Name: synthesis of ionic liquid based electrolytes, assembly of li-ion batteries, and measurements of performance at high temperature
Uploaded: 2016-12-20T13:00:00.000+00:00
Duration: 11 min 4 s
Description: Watch this Scientific Journal Video about Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature at JoVE.com

This article was supported in part by BU and by the Advanced Energy Consortium:

염화물 (CL)과 비스 (트리 플루오로 메탄) 술폰 (TFSI) 음이온과 짝 모노 및 디 - 포스 이온 성 액체의 1.Synthesis 주 : 세 헥실 포스 포늄 양이온을 둘러싸는 하나 데실 알킬 체인을 갖는 모노 포스 포늄 이온 성 액체에 대한 절차를 설명하고,이 이온 성 액체는 모노 HexC10Cl로 약칭된다. 동일한 과정을 높은 수율로 디 포스 포늄 이온 성 액체를 얻었다 1,10- dichlorodecane을 이용하여 반복하고,이 이온 성 액체는 디 HexC10Cl로 약칭된다. <ol><li> 아르곤 하에서 글러브 박스에있는 동안 trihexylphosphine (8.3 g, 29 mmol)을 유리 피펫을 사용을 달아 무거운 벽의 압력 용기에 분주. 다음에, 같은 용기로 유리 피펫을 사용하여 1 chlorodecane (5.22 g, 29.6 밀리몰)을 추가한다. PTFE를 부싱 혼합물을 함유하는 용기 캡. </li><li> 모노 HexC10Cl을 구하는 혼합하면서 24 시간 동안 140 ℃에서 아르곤하에, 생성 된 혼합물을 가열한다. 혼합물 것점성 온다. </li><li> 조 모노 - HexC10Cl를 얻기 위해 나머지 휘발성 출발 물질을 제거하기 위해 교반하면서 140 ℃에서 고 진공하에 혼합물을 놓는다. <ol><li> , 정제 1 약 10 mL를 사용하여 조 질의 혼합물로부터 모노 HexC10Cl을 추출하려면 250 ㎖의 분액 깔때기에 포화 염화나트륨 용액 (염수)로 1 디클로로 메탄 (DCM)을. DCM 단계를 수집합니다. 추출 과정을 세 번 반복합니다. </li><li> 생성물을 함유하는 수집 된 DCM 용액의 15 mL의 결합 및 모노 HexC10Cl 생성물을 얻기 위해 회전 증발기를 사용하여 용매를 증발시켰다. </li></ol></li><li> (6.25 g, 21.76 mmol)을 DCM 10ml에 (7.75 g, 16.74 mmol)을 모노 HexC10Cl을 용해 LiTFSI를 추가, 탈 이온수 10 ml의 사전은 용해. 생성 된 혼합물을 캡핑하고, 실온에서 24 시간 동안 저어. </li><li> DCM의 약 20 ㎖로 채워진 250 ml의 분별 깔때기를 사용하여 혼합물로부터 모노 - HexC10TFSI의 압축을 풉니 다. 의 EXT를 반복raction 과정을 세 번. DCM 솔루션을 결합합니다. </li><li> 유기상에서 염화 음이온의 완전한 제거를 확인하기 위해 1 N AGNO DCM 단계 1 ml의 3 용액을 1 ~ 2 방울을 추가합니다. 염화 음이온 용액에 남아있는 경우 백색 침전물이 생성됩니다. 더 흰색 침전물이 생성되지 않을 때까지 추출 단계를 반복합니다. </li><li> 의 DCM 용액에 무수 황산 1 g을 넣고 혼합 교반 한 후 건조 DCM 솔루션을 가만히 따르다. 이어서, 회전 증발에 의해 용매를 증발시켰다. 수율은 전형적으로 98 %보다 크다. </li><li> 높은 수율로 두 디 포스 포늄 이온 성 액체를 얻었다 1,10- dichlorodecane를 사용하여 동일한 방법으로, 디 - 및 디 HexC10Cl HexC10TFSI를 반복한다. </li><li> 1 H, 13 C, 그리고 중수 소화 클로로포름 19 F NMR을 (7.24 시프트)을 사용하여 이온 성 액체의 특성과 원소 분석 및 질량 분광 분석을위한 샘플을 제출한다. </li></ol> 2. CHARACT이온 액의 erization <ol><li> 시차 주사 열량계 (DSC) <ol><li> 이온 성 액체 (기록 실제 질량)의 5 ~ 10 mg의 칭량하고이어서 밀폐 된 알루미늄 샘플 팬의 중심에 추가. 이온 성 액체는 흡습성하고 방치하는 경우 무게가 변경됩니다 효율적으로이 단계를 완료해야합니다. </li><li> 샘플 팬과 시차 주사 열량계로의 언로드 (참조) 팬을로드합니다. 사용 된 특정 DSC의 결정에 따라 적절한 위치에 샘플 및 참조 팬을 배치해야합니다. </li><li> 프로그램 승온 사이클 냉각 : 10 ℃ / 분의 가열 속도로 200 ℃까지 -70 ℃ 내지 1) 열, 2) 5 ℃ / 분의 냉각 속도로 -70 ℃까지 쿨 3) 열 멋진 자전거를 세 번 반복한다. </li><li> 열 트레이스를 분석하여, 융점 (T m의) 결정 (T의 C)을 결정유리 전이 온도 (T g의) (적용 가능한 경우). </li></ol></li><li> 열 중량 분석 (TGA) <ol><li> 깨끗하고는 TGA의 가동 팔에 백금 팬 용기를. 팬에 이온 성 액체의 5 내지 10 mg을 추가합니다. 전용 핀셋을 사용하여 팬을 터치합니다. </li><li> 10 ℃ / 분의 가열 속도로 20 내지 500 ℃로 샘플을 가열한다. </li><li> 원래 샘플 중량의 10 %가 손실 분해 온도를 확인한다. 장기 안정성 시험의 경우, 연장 된 시간 동안 정해진 온도에서 샘플을 가열하고 중량 손실을 모니터링한다. </li></ol></li><li> 점도 측정 <ol><li> 유리 피펫으로 제어 변형 레오 미터의 펠티에 무대에서 이온 성 액체 1ml를 배치합니다. 알루미늄 플레이트가 완전히 이온 성 액체로 덮여 있는지 확인합니다. </li><li> 20 mm 직경의 평행 한 알루미늄 판 (또는 콘)을 사용하여 알루미늄 판 및 t의 상면 사이의 간격을 설정할런들의 모든 2.0 mm - 그는 1.0로 샘플. </li><li> 공기 중의 수분의 영향을 최소화하기 위해 질소 가스로 채워진 글로브 백에서 측정을 수행한다. </li><li> 앞서 각각의 시험하기 위해, 정상 상태에 도달하는 샘플 순서로 15 분 평형 단계로 수행 시료의 물리적 메모리를 제거하기 위해 10 초 동안 100 Hz의 전단 속도에서 샘플을 미리 전단. </li><li> 0.1 내지 10 %의 변형 크기와 고정 주파수 (Hz의 1)에서의 진동 스트레인 스윕 통해 선형 점탄성 영역 (LVR)을 결정한다. </li><li> LVR에있다 변형을 선택하고, 0.1 ~ 10 Hz에서까지 진동 주파수 스위프를 수행합니다. 특정 주파수 및 변형의 복잡한 점도를 결정합니다. </li><li> (10)로부터 구 소프트웨어에 의해 제어되는 진동형 온도 스위프를 수행 95 C를 ° (5)의 증가와 C를 ° ° C 각 온도에서 1 분간 평형. 변형 및 frequenc을 정의Y는, 예를 들어 각각 1.0 % 및 1 ㎐,한다. 