Invasive Insertion of Reference Electrodes into Commercial Lithium-Ion Pouch Cells.</a> Ecs Electrochemistry Letters. 4 (12), 145-147 (2015).</li><li>Garcia, G., Schuhmann, W., Ventosa, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Three-Electrode,+Battery-Type+Swagelok+Cell+for+the+Evaluation+of+Secondary+Alkaline+Batteries:+The+Case+of+the+Ni-Zn+Battery.">A Three-Electrode, Battery-Type Swagelok Cell for the Evaluation of Secondary Alkaline Batteries: The Case of the Ni-Zn Battery.</a> Chemelectrochem. 3 (4), 592-597 (2016).</li><li>Solchenbach, S., Pritzl, D., Kong, E. J. Y., Landesfeind, J., Gasteiger, H. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Gold+Micro-Reference+Electrode+for+Impedance+and+Potential+Measurements+in+Lithium+Ion+Batteries.">A Gold Micro-Reference Electrode for Impedance and Potential Measurements in Lithium Ion Batteries.</a> Journal of the Electrochemical Society. 163 (10), 2265-2272 (2016).</li><li>Waldmann, T., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Interplay+of+Operational+Parameters+on+Lithium+Deposition+in+Lithium-Ion+Cells:+Systematic+Measurements+with+Reconstructed+3-Electrode+Pouch+Full+Cells.">Interplay of Operational Parameters on Lithium Deposition in Lithium-Ion Cells: Systematic Measurements with Reconstructed 3-Electrode Pouch Full Cells.</a> Journal of the Electrochemical Society. 163 (7), 1232-1238 (2016).</li><li>Costard, J., Ender, M., Weiss, M., Ivers-Tiffee, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Three-Electrode+Setups+for+Lithium-Ion+Batteries+II.+Experimental+Study+of+Different+Reference+Electrode+Designs+and+Their+Implications+for+Half-Cell+Impedance+Spectra.">Three-Electrode Setups for Lithium-Ion Batteries II. Experimental Study of Different Reference Electrode Designs and Their Implications for Half-Cell Impedance Spectra.</a> Journal of the Electrochemical Society. 164 (2), 80-87 (2017).</li><li>Dees, D. W., Jansen, A. N., Abraham, D. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Theoretical+examination+of+reference+electrodes+for+lithium-ion+cells.">Theoretical examination of reference electrodes for lithium-ion cells.</a> Journal of Power Sources. 174 (2), 1001-1006 (2007).</li><li>Ender, M., Weber, A., Ivers-Tiffee, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analysis+of+Three-Electrode+Setups+for+AC-Impedance+Measurements+on+Lithium-Ion+Cells+by+FEM+simulations.">Analysis of Three-Electrode Setups for AC-Impedance Measurements on Lithium-Ion Cells by FEM simulations.</a> Journal of the Electrochemical Society. 159 (2), 128-136 (2012).</li><li>La Mantia, F., Wessells, C. D., Deshazer, H. D., Cui, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reliable+reference+electrodes+for+lithium-ion+batteries.">Reliable reference electrodes for lithium-ion batteries.</a> Electrochemistry Communications. 31, 141-144 (2013).</li><li>Nakahara, K., Nakajima, R., Matsushima, T., Majima, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+of+particulate+Li4Ti5O12+having+excellent+characteristics+as+an+electrode+active+material+for+power+storage+cells.">Preparation of particulate Li4Ti5O12 having excellent characteristics as an electrode active material for power storage cells.</a> Journal of Power Sources. 117 (1-2), 131-136 (2003).</li><li>Shi, Y., Wen, L., Li, F., Cheng, H. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanosized+Li4Ti5O12/graphene+hybrid+materials+with+low+polarization+for+high+rate+lithium+ion+batteries.">Nanosized Li4Ti5O12/graphene hybrid materials with low polarization for high rate lithium ion batteries.</a> Journal of Power Sources. 196 (20), 8610-8617 (2011).</li><li>Dolle, M., Orsini, F., Gozdz, A. S., Tarascon, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+reliable+three-electrode+impedance+measurements+in+plastic+Li-ion+batteries.">Development of reliable three-electrode impedance measurements in plastic Li-ion batteries.</a> Journal of the Electrochemical Society. 148 (8), 851-857 (2001).</li><li>Zaghib, K., Simoneau, M., Armand, M., Gauthier, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+study+of+Li4Ti5O12+as+negative+electrode+for+Li-ion+polymer+rechargeable+batteries.">Electrochemical study of Li4Ti5O12 as negative electrode for Li-ion polymer rechargeable batteries.</a> Journal of Power Sources. 81, 300-305 (1999).</li><li>Delacourt, C., Ridgway, P. L., Srinivasan, V., Battaglia, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Measurements+and+Simulations+of+Electrochemical+Impedance+Spectroscopy+of+a+Three-Electrode+Coin+Cell+Design+for+Li-Ion+Cell+Testing.">Measurements and Simulations of Electrochemical Impedance Spectroscopy of a Three-Electrode Coin Cell Design for Li-Ion Cell Testing.</a> Journal of the Electrochemical Society. 161 (9), 1253-1260 (2014).</li></ol>

저자는 공개 없다.

셀 압력 crimping 준비 작업 셀의 성공률에 중요 한 역할을 한다. 너무 높은 압력에서 셀에 대 한 주름을 잡은 경우 (> 800 psi), 참조 전극 때문에 참조 셀 캡으로 누전 될 수 있는 모자와 개 스 위치 사이 와이어. Note이 인터페이스를 건너 와이어 외부 측정 장치에 읽기 참조 전극 연결 하려면 요구 사항입니다. 셀 압력이 너무 낮은 경우 (< 700 psi), 셀 수 있는 문제가 불완전 crimping 전해질 누설을 발생할 ?...

리튬 배터리의 근원 추적 될 수 있다까지 임의로 다시 대규모 생산 및 상용화 오늘날의 많은 과거에 일반적으로 발견된 리튬-이온 배터리는 1980 년대에서 시작 했다. 이 시대, 한 예로 리튬 코발트 산화물 (LiCoO2) 되 고 개발 하는 물자의 많은 여전히 일반적으로 사용 하 여 오늘1에서 발견 된다. 많은 현재 연구의 감소 또는 제거 대신에 다른 저렴 한 비용 및 환경 양성 금속 코발트를 사용 하 여 같은 쪽으로 배치 일부 강조와 다양 한 다른 금속 산화물 구조 개발 쪽으로 초점을 맞춘 되었습니다. 망간 또는 니켈2. 리튬-이온 배터리에 사용 되는 재료의 지속적으로 변화 하는 풍경 특성화 그들의 성능 및 안전의 효과적이 고 정확한 방법이 필요로 합니다. 모든 배터리의 작동 긍정적이 고 부정적인 전극의 결합 된 전기 화학 반응 포함, 때문에 전형적인 두 전극 배터리 전극에 특성을 독립적으로 수 있는 짧은을. 불 쌍 한 특성화 및 이해의 후속 부족 다음 위험한 상황 또는 저하 현상의 존재로 인해 전체 배터리 성능 저하를 발생할 수 있습니다. 이전 연구는 일반적인 2 전극 셀3에 대 한 처리 기법 표준화 목적 되었습니다. 표준 셀 구성의 단점에는 한 가지 방법은 3 전극 셀입니다.
3 전극 설치 두 전극의 응답을 분리 하 고 배터리 작동의 근본적인 물리학에 큰 통찰력을 제공 하는 방법은 이다. 3 전극 설치 참조 전극은 음극과 양극 소개 된다. 이 참조 전극 다음 작업 하는 동안 동적으로 양극과 음극의 잠재력을 측정 하는 데 사용 됩니다. 아니 현재 참조 전극을 통해 전달 되 고 따라서, 그것은 단 수, 그리고 이상적으로 안정적인 전압을 제공 한다. 3 전극 설치를 사용 하 여 전체 셀 전압, 음극 잠재력 및 양극 잠재력 수집할 수 있습니다 동시에 작업 중. 잠재적인 측정 뿐만 아니라 전극의 임피던스 기여 충전4셀 상태의 기능으로 특징 수 있습니다.
3 전극 체제는 공부 하는 리튬-이온 배터리, 리튬 금속, 리튬 도금 라고도 electrodeposition 등에서 저하 현상에 대 한 매우 유용 합니다. 다른 그룹 3-전극 설정5,6,7,,89,10,11,12, 제안 했다 13 하지만 그들은 종종 본질적으로 불안정 한 리튬 금속을 사용 하 여 참조로 하 고 사용자 정의 설정을 감소 된 안정성으로 이끌어 조립 하기가 포함 됩니다. 리튬 도금 일어난다 때 호스트 전극 구조에 intercalating 대신, 리튬 구조체의 표면에 입금 됩니다. 이 예금은 일반적으로 (비교적) 균일 한 금속 레이어 (도금) 또는 작은 돌기 구조 형태를 가정합니다. 도금 자전거 성능을 방해에 안전 문제를 일으키는에서 배열 하는 효과 가질 수 있습니다. 현상 학적 관점에서 리튬 도금 호스트 전극 구조에 효과적으로 intercalate 리튬의 무 능력으로 인해 발생 합니다. 도금 낮은 온도, 높은 충전 속도, 충전 (SOC), 높은 전극 상태 또는 이러한 세 가지 요소12의 조합에서 발생 해 경향이 있다. 낮은 온도에서 고체 확산 전극 내부 온도에 Arrhenius 확산 의존 때문, 감소 된다. 낮은 고체 확산 리튬 전극-전해질 인터페이스에서의 리튬의 후속 증 착 결과. 높은 충전 속도로 비슷한 현상이 발생합니다. 리튬 전극 구조에 매우 신속 하 게 intercalate 시도 하지만 수 이며 따라서 도금입니다. 높은 SOC에 덜 사용 가능한 공간 구조, intercalate을 리튬에 대 한 평균입니다 그리고 따라서 더 유리한 표면에 입금 됩니다.
리튬 dendrites 그들이 발생할 안전 관심사 때문에 특별 한 중요성의 있습니다. 모 수석 세포 안에 형성, 그들 성장, 통과 하는 구분 기호, 양극과 음극 사이의 내부 짧은 발생 하는 가능성이 있다. 이 내부 짧은 매우 높은 지역화 온도 열 폭주에 셀의 폭발에도 자주 발생 하는 가연성 전해질에서 발생할 수 있습니다. 모 수석 형성에 관련 된 또 다른 문제는 반응 리튬의 증가 표면 영역입니다. 새로 입금된 리튬 전해질으로 반작용 하 고 증가 용량 감소와 사이클 성능 저하로 이어질 것입니다 증가 고체 전해질 interphase (SEI) 형성을 일으킬 것입니다.
3 전극 시스템의 설계와 관련 된 하나의 문제는 적절 한 참조 전극의 선택 이다. 물류 및 관련 된 위치 참조의 크기, 긍정적인, 부정적인 전극 시스템에서 정확한 결과 인수에 중요 한 역할을 재생할 수 있습니다. 한 예로 셀 및 결과 가장자리 효과 중 긍정적이 고 부정적인 전극의 부정합14,15을 읽고 참조에서 오류를 발생할 수 있습니다. 물자 선택의 점에서 참조 전극 해야 안정적이 고 신뢰할 수 있는 전압을가지고 있고 높은 비-polarizability. 종종 데 사용 되는 참조 전극으로 많은 연구 그룹에 의해, 리튬 금속 수동 표면 필름에 따라 잠재력이 있다. 청소 하기 때문에이 문제를 생산할 수 있는 고 세 리튬 전극 다른 후보16을 표시 합니다. 장기 노화 효과 공부 하는 경우 이것은 문제가 된다. Solchenbach 외에 의해 연구는 리튬 및 그들의 참고11로 그것을 사용 하 여 합금 골드 이러한 불안정성 문제를 제거 하려고 했습니다. 다른 연구는 리튬 타이타늄, 실험적으로 공부 하 고 주위 큰 전기 화학 잠재적인 고원 범위 표시를 포함 하 여 다른 재료를 쳐다보면서 1.5-1.6 V17 (~ 50 %SOC). 이 고원의 전극의 상태를 실수로 섭 동 경우 특히 안정적인 잠재력을 유지 하기 위해 도움이 됩니다. 탄소 기반 전도성 첨가제를 포함 하 여 LTO의 잠재적인 안정성도 다른 C-속도 온도에 유지 됩니다. 18 그것은 강조 하는 중요 한 기준 전극의 선택 3 전극 전지 설계에서 중요 한 단계 이다.
많은 연구 단체는 실험 3 전극 셀 설치를 제안 했다. Dolle 외. 사이클링과 높은 온도19스토리지 임피던스에 변화를 공부 하는 리튬 타이타늄 구리선 참조 전극 얇은 플라스틱 셀 사용. McTurk 외. 고용에 의하여 리튬 도금 구리 와이어 비 침 투 적인 삽입 기법9의 중요성을 설명 하 고 주요 목표와 상업적인 파우치 셀에 삽입 된 기술. Solchenbach 외. 수정된 Swagelok 형 T-세포와 (앞에서 언급 한) 골드 마이크로 참조 전극 임피던스 및 잠재적인 측정 사용. 11 Waldmann 외. 전극을 상용 셀에서 수확 하 고 리튬 증 착12공부에 사용 하기 위해 그들의 자신의 주머니 3 전극 셀을 재건. Costard 외 다른 기준 전극 재료 및 구성13의 효과 테스트 하는 사내 실험 3 전극 셀 주택 개발.
이 연구 그룹의 대부분 특히 장기간 사용으로 안정성 및 SEI 성장 우려를 가질 수 있습니다, 참고로 순수 리튬 금속을 사용 합니다. 다른 문제는 복잡 하 고 시간이 걸리는 기존 또는 상업적 설정에 대 한 수정 포함. 본이 논문에서는 그림 1에서 같이 전기 테스트에 대 한 3-전극 리튬 동전 세포를 건설 하기 위한 안정적이 고 비용 효율적인 기술 제공 됩니다. 이 3-전극 설치 표준 코인 셀 구성 요소, 구리 와이어, 및 리튬 타이타늄 기반 참조 전극 ( 그림 2참조)를 사용 하 여 생성할 수 있습니다. 이 메서드는 어떤 특수 장비 또는 정교한 수정 필요 하지 않습니다 하 고 상업용 공급 업체에서 표준 실험실 규모 전기 화학 절차와 자료를 다음과 같습니다.

<table><tbody><tr><td>Agate Mortar and Pestle</td><td>VWR</td><td>89037-492</td><td>5 in diameter</td></tr><tr><td>Die Set</td><td>Mayhew</td><td>66000</td><td></td></tr><tr><td>Laboratory Press</td><td>MTI</td><td>YLJ-12</td><td></td></tr><tr><td>Analytical Scale</td><td>Ohaus</td><td>Adventurer AX</td><td></td></tr><tr><td>High-Shear Mixing Device</td><td>IKA</td><td>3645000</td><td></td></tr><tr><td>Argon-filled Glovebox</td><td>MBraun</td><td>LABstar</td><td></td></tr><tr><td>Hydraulic Crimper</td><td>MTI</td><td>MSK-110</td><td></td></tr><tr><td>Battery Cycler</td><td>Arbin Instruments</td><td>BT2000</td><td></td></tr><tr><td>Potentiostat/Galvanostat/EIS</td><td>Bio-Logic</td><td>VMP3</td><td></td></tr><tr><td>Vacuum Oven and Pump</td><td>MTI</td><td>-</td><td></td></tr><tr><td>Copper Wire</td><td>Remington</td><td>PN155</td><td>32 AWG</td></tr><tr><td>Glass Balls</td><td>McMasterr-Carr</td><td>8996K25</td><td>6 mm borosilicate glass balls</td></tr><tr><td>Stirring Tube</td><td>IKA</td><td>3703000</td><td>20 ml</td></tr><tr><td>Celgard 2500 Separator</td><td>MTI</td><td>EQ-bsf-0025-60C</td><td>25 &amp;mu;m thick; Polypropylene</td></tr><tr><td>Stainless Steel CR2032 Coin Cell Kit</td><td>Pred Materials</td><td></td><td>Coin cell kit includes: case, cap, PP gasket</td></tr><tr><td>Stainless Steel Spacer</td><td>Pred Materials</td><td></td><td>15.5 mm diameter &amp;times; 0.5 mm thickness</td></tr><tr><td>Stainless Steel Wave Spring</td><td>Pred Materials</td><td></td><td>15.0 mm diameter &amp;times; 1.4 mm height</td></tr><tr><td>Li-ion Battery Anode - Graphite</td><td>MTI</td><td>bc-cf-241-ss-005</td><td>Cu Foil Single Side Coated by CMS Graphite (241mm L x 200mm W x 50&amp;mu;m Thickness)</td></tr><tr><td>Li-ion Battery Cathode - LiCoO&lt;sub&gt;2&lt;/sub&gt;</td><td>MTI</td><td>bc-af-241co-ss-55</td><td>Al Foil Single Side Coated by LiCoO&lt;sub&gt;2&lt;/sub&gt; (241mm L x 200mm W x 55&amp;mu;m Thickness)</td></tr><tr><td>Polyvinylidene Difluoride (PVDF)</td><td>Kynar</td><td>Flex 2801</td><td></td></tr><tr><td>N-Methyl-2-Pyrrolidinone Anhydrous (NMP), 99.5%</td><td>Sigma Aldrich</td><td>328634</td><td></td></tr><tr><td>CNERGY Super C-65</td><td>Timcal</td><td></td><td></td></tr><tr><td>Electrolyte (1.0 M LiPF&lt;sub&gt;6&lt;/sub&gt; in EC/DEC, 1:1 by vol.)</td><td>BASF</td><td>50316366</td><td></td></tr><tr><td>Lithium Titanate (Li&lt;sub&gt;4&lt;/sub&gt;Ti&lt;sub&gt;5&lt;/sub&gt;O&lt;sub&gt;12&lt;/sub&gt;)</td><td>Sigma Aldrich</td><td>702277</td><td></td></tr><tr><td>KS6 Synthetic Graphite</td><td>Timcal</td><td></td><td></td></tr><tr><td>Lithium Metal Ribbon</td><td>Sigma Aldrich</td><td>320080</td><td>0.75 mm thickness</td></tr><tr><td>Epoxy Multipurpose</td><td>Loctite</td><td></td><td></td></tr><tr><td>Electrical Tape</td><td>Scotch 3M Super 88&amp;nbsp;</td><td></td><td></td></tr><tr><td>Isopropyl Alcohol (IPA), ACS reagent, &amp;ge;99.5%</td><td>Sigma Aldrich</td><td>190764</td><td></td></tr></tbody></table>

three-electrode coin cell preparation and electrodeposition analytics for lithium-ion batteries

리튬-이온 배터리 찾아 사용 높은 에너지 및 전력 응용 프로그램에서와 같은 전기 및 하이브리드 전기 자동차에 점점 더 중요 해지고 저하 문제와 후속 안전 모니터링. 리튬 이온 셀 설정에서 포지티브 및 네거티브 터미널에서 전압 측정은 본질적으로 결합 하는 음극과 양극의 효과 및 합계 총 셀 성능에 포함 됩니다. 따라서, 특정 전극과 관련 된 저하 측면을 모니터링 하는 능력은 전극은 근본적으로 결합 하기 때문에 매우 어렵습니다. 3 전극 설치가이 문제를 극복할 수 있다. 세 번째 (참조) 전극, 도입 하 여 각 전극의 영향을 분리 될 수 있다, 그리고 독립적으로 측정 하는 전기 속성 될 수 있다. 다음 측정 될 수 있다 알려진된 참조에 대 한 예를 들어 안정 된 잠재력, 리튬 금속 기준 전극 (RE)가 있어야 합니다. 3 전극 셀은 순환, 순환 voltammetry, 그리고 전기 화학 임피던스 분광학 (EIS) 등 전기 테스트를 실행 하려면 사용할 수 있습니다. 3 전극 셀 EIS 측정 전체 셀을 개별 전극 임피던스의 기여를 명료 하 게 수 있습니다. 또한, 잠재적인 양극 모니터링 때문에 안전 문제를 일으킬 수 있는 리튬 도금 electrodeposition 감지 수 있습니다. 이것은 특히 빠른 전기 자동차에서 리튬 이온 배터리의 충전에 대 한 중요입니다. 모니터링 하 고 특성의 전기 화학 셀 안전과 저하 측면, 3 전극 설치 귀중 한 증명할 수 있다. 이 종이 3-전극 동전 셀 설치 이며 쉽게 생산, 신뢰성, 비용 효율적인 2032-코인 셀 아키텍처를 사용 하 여 생성 하는 지침을 제공 하는 것을 목표로.

전압에 대 한 일반적인 결과 3 전극 셀에 대 한 잠재적인 프로 파일은 그림 7에서 볼 수 있습니다. 이상적인 설치에서 전체 셀 전압 같은 전극 쌍을 사용 하 여 2 전극 셀에서 생산에 동일 해야 합니다. 이 참조 전극의 삽입은 셀의 성능 수정 여부를 확인 하려면 한 방법입니다. 2-3-전극 전체 셀 (동일 작업 및 성능 카운터 전극) 사이 상당한 차이가 있는 ...

Watch this Scientific Journal Video about Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries at JoVE.com

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

3 전극 셀은 리튬-이온 배터리의 전기 화학 공부에 유용 합니다. 이러한 전기 설치 현상을 음극 및 양극 분리 하 여 독립적으로 검사와 관련 된 수 있습니다. 여기, 선물이 리튬 도금 분석에 중점을 함께 건설 하 고 3-전극 코인 셀의 사용에 대 한 가이드.

3 전극 동전 전지 준비 및 Electrodeposition 리튬-이온 배터리에 대 한 분석

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

three-electrode-coin-cell-preparation-electrodeposition-analytics-for

Research

JoVE Journal

Engineering

36.5K 조회수.  Texas A&M University. 3 전극 셀은 리튬-이온 배터리의 전기 화학 공부에 유용 합니다. 이러한 전기 설치 현상을 음극 및 양극 분리 하 여 독립적으로 검사와 관련 된 수 있습니다. 여기, 선물이 리튬 도금 분석에 중점을 함께 건설 하 고 3-전극 코인 셀의 사용에 대 한 가이드.

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

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

건설과 리튬 이온 배터리의 동전 전지의 테스트

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

연구

공학

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 &deg;C), flammable, and volatile organic electrolytes. These organic based electrolyte systems are viable at ambient temperatures, but require a cooling system to ensure that temperatures do not exceed 80 &deg;C. These cooling systems tend to increase battery costs and can malfunction which can lead to battery malfunction and explosions, thus endangering human life. Increases in petroleum prices lead to a huge demand for safe, electric hybrid vehicles that are more economically viable to operate as oil prices continue to rise. Existing organic based electrolytes used in lithium ion batteries are not applicable to high temperature automotive applications. A safer alternative to organic electrolytes is solid polymer electrolytes. This work will highlight the synthesis for a graft copolymer electrolyte (GCE) poly(oxyethylene) methacrylate (POEM) to a block with a lower glass transition temperature (Tg) poly(oxyethylene) acrylate (POEA). The conduction mechanism has been discussed and it has been demonstrated the relationship between polymer segmental motion and ionic conductivity indeed has a Vogel-Tammann-Fulcher (VTF) dependence. Batteries containing commercially available LP30 organic (LiPF6 in ethylene carbonate (EC):dimethyl carbonate (DMC) at a 1:1 ratio) and GCE were cycled at ambient temperature. It was found that at ambient temperature, the batteries containing GCE showed a greater overpotential when compared to LP30 electrolyte. However at temperatures greater than 60 &deg;C, the GCE cell exhibited much lower overpotential due to fast polymer electrolyte conductivity and nearly the full theoretical specific capacity of 170 mAh/g was accessed.

Lithium ion batteries employ flammable and volatile organic electrolytes that are suitable for ambient temperature applications. A safer alternative to organic electrolytes are solid polymer batteries. Solid polymer batteries operate safely at high temperatures (&gt;120 &deg;C), thus making them applicable to high temperature applications such as deep oil drilling and hybrid electric vehicles. This paper will discuss (a) the polymer synthesis, (b) the polymer conduction mechanism, and (c) provide temperature cycling for both solid polymer and organic electrolytes.

리튬 배터리 애플리케이션을위한 고체 그래프트 공중 합체 전해질

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

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

방사광 기술을 사용하여 리튬 이온과 나트륨 이온 배터리 용 전극 재료의 특성

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

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.

제자리 중성자 분말 회절에서 사용자 정의 - 만든 리튬 이온 배터리를 사용하여

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.

싱크로 기반 하드 X 선 Microtomography를 사용하여 배터리의 실패 분석

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

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.

리튬 이온 코인 셀의 비수 전극 가공 및 건설

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

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

비 양성 자성 리튬 O의 전기 시험 프로토콜 및 특성<sub&gt; 2</sub&gt; 배터리

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

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.

이온 성 액체 기반 전해질의 합성 리튬 이온 배터리의 조립 및 고온에서의 성능 측정

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

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate multiple processes responsible for long-term performance decay. Given the complexity of physical processes occurring inside the cell, it is often challenging to achieve a full understanding of the root causes of this performance degradation. This difficulty arises in part from the fact that any electrochemical measurement of a battery will return the combined contributions of all components in the cell. Incorporation of a reference electrode can solve part of the problem, as it allows the electrochemical reactions of the cathode and the anode to be individually probed. A variation in the voltage range experienced by the cathode, for example, can indicate alterations in the pool of cyclable lithium ions in the full-cell. The structural evolution of the many interphases existing in the battery can also be monitored, by measuring the contributions of each electrode to the overall cell impedance. Such wealth of information amplifies the reach of diagnostic analysis in Li-ion batteries and provides valuable input to the optimization of individual cell components. In this work, we introduce the design of a test cell able to accommodate multiple reference electrodes, and present reference electrodes that are appropriate for each specific type of measurement, detailing the assembly process in order to maximize the accuracy of the experimental results.

The incorporation of reference electrodes in a Li-ion battery provides valuable information to elucidate degradation mechanisms at high voltages. In this article, we present a cell design that accommodates multiple reference electrodes, along with the assembly steps to assure maximum accuracy of the data obtained in electrochemical measurements.

원래의 Lithiated 참조 전극: 4 개의 전극 디자인-operando 임피던스 분광학에 대 한

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

화학

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.

그래 액체 셀 리튬-이온 배터리 재료의 관찰에 대 한 준비

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