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. 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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 border="0" cellpadding="0" cellspacing="0" width="653">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Silicone oil</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;">85409</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Potassium hydroxide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">221473</td>
			<td>Corrosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Rotary evaporator</td>
			<td style="width:108px;">Buchi</td>
			<td style="width:119px;">R-124</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">High-vacuum pump</td>
			<td style="width:108px;">Welch</td>
			<td align="right" style="width:119px;">8907</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Nitrogen, ultra high purity</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">NI UHP300</td>
			<td>Compressed gas</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Tetrahydrofuran, stabilized with BHT</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">346000</td>
			<td>Flammable. Dried through column of XXX</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Dichloromethane</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">313000</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Separatory funnel (1 L)</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">13-678-606</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Sodium sulfate</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">239313</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Ethanol, absolute</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">111USP200</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Buchner funnel</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">FB-966-F</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Methanol</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">339000ACS</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Triethylamine (anhydrous)</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">471283</td>
			<td>Toxic, flammable, harmful to environment</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glass syringe</td>
			<td style="width:108px;">Hamilton Company</td>
			<td style="width:119px;">1700-series</td>
			<td></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:259px;">Deuterated chloroform</td>
			<td style="width:108px;">Cambridge Isotopes Laboratories, Inc.</td>
			<td style="width:119px;">DLM-29-10</td>
			<td>Toxic</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Nuclear magnetic resonance instrument</td>
			<td style="width:108px;">Varian</td>
			<td style="width:119px;">V400</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Hydrogen</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">HY HP300</td>
			<td>Highly flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Hexanes</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">359000ACS</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Differential scanning calorimeter</td>
			<td style="width:108px;">TA Instruments</td>
			<td style="width:119px;">Q100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">N,N-dimethylformamide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">227056</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Trihexylphosphone</td>
			<td style="width:108px;">TCI America</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1-Chlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Bis(trifluoromethane)sulfonimide lithium salt</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Hydrophilic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1, 10-dichlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Thermal Gravemetric Analysis (TGA)</td>
			<td style="width:108px;">TA Q50</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Differential scanning calorimeter (DSC)</td>
			<td style="width:108px;">TA Q100</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Controlled Strain Rheometer</td>
			<td style="width:108px;">AR 1000&#160;</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Conductivity Meter&#160;</td>
			<td style="width:108px;">Consort</td>
			<td style="width:119px;">K912</td>
			<td>4-electrode cell</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;">Potentiostate/Galvanostat</td>
			<td style="width:108px;">Princeton Applied Research&#160;</td>
			<td style="width:119px;">VersaStat MC4&#160;</td>
			<td style="width:167px;">Electrochemical testing</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">Separators&#160;</td>
			<td style="width:108px;">Celgard&#160;</td>
			<td style="width:119px;">C480&#160;</td>
			<td style="width:167px;">polypropylene/polyethylene</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">CR2032 coin cells</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032-CASE</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">LiCoO2 electrode&#160;</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032</td>
			<td style="width:167px;">Cathode material</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">lithium metal&#160;</td>
			<td style="width:108px;">Alfa Aesar</td>
			<td align="right" style="width:119px;">10769</td>
			<td style="width:167px;">Anode Material</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Stainless Steel Spacer</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20-Spacer304-02</td>
			<td style="width:167px;">15.5 mm Dia x 0.2 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Wave Spring</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20WS-Spring304</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Electric Coin Cell Crimping Machine</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">MSK-160D</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glove box</td>
			<td style="width:108px;">Mbraun</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">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

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

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

극단적 인 압력과 온도에서 합성 부위 회절

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

액체 환경에서의 펄스 자외선 레이저 조사에 의한 실리콘 표면의 젖음성의 선택 영역 수정

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of ...

Research and Development of High-performance Explosives

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. For newly developed formulations, the process begins with small-scale mixes, thermal testing, and impact and friction sensitivity. Only then do subsequent larger scale formulations proceed to detonation testing, which will be covered in this paper. Recent advances in characterization techniques have led to unparalleled precision in the characterization of early-time evolution of detonations. The new technique of Photonic Doppler Velocimetry (PDV) for the measurement of detonation pressure will be shared and compared with traditional fiber-optic detonation velocity and plate-dent calculation of detonation pressure. In particular, the role of aluminum in explosive formulations will be discussed. Recent developments led to the development of explosive formulations that result in reaction of aluminum very early in the detonation product expansion. This enhanced reaction leads to changes in the detonation velocity and pressure due to reaction of the aluminum with oxygen in the expanding gas products.

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. This paper will share typical development tests associated with the measurement of detonation velocity and detonation pressure.

고성능 폭발물의 연구 개발

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance ...

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 ...