서로 다른 온도에서 복잡한 점도가 판독된다. </li></ol></li><li> 전도도 측정 <ol><li> 실험 전에 수분의 미량을 제거하기 위해 12 시간 동안 고 진공하에 100 ℃에서 이온 성 액체를 건조. </li><li> 아르곤 분위기 하의 글로브 박스 내에서, 부하는 약 시험관에 시료 4 ㎖를 완전히 도전 프로브의 감지 테이프 젖어 충분한 샘플을 추가해야. </li><li> 온도 제어 및 균일 성을 유지하기 위해 측정 중에 교반을 유지하도록 가열 블록을 사용한다. </li><li> 30 분 평형 시간 후 각각의 온도에서의 전도도를 참조하십시오. </li></ol></li><li> 순환 전압 전류 법 (CV) <ol><li> 아르곤 대기하에 글로브 박스 내에서 리튬 / 리튬 / 백금 3 전극 계를 조립한다. </li><li> 이온 성 액체와 용기를 충전하고 모든 전극이 imme되어 있는지 확인이온 성 액체 rsed. 아르곤 하에서 용기를 밀봉합니다. </li><li> 20 분 동안 목적하는 온도로 평형화 용기. 1 MV / sec로 리튬 이온 / 리튬 대 V V -0.2 사이 6.5 잠재적 인 속도를 쓸어. </li></ol></li></ol> 전해질 3. 준비 <ol><li> 물에 미량의 제거를 보장하기 위해 엄격하게 교반하면서 밤새 80 ℃에서 고 진공하에 이온 성 액체를 건조. </li><li> 진공 오븐에서 3 일 동안 70 ° C에서 LiTFSI를 건조. </li><li> 글러브 박스에 무수 이온 성 액체와 LiTFSI를 염을 옮긴다. </li><li> 이온 성 액체를 추가합니다 (예를 들어, 모노 - HexC10TFSI, 4.50 g, 6.4 mmol) 및 LiTFSI를 교반 막대를 포함하는 오븐 건조 플라스크 (1.83 g, 6.4 mmol)을 첨가 하였다. 이 전해액에 대해 1.6 M의 농도를 얻기 위해 균질해질 때까지 혼합물을 밤새 교반 하였다. </li></ol> 리튬 이온 코인 셀 배터리 4. 제작 <ol><li> 아르곤 atmosp에서 글러브 박스에서여기서, 하나의 스프링 및 코인 셀의 하단 캡 한 스테인레스 스틸 디스크를 배치했다. 스테인레스 스틸 디스크에서 12.7 mm 직경의 LiCoO2 2 전극 (24 mg)을 놓는다. </li><li> 15 분 동안 핫 플레이트상에서 60 ℃에서 상기 제조 된 이온 성 액체 전해질의 세퍼레이터 (다공성 폴리 프로필렌 막)의 두 부분을 담근다. </li><li> 재료가 완전히 전해액 (≈ 0.5 ml)로 덮여 질 때까지는 LiCoO2 양극의 표면에 이온 성 액체 전해질을 추가한다. </li><li> 코인 셀의 중심에 전해액에 침지 세퍼레이터를 놓습니다. 이어서 세퍼레이터 상에 이온 성 액체 전해질 몇 방울 (몇 마이크로 리터)를 추가한다. </li><li> 글러브 박스에서, 12.7 mm의 직경을 갖는 리튬 금속 조각을 잘라. 세퍼레이터의 상단에 리튬 금속을 놓습니다. </li><li> 코인 셀을 캡과 글로브 박스 크림 퍼로 밀봉. </li><li> 글러브 박스에서 코인 셀을 전송하고 앞서 번째 개시 12 시간 동안 세포 휴식전자 배터리 / 전기 테스트합니다. </li></ol> 100 ℃에서 전지의 성능 5. <ol><li> 전기 테스트 스테이션에서 케이블 스레드 된 후면 벽에 작은 구멍이 100 ° C에서 동작하는 오븐 코인 셀을 놓는다. 전기 테스트 스테이션에 코인 셀을 연결합니다. </li><li> 30 분의 온도로 평형을 100 ° C에서 셀을 둡니다. </li><li> 전기 테스트 스테이션의 정전류 충전 - 방전 사이클을 선택합니다. 500 사이클 수를 설정합니다. </li><li> 500 μA 각 충전 후 0 V에서 4.2 V. 세트 60 초 휴식 시간에 전압 상한에 ​​충전 전류를 설정합니다. </li><li> 500 μA에 방전 전류 및 각 방전 후 0 V에서 3.0 V. 세트 60 초 휴식 시간에 전압 하한을 설정합니다. </li><li> 소프트웨어를 사용하여 500 μA의 전류로 4.2 V 3.0 V 사이를 충 방전 사이클을 시작한다. 충전 출력 AG 평가ainst 시간. </li></ol>

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Rev. 114, 11503-11618 (2014).</li><li>Sakaebe, H., Matsumoto, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=N-Methyl-N-propylpiperidinium+bis(trifluoromethanesulfonyl)imide+(PP13-TFSI)+-+novel+electrolyte+base+for+Li+battery.">N-Methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide (PP13-TFSI) - novel electrolyte base for Li battery.</a> Electrochem. Commun. 5, 594-598 (2003).</li><li>Paillard, E., 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=Electrochemical+and+Physicochemical+Properties+of+PY14FSI-Based+Electrolytes+with+LiFSI.">Electrochemical and Physicochemical Properties of PY14FSI-Based Electrolytes with LiFSI.</a> J. Electrochem. Soc. 156, A891-A895 (2009).</li><li>Tsunashima, K., Sugiya, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physical+and+electrochemical+properties+of+low-viscosity+phosphonium+ionic+liquids+as+potential+electrolytes.">Physical and electrochemical properties of low-viscosity phosphonium ionic liquids as potential electrolytes.</a> Electrochem. Commun. 9, 2353-2358 (2007).</li><li>Nakagawa, H., 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=Application+of+nonflammable+electrolyte+with+room+temperature+ionic+liquids+(RTILs)+for+lithium-ion+cells.">Application of nonflammable electrolyte with room temperature ionic liquids (RTILs) for lithium-ion cells.</a> J. Power Sources. 174, 1021-1026 (2007).</li><li>Fuller, J., Carlin, R. T., Osteryoung, R. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Room+Temperature+Ionic+Liquid+1-Ethyl-3-methylimidazolium+Tetrafluoroborate:+Electrochemical+Couples+and+Physical+Properties.">The Room Temperature Ionic Liquid 1-Ethyl-3-methylimidazolium Tetrafluoroborate: Electrochemical Couples and Physical Properties.</a> J. Electrochem. Soc. 144, 3881-3886 (1997).</li><li>Mun, J., 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=Electrochemical+stability+of+bis(trifluoromethanesulfonyl)imide-based+ionic+liquids+at+elevated+temperature+as+a+solvent+for+a+titanium+oxide+bronze+electrode.">Electrochemical stability of bis(trifluoromethanesulfonyl)imide-based ionic liquids at elevated temperature as a solvent for a titanium oxide bronze electrode.</a> J. Power Sources. 194, 1068-1074 (2009).</li><li>Garcia, B., Lavall&#233;e, S., Perron, G., Michot, C., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Room+temperature+molten+salts+as+lithium+battery+electrolyte.">Room temperature molten salts as lithium battery electrolyte.</a> Electrochim. Acta. 49, 4583-4588 (2004).</li><li>Lewandowski, A., &#346;widerska-Mocek, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquids+as+electrolytes+for+Li-ion+batteries-an+overview+of+electrochemical+studies.">Ionic liquids as electrolytes for Li-ion batteries-an overview of electrochemical studies.</a> J. Power Sources. 194, 601-609 (2009).</li><li>Gali&#324;ski, M., Lewandowski, A., St&#281;pniak, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquids+as+electrolytes.">Ionic liquids as electrolytes.</a> Electrochim. Acta. 51, 5567-5580 (2006).</li><li>Lin, X., 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=Thermally-responsive,+nonflammable+phosphonium+ionic+liquid+electrolytes+for+lithium+metal+batteries:+operating+at+100+degrees+celsius.">Thermally-responsive, nonflammable phosphonium ionic liquid electrolytes for lithium metal batteries: operating at 100 degrees celsius.</a> Chem. Sci. 6, 6601-6606 (2015).</li><li>Xu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonaqueous+Liquid+Electrolytes+for+Lithium-Based+Rechargeable+Batteries.">Nonaqueous Liquid Electrolytes for Lithium-Based Rechargeable Batteries.</a> Chem. Rev. 104, 4303-4418 (2004).</li><li>Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+solid+electrolytes-an+overview.">Polymer solid electrolytes-an overview.</a> Solid State Ionics. 9-10, 745-754 (1983).</li><li>Meyer, W. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+electrolytes+for+lithium-ion+batteries.">Polymer electrolytes for lithium-ion batteries.</a> Adv. Mater. 10, 439-448 (1998).</li></ol>

The authors declare that they have no competing financial interests.

불연성 및 고온 기능 리튬 이온 배터리를 개발하기 위해 우리의 접근 방식은 원형 동전 세포의 새로운 이온 성 액체 전해질의 합성 및 사후 평가를 포함한다. 구체적으로, 모노 - 및 디 HexC10TFSI HexC10TFSI 계 전해질은 리튬 금속 애노드는 LiCoO2 양극을 가진 코인 셀을 시험 하였다. 이 방법 내에서 중요한 단계는 다음과 같다 1) 설계 사양의 설정에 따라 리드 전해질을 식별; 2) 건조를 유지하여 ...

리튬 이온 배터리는 전기 에너지를 화학 에너지 사이의 에너지 변환 및 저장하고 수요와 온 - 더 - 이동 에너지를 제공하는 편리한 수단을 제공하는 장치입니다. 오늘날, 리튬 이온 전지는 그들의 높은 에너지 밀도와 재 대전의 휴대용 전자 기기 시장을 지배하고, 이러한 다운 - 홀 드릴링 및 자동차 등의 대형 및 특수 응용 프로그램에 대한 관심이다. 양극, 음극, 분리막, 전해질 : 1-5 배터리는 네 개의 주요 구성 요소로 구성된다. 두 전극의 화학 전지의 이론 에너지 밀도를 지시하지만, 안전성 및 작동 온도는 주로 전해질 재료에 의해 제한된다. 6-9 카보네이트 계 유기 용매에 전해질 (예를 들면, 디메틸 카보네이트 (DMC)와 에틸렌 카보네이트 (EC)가) 널리 인해 낮은 점도, 높은 도전성, 높은 리튬 염의 용해도에 리튬 이온 전지에 사용된다. 또한, 특정 combina카보네이트 계 용매 (DMC / EC) 등이있을 경우, 또한 이에 의해, 전해질과 전극과 연장 된 배터리 수명간에 분해 반응을 방지 안정한 고체 전해질 계면 (SEI)을 형성한다. 그러나 카보네이트 용매 단락이있을 때 잠재적으로 심각한 안전 문제, 55 ° C 이하로 리튬 이온 전지의 동작 온도가 제한 저비점 및 인화점 겪는다. 10, 11 이온 성 액체는 100 ℃ 이하의 온도를 용융 염 클래스이다. 전형적인 무기 염 달리 12, 이온 성 액체는 넓은 액체 범위를 갖고, 실온에서 액체 일 수있다. 이온 성 액체는 이미 다 졸리움, 포스 포늄, 피리 디늄, 암모늄 등의 하나 이상의 유기 양이온 중심으로 구성하며 methansulfonate, 헥사 플루오로 포스페이트, 또는 할라이드와 같은 무기 또는 유기 음이온과 쌍. 가능한 양이온과 음이온 조합 13, 14 넓은 다양한가변 특성을 갖는 많은 조성물을 허용한다. 또한, 이온 성 액체 내에서 강한 이온 성 상호 작용이 무시할 증기압, 불연성, 높은 열적 및 전기 화학적 안정성을 초래한다. (15, 16) 이온 성 액체가 통상의 전해질 장착 현재 리튬 - 이온 배터리의 고유 안전 문제를 해결하고, 고온 적용 할 수 있도록 하나의 해결책이다. 17-27 고온 응용을위한 이온 성 액체를 포함하는 리튬 이온 전지를 구성하는 데 사용되는 일반적인 합성 및 재료 처리 방법을 설명하기 위해, 우리는 합성, 열적 특성 및 페어링 모노 - 및 디 - 포스 포늄 이온 성 액체의 전기 화학적 특성을 설명 어느 염화물 (CL) 또는 비스 (트리 플루오로 메탄) 술폰 (TFSI) 음이온. 리튬 비스 (트리 플루오로 메탄) 술폰 상이한 농도 (LiTFSI를)는이어서 포스 포늄 이온 성 액체 비누에 첨가ID는 전해질을 제공합니다. 염화물 유사체에 비해 추가 LiTFSI를 가진 포스 TFSI 전해질의 성능에 기초하여, 코인 전지는 리튬 금속 애노드는 LiCoO2 양극과 함께 어느 모노 - 또는 디 - 포스 TFSI 전해질로 구성된다. 마지막으로, 전지 성능이 서로 다른 코인 셀 배터리를 100 ℃에서 평가된다. 이러한 실험을 수행에서 얻은 상세한 절차, 실행의 도전과 통찰력은 아래에 설명되어 있습니다.

<table><tbody><tr><td>Silicone oil</td><td>Sigma-Aldrich</td><td>85409</td><td></td></tr><tr><td>Potassium hydroxide</td><td>Sigma-Aldrich</td><td>221473</td><td>Corrosive</td></tr><tr><td>Rotary evaporator</td><td>Buchi</td><td>R-124</td><td></td></tr><tr><td>High-vacuum pump</td><td>Welch</td><td>8907</td><td></td></tr><tr><td>Nitrogen, ultra high purity</td><td>Airgas</td><td>NI UHP300</td><td>Compressed gas</td></tr><tr><td>Tetrahydrofuran, stabilized with BHT</td><td>Pharmco-Aaper</td><td>346000</td><td>Flammable. Dried before use.</td></tr><tr><td>Dichloromethane</td><td>Pharmco-Aaper</td><td>313000</td><td>Flammable, toxic.</td></tr><tr><td>Separatory funnel (1 L)</td><td>Fisher Scientific</td><td>13-678-606</td><td></td></tr><tr><td>Sodium sulfate</td><td>Sigma-Aldrich</td><td>239313</td><td></td></tr><tr><td>Ethanol, absolute</td><td>Pharmco-Aaper</td><td>111USP200</td><td>Flammable, toxic.</td></tr><tr><td>Buchner funnel</td><td>Fisher Scientific</td><td>FB-966-F</td><td></td></tr><tr><td>Methanol</td><td>Pharmco-Aaper</td><td>339000ACS</td><td>Flammable, toxic.</td></tr><tr><td>Triethylamine (anhydrous)</td><td>Sigma-Aldrich</td><td>471283</td><td>Toxic, flammable, harmful to environment</td></tr><tr><td>Glass syringe</td><td>Hamilton Company</td><td>1700-series</td><td></td></tr><tr><td>Deuterated chloroform</td><td>Cambridge Isotopes Laboratories, Inc.</td><td>DLM-29-10</td><td>Toxic</td></tr><tr><td>Nuclear magnetic resonance instrument</td><td>Varian</td><td>V400</td><td></td></tr><tr><td>Hydrogen</td><td>Airgas</td><td>HY HP300</td><td>Highly flammable.</td></tr><tr><td>Hexanes</td><td>Pharmco-Aaper</td><td>359000ACS</td><td>Toxic, flammable.</td></tr><tr><td>Differential scanning calorimeter</td><td>TA Instruments</td><td>Q100</td><td></td></tr><tr><td>&lt;em&gt;N,N&lt;/em&gt;-dimethylformamide</td><td>Sigma-Aldrich</td><td>227056</td><td>Toxic, flammable.</td></tr><tr><td>Trihexylphosphone</td><td>TCI America</td><td></td><td>Toxic, flammable.</td></tr><tr><td>1-Chlorodecane</td><td>Sigma-Aldrich</td><td></td><td>Toxic, flammable.</td></tr><tr><td>Bis(trifluoromethane)sulfonimide lithium salt</td><td>Sigma-Aldrich</td><td></td><td>Hydrophilic</td></tr><tr><td>1,10-dichlorodecane</td><td>Sigma-Aldrich</td><td></td><td>Toxic, flammable.</td></tr><tr><td>Thermal Gravemetric Analysis (TGA)</td><td>TA Q50</td><td>TA instruments</td><td></td></tr><tr><td>Differential scanning calorimeter (DSC)</td><td>TA Q100</td><td>TA instruments</td><td></td></tr><tr><td>Controlled Strain Rheometer</td><td>AR 1000&amp;nbsp;</td><td></td><td></td></tr><tr><td>Conductivity Meter&amp;nbsp;</td><td>Consort</td><td>K912</td><td>4-electrode cell</td></tr><tr><td>Potentiostat/Galvanostat</td><td>Princeton Applied Research&amp;nbsp;</td><td>VersaStat MC4&amp;nbsp;</td><td>Electrochemical testing</td></tr><tr><td>Separators</td><td>Celgard&amp;nbsp;</td><td>C480&amp;nbsp;</td><td>polypropylene/polyethylene</td></tr><tr><td>CR2032 coin cells</td><td>MTI Corp.</td><td>EQ-CR2032-CASE</td><td></td></tr><tr><td>LiCoO&lt;sub&gt;2&lt;/sub&gt; electrode&amp;nbsp;</td><td>MTI Corp.</td><td>EQ-CR2032</td><td>Cathode material</td></tr><tr><td>lithium metal&amp;nbsp;</td><td>Alfa Aesar</td><td>10769</td><td>Anode Material</td></tr><tr><td>Stainless Steel Spacer</td><td>MTI Corp.</td><td>EQ-CR20-Spacer304-02</td><td>15.5 mm Dia x 0.2 mm</td></tr><tr><td>Wave Spring</td><td>MTI Corp.</td><td>EQ-CR20WS-Spring304</td><td></td></tr><tr><td>Electric Coin Cell Crimping Machine</td><td>MTI Corp.</td><td>MSK-160D</td><td></td></tr><tr><td>Glove box</td><td>Mbraun</td><td></td><td>Water free, oxygen free operation</td></tr></tbody></table>

synthesis of ionic liquid based electrolytes, assembly of li-ion batteries, and measurements of performance at high temperature

전통적인 전해질의 화학적 불안정성은 리튬 이온 배터리로서 널리 사용되는 에너지 저장 장치의 안전 문제가 남아있다. 고온에서 작동하는 장치에서 사용하기위한 리튬 이온 전지는 열적 안정성 및 불연성 전해액을 필요로한다. 열적으로 안정한 용융 염, 비 휘발성, 불연성 이온 성 액체 (ILS)가 현재 현재 사용되는 가연성 및 저비점 유기 용매 전해질 이상적인 여분이다. 1) 클로라이드 또는 비스 (트리 플루오로 메탄) 술폰 (TFSI) 음이온과 짝 모노 및 디 - 포스 이온 성 액체를 합성, 우리는 여기하는 절차를 설명 2) 시차 주사 열량계 (DSC) 및 열 중량 분석 (TGA)에 의하여 이들 이온 성 액체의 성질 및 열적 안정성을 측정; 3) 사이 클릭 볼타 메 트리 (CV)에 의해 이온 성 액체의 전기 화학적 특성을 측정; 4) 리튬 비스 (트리 플루오로 메탄) 설폰 아미드를 포함하는 전해질을 준비; 5) 동시 측정온도의 함수로서 전해질 nductivity; 6) 리튬 금속 애노드와 캐소드는 LiCoO2와 함께 전해질이 함께 코인 전지 배터리의 조립; 7) 100 ℃에서 전지의 성능을 평가한다. 우리는 또한 이러한 실험을 수행에서 얻은 실행의 문제뿐만 아니라 통찰력을 설명합니다.

이온 성 액체, 모노 - 및 디 HexC10Cl HexC10Cl은 친 핵성 반응을 통해 제조하고, 후속 할라이드 교환 반응은 모노 - 및 디 HexC10TFSI HexC10TFSI 이온 성 액체를 각각 (도 1A)을 얻었다. 14 네 이온 성 액체는 무색의 약간 점성 액체 (그림 1B)를했다. 모노 HexC10TFSI 이온 성 액체의 대표적인 1 H NMR은도 1c에 도시 한 질량 분석 및 원소 분?...

Watch this Scientific Journal Video about Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature at JoVE.com

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

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 ...

synthesis-ionic-liquid-based-electrolytes-assembly-li-ion-batteries

Universidad San Sebastian

Research

JoVE Journal

Engineering

12.9K 조회수.  Boston University. 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.

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

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. ...

Ultrasound Velocity Measurement in a Liquid Metal Electrode

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently more difficult than measuring the flow of a transparent fluid, since optical methods are not applicable. Ultrasound can be used to measure the velocity of an opaque fluid, not only at isolated points, but at hundreds or thousands of points arrayed along lines, with good temporal resolution. When applied to a liquid metal electrode, ultrasound velocimetry involves additional challenges: high temperature, chemical activity, and electrical conductivity. Here we describe the experimental apparatus and methods that overcome these challenges and allow the measurement of flow in a liquid metal electrode, as it conducts current, at operating temperature. Temperature is regulated within &#177;2 &#176;C using a Proportional-Integral-Derivative (PID) controller that powers a custom-built furnace. Chemical activity is managed by choosing vessel materials carefully and enclosing the experimental setup in an argon-filled glovebox. Finally, unintended electrical paths are carefully prevented. An automated system logs control settings and experimental measurements, using hardware trigger signals to synchronize devices. This apparatus and these methods can produce measurements that are impossible with other techniques, and allow optimization and control of electrochemical technologies like liquid metal batteries.

Ultrasound velocimetry is used to study mixing by fluid flow in liquid metal electrodes. The focus of this manuscript is to illustrate the methods used for making precise, spatially-resolved ultrasound measurements while limiting oxidation and controlling and monitoring temperature, applied current, and the heater power being supplied.

액체 금속 전극의 초음파 속도 측정

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently ...

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 ...

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.

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 ...

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 ...

Identification and Quantification of Decomposition Mechanisms in Lithium-Ion Batteries; Input to Heat Flow Simulation for Modeling Thermal Runaway

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of thermal runaway (TR), the exothermic decomposition reactions in anode and cathode were studied, using a Simultaneous Thermal Analysis (STA)/Gas Chromatography-Mass Spectrometry (GC-MS)/Fourier Transform Infrared (FTIR) spectrometer system. These techniques allowed the identification of the reaction mechanisms in each electrode, owing to the analysis of evolved gaseous species, the amount of heat released and mass loss. These results provided insight into the thermal events happening within a broader temperature range than covered in previously published models. This allowed the formulation of an improved thermal model to depict TR. The heat of reaction, activation energy, and frequency factor (thermal triplets) for each major exothermic process at material level were investigated in a Lithium Nickel-Manganese-Cobalt-Oxide (NMC (111))-Graphite battery cell. The results were analyzed, and their kinetics were derived. These data can be used to successfully simulate the experimental heat flow.

This work aims at determining the reaction kinetics of Li-ion battery cathode and anode materials undergoing thermal runaway (TR). Simultaneous Thermal Analysis (STA)/Fourier Transform Infrared (FTIR) spectrometer/Gas Chromatography Mass Spectrometry (GC-MS) were used to reveal thermal events and to detect evolved gases.

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of ...