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The characteristics of the C84-embedded Si surface, such as atomic resolution topography, local electronic density of states, band gap energy, field emission properties, nanomechanical stiffness, and surface magnetism, were examined using a variety of surface analysis techniques under ultra, high vacuum (UHV) conditions as well as in an atmospheric system. Experimental results demonstrate the high uniformity of the C84-embedded Si surface fabricated using a controlled self-assembly nanotechnology mechanism, represents an important development in the application of field emission display (FED), optoelectronic device fabrication, MEMS cutting tools, and in efforts to find a suitable replacement for carbide semiconductors. Molecular dynamics (MD) method with semi-empirical potential can be used to study the nanoindentation of C84-embedded Si substrate. A detailed description for performing MD simulation is presented here. Details for a comprehensive study on mechanical analysis of MD simulation such as indentation force, Young&#39;s modulus, surface stiffness, atomic stress, and atomic strain are included. The atomic stress and von-Mises strain distributions of the indentation model can be calculated to monitor deformation mechanism with time evaluation in atomistic level.

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports the nanomaterial fabrication of a fullerene Si substrate inspected and verified by nanomeasurements and molecular dynamic simulation.

C 프로빙<sub&gt; (84)</sub&gt;은 스캐닝 프로브 현미경 및 분자 역학을 사용하여 실리콘 기판을 - 임베디드

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The ...

A High Performance Impedance-based Platform for Evaporation Rate Detection

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was employed here for demonstration purposes. Multiple evaporation tests on the model compound as a humectant with various concentrations in solutions were conducted for comparison purposes. A conventional weight loss approach is known as the most straightforward, but time-consuming, measurement technique for evaporation rate detection. Yet, a clear disadvantage is that a large volume of sample is required and multiple sample tests cannot be conducted at the same time. For the first time in literature, an electrical impedance sensing chip is successfully applied to a real-time evaporation investigation in a time sharing, continuous and automatic manner. Moreover, as little as 0.5 ml of test samples is required in this impedance-based apparatus, and a large impedance variation is demonstrated among various dilute solutions. The proposed high-sensitivity and fast-response impedance sensing system is found to outperform a conventional weight loss approach in terms of evaporation rate detection.

This paper presents an impedance-based apparatus for evaporation rate detection of solutions. It offers clear advantages over a conventional weight loss approach: a fast response, high-sensitivity detection, a small sample requirement, multiple sample measurements, and easy disassembly for cleaning and reuse purposes.

증발 속도 검출을위한 고성능 임피던스 기반 플랫폼

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was ...

Detecting the Water-soluble Chloride Distribution of Cement Paste in a High-precision Way

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a high-precision chloride profile. Firstly, paste specimens are molded, cured, and exposed to cyclic wet-dry conditions. Then, powder samples at different specimen depths are grinded when the exposure age is reached. Finally, the water-soluble chloride content is detected using a silver nitrate titration method, and chloride profiles are plotted. The key to improving the accuracy of the chloride distribution along the depth is to exclude the error in the powderization, which is the most critical step for testing the distribution of chloride. Based on the above concept, the grinding method in this protocol can be used to grind powder samples automatically layer by layer from the surface inward, and it should be noted that a very thin grinding thickness (less than 0.5 mm) with a minimum error less than 0.04 mm can be obtained. The chloride profile obtained by this method better reflects the chloride distribution in specimens, which helps researchers to capture the distribution features that are often overlooked. Furthermore, this method can be applied to studies in the field of cement-based materials, which require high chloride distribution accuracy.

A protocol for obtaining a water-soluble chloride profile by using a high precision milling method is presented.

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a ...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect of aggregate surface morphology on the formation of ITZ. First, a model concrete sample is prepared with a spherical ceramic particle in roughly the central part of the cement matrix, acting as a coarse aggregate used in common concrete/mortar. After curing until the designed age, the sample is scanned by X-ray computed tomography to determine the relative location of the ceramic particle inside the cement matrix. Three locations of the ITZ are chosen: above the aggregate, on the side of the aggregate, and below the aggregate. After a series of treatments, the samples are scanned with a SEM-BSE detector. The resultant images were further processed using a digital image processing method (DIP) to obtain quantitative characteristics of the ITZ. The surface morphology is characterized at the pixel level based on the digital image. Thereafter, K-means clustering method is used to illustrate the effect of surface roughness on ITZ formation.

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface roughness.

계면 전환 영역(ITZ)에서 골재 표면 형태 측정

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect ...

Fabrication and Design of Wood-Based High-Performance Composites

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber reinforced composites, due to its excellent mechanical properties. Delignified wood, however, is rather fragile in a wet state, which makes handling and shaping challenging. Here we present two fabrication processes, closed-mold densification and vacuum densification, to produce high-performance cellulose composites based on delignified wood, including an assessment of their advantages and limitations. Further, we suggest strategies for how the composites can be re-used or decomposed at the end-of-life cycle. Closed-mold densification has the advantage that no elaborate lab equipment is needed. Simple screw clamps or a press can be used for densification. We recommend this method for small parts with simple geometries and large radii of curvature. Vacuum densification in an open-mold process is suitable for larger objects and complex geometries, including small radii of curvature. Compared to the closed-mold process, the open-mold vacuum approach only needs the manufacture of a single mold cavity.

Delignified densified wood represents a new promising lightweight, high-performance and bio-based material with great potential to partially substitute natural fiber reinforced- or glass fiber reinforced composites in the future. We here present two versatile fabrication routes and demonstrate the possibility to create complex composite parts.

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber ...