Name: protocol of electrochemical test and characterization of aprotic li-o2 battery
Uploaded: 2016-07-12T13:00:00.000+00:00
Duration: 8 min 18 s
Description: Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

Research at Argonne National Laboratory was funded by U.S. Department of Energy, FreedomCAR and Vehicle Technologies Office. Use of the Advanced Photon Source and research carried out in the Electron Microscopy Center at Argonne National Laboratory was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

사용하기 전에 모든 관련 물질 안전 보건 자료 (MSDS)를 참조하십시오. 이러한 합성에 사용되는 화학 물질 중 일부는 급성 독성 및 발암 성이다. 나노 물질은 대량의 대응에 비해 추가적인 위험이있을 수 있습니다. 공학적 관리 (흄 후드, 글러브 박스) 및 개인 보호 장비의 사용을 포함하는 나노 결정 반응을 수행 할 때 모든 적절한 안전 방법을 사용하십시오 (보안경, 장갑, 실험실 코트, 전체 길이 바지, 폐쇄 발가락 신발). 다음 절차 중 일부는 표준 공기가없는 처리 기술을 포함한다. 음극 재료 1. 합성 주 : 양극 활물질은 하나의 원자 층 증착 또는 습식 화학 반응에 의해 합성 할 수있다. <ol><li> 원자 층 증착 (ALD) <ol><li> 12 시간 동안 자성 교반 하에서 100 ml의 1 M KMnO 4 용액에 다공성 탄소 5 g의 분산. </li><li> 일 100 mg의 확산E는 ALD 악기 스테인리스 트레이 상에 카본 분말을 산화하고, 트레이 위에 스테인리스 메쉬 커버 클램프. </li><li> 30 분 동안 1 Torr의 압력에서 300 sccm의 초 고순도 질소 캐리어 가스의 연속적인 흐름하에 200 ℃에서 트레이에 카본 분말을 잡아. </li><li> 다음 전체 ALD주기에 카본 분말을 취급한다. 참고 :이 프로토콜의 전극 촉매의 예로서 팔라듐 나노 입자를 가져 가라. 시약의 특정 요구 사항에 따라 변경 될 수있다. 더 이상의 정제없이받은-모든 시약이 사용된다. <ol><li> 100 분 동안 200 ° C에서 팔라듐 헥사 플루오로 탄소 기재 (100 mg)을 (PD (hfac) [식중이, 99.9 %)을 노출. </li><li> 300 분 동안 1 Torr의 압력에서 300 sccm의 초 고순도 질소 캐리어 가스의 연속적인 흐름 트레이를 제거. </li><li> 100 분 동안 포르말린에 탄소 기판 (HCHO 37 중량. H 2 O의 %) 200 ° C에 노출됩니다. </li><li> 퍼지 t그는 300 분 동안 1 Torr의 압력에서 300 sccm의 초 고순도 질소 캐리어 가스의 연속적인 흐름 트레이. </li></ol></li><li> ALD 사이클을 반복 필요. 일반적으로 3-10 회 반복. </li></ol></li><li> 습식 화학 반응 참고 :이 프로토콜에서 전기의 예를 들어 철 나노 입자를 가져 가라. 시약의 특정 요구 사항에 따라 변경 될 수있다. 더 이상의 정제없이받은-모든 시약이 사용된다. <ol><li> 12 시간 동안 자성 교반 하에서 100 ml의 1 M KMnO 4 용액에 다공성 탄소 5 g의 분산. </li><li> 탈 이온수로 산화 탄소를 씻으십시오. </li><li> 유리 섬유 필터가 장착 된 플라스크로 세척하고 탄소를 필터링 한 다음 12 시간 동안 110 ℃의 오븐에서 건조시킨다. </li><li> 탈 이온수 100 ㎖에있는 말린 탄소를 분산하고 자기 교반 50ml을 1 g을 추가합니다. </li><li> 1 M NaOH 용액을 사용하여, 약 9 pH 값을 조정합니다. </li><li> 는 R 볶음5 시간 동안 슬러리를 esulting 후 유리 섬유 필터가 장착 된 플라스크로 슬러리를 필터. </li><li> 탈 물과 에탄올로 제품을 씻으십시오. 밤새 110 ℃의 오븐에서 건조시킨다. </li><li> 석영 튜브로에서 H 2 / 아르곤 혼합물 (4 % H 2)의 연속적인 흐름으로 450 ° C에서 제품을 열 - 처리한다. 5 시간 동안 100 ml / 분의 유속을 사용한다. </li></ol></li></ol> 전극과 전해질의 2. 준비 <ol><li> 음극 <ol><li> 1 중량비 4 : 상기와 같은 제조 된 양극 재료 및 결착 된 폴리 (비닐 리덴 플루오 라이드) (PVDF)을 혼합한다. 주의 : 혼합물의 총 음극의 양에 의존한다. 각 부분에 음극 물질의 로딩은 0.1 mg의 범위이다. </li><li> 상기 혼합물에 1- 메틸 -2- 피 롤리 디논 (NMP)를 첨가하고, 균일 한 슬러리 질감을 잘 교반한다. 혼합물의 약 3 배의 무게에 NMP를 추가합니다. </li><li> 카르 보 위에 코트 슬러리100 μm의 주위에 두께 닥터 블레이드에 의해 N 용지. </li><li> 하룻밤 동안 100 ℃에서 진공 오븐에서 건조시켜 적층 체. </li><li> 7/16 인치 직경 구멍을 펀치로 디스크에 적층 체를 펀치하고 무게. </li></ol></li><li> 비 양성 자성 전해질 <ol><li> 하룻밤 동안 100 ℃에서 진공 오븐에서 건조, 리튬 트리 플루오로 메탄 술포 네이트 (SO 3 LiCF 3). </li><li> 테트라 에틸렌 글리콜 디메틸 에테르 SO 3 LiCF 3 건조 추가 상기 염이 용해 될 때까지 1 몰 / L의 농도로 (TEGDME H 2 O ~ 10 PPM)를 다음 자기 교반으로 용액을 교반한다. </li><li> 아르곤 가득 글로브 박스에 전해질을 유지합니다. </li></ol></li><li> 양극 <ol><li> 7/16 인치의 직경에 구멍 구멍을 뚫는와 디스크에 리튬 포일 / 칩 펀치. </li></ol></li></ol> 3. 전기 테스트 <ol><li> 은 Swagelok 셀의 조립 &lt;&gt; / 강해 참고 : 어셈블리의 모든 단계는 3.1.9를 제외하고, 아르곤으로 채워진 글로브 박스에 운영됩니다. <ol><li> 도 1a에 도시 된 바와 같이은 Swagelok 세트를 조립한다. 양극의 단부를 조여, 상기 캐소드 단부를 풀고. </li><li> 애노드 단부의 스테인레스로드의 상부에 리튬 금속 칩 (직경 7/16 인치) 조각을 넣고. </li><li> 리튬 금속 애노드의 상부에 유리 섬유 세퍼레이터 (직경 1/2 인치) 조각을 넣고. </li><li> 완전히 유리 섬유 분리기 젖은 전해질의 5-7 방울을 추가합니다. 부드럽게 거품을 제거하기 위해 분리를 누릅니다. </li><li> 애노드 대향 활물질, 습윤 분리기의 상부에 음극의 조각을 넣어. </li><li> 알루미늄 메쉬 (직경 7/16 인치)의 조각과 음극을 커버. </li><li> 눌러 알루미늄 튜브 위에서 언급 한 층은 다음 음극 끝을 조입니다. </li><li> 유리 챔버는 Swagelok 전체 셀을 밀봉하고, 도시 된 바와 같이, 클램프와 상기 챔버를 해결 <st룽&gt; 그림 1. </li><li> 글러브 박스에서 전체 셀을 가져 가라. 초 고순도 산소 탱크 유리 챔버를 연결하고, 30 분 동안 1 기압의 압력에서 산소 연속 흐름과 퍼지. </li></ol></li><li> 배터리 성능 테스트 <ol><li> 25 ° C까지 온도 조절 장치를 설정합니다. </li><li> 온도 조절 장치로 세포와 전극 (케이블로 기기에 연결된 전자 클립)를 넣고, 그 문제를 해결. </li><li> 전자 클립 대응 유리 실에 음극과 양극을 클립. </li><li> 배터리 테스트 시스템의 운영 소프트웨어를 열고 케이블로 연결 채널을 선택합니다. </li><li> 전기 테스트 절차를 설정합니다. 참고 : 100mA / g 활성 물질의 전류 밀도를 설정하고 2.2-4.5 V.의 전압 범위 <ol><li> 방전 시험 2.2 V의 방전 차단 전압을 설정합니다. </li><li> 용량 제어 사이클 시험 5 또는 10 시간의 방전 / 충전 단계-시간을 설정합니다. </리&gt; <li> 전압 제어 사이클 시험을 4.5 V 2.2 V와 전하 차단 전압의 방전 차단 전압을 설정한다. </li></ol></li><li> 소프트웨어 인터페이스에서 &quot;실행&quot;버튼을 클릭하여 절차를 실행합니다. </li></ol></li><li> 분해 셀의 청소 <ol><li> 글로브 박스에 세포를 분해. </li><li> 다음과 같은 특성화를 위해 유리 병에 전극을 유지합니다. 글러브 박스에서 다른 세포 부품을 전송합니다. </li><li> 비이커에 아세톤 용액 (~ 20 %) 또는 탈 이온수은 Swagelok 부품 스테인리스 막대, 알루미늄 튜브, 및 알루미늄 메쉬를 넣고 15-30 분간 초음파로 세척. </li><li> 60 ~ 80 ℃로 설정된 온도에서 부품 및 유리 챔버를 건조. </li></ol></li></ol> 특성 표본 4. 준비 주 : 시험편 (같이 제조 된 물질에 대해)을 후드에 제조 또는 글로브 박스는 공기를위한 AR (가득민감한 표본). <ol><li> SEM 및 XPS에 대한 표본 <ol><li> 샘플 단계에 탄소 막대기 테이프. 카본 테이프 시료 편으로서 시료 스테이지만큼 크거나 작게 할 수있다. </li><li> 5mm 약 2 시료의 조각을 절단하고 카본 테이프를 부착. 주 : 표본이 아닌 자기 샘플이 될 수 있습니다. 전기 시험 후 시험편의 경우, 탄소 테이프 스틱 전에 전해질 용매로 씻는다. </li><li> 측정 전에 메이슨 항아리에 공기에 민감한 시료를 밀봉합니다. </li><li> 제조업체의 지시에 따라 SEM 34-36 또는 XPS 37, 38을 운영하고 있습니다. </li></ol></li><li> TEM에 대한 표본 <ol><li> 시료 분말 밀 1 밀리그램. 전극 표본은 밀링 전에 탄소 종이를 활성 물질을 긁어 참고. </li><li> 구리 그리드에 샘플 분말을로드하고, 루즈 파우더를 제거합니다. </li><li> 구리 g을로드TEM의 샘플 홀더에 제거. 참고 : 공기에 민감한 샘플에 대한 가능한 한 빨리 수행이 단계를 가져옵니다. </li><li> TEM을 수행합니다. 39 ~ 41을 </li></ol></li><li> 고 에너지 XRD에 대한 표본 <ol><li> 분말 표본 <ol><li> 점토 또는 접착제로 폴리이 미드 튜브의 일단을 밀봉. </li><li> 튜브에 파우더를 넣습니다. </li><li> 튜브의 다른 쪽 끝을 밀봉합니다. </li></ol></li><li> 디스크 시편 참고 : 전극의 활성 물질을 측정하기 위해, 또 다른 옵션은 탄소 종이를 긁어 단계 4.3.1을 따르는 것입니다. <ol><li> 폴리 아미드 테이프의 조각 샘플 조각을 밀봉합니다. 테이프의 일 부분의 중간에 샘플을 넣고, 테이프의 다른 조각을 감싸는 밀봉. , 전기 시험 후의 시험편의 경우 밀봉하기 전에 전해질 용매로 세척 :합니다. </li></ol></li><li> 고급 pH의 고 에너지 XRD 42-44를 작동아르곤 국립 연구소 (Argonne National Laboratory)에서 oton 소스. </li></ol></li><li> XANES에 대한 표본 <ol><li> 파우더 샘플 <ol><li> 측정 된 원소의 농도가 묽은 제로 블랙 질화 붕소 (BN) 또는 카본을 사용하여, 높은 경우에는 샘플을 희석한다. 여기에, 3 ~ 5 중량 희석. %. </li><li> , 7mm의 직경 약 1mm의 두께로 디스크에 파우더를 눌러 KBr을 보도 자료를 사용 7mm은 다이 세트. </li><li> 윈도우 필름 디스크 인감. </li></ol></li><li> 디스크 시편 <ol><li> 윈도우 필름으로 표본을 밀봉합니다. </li></ol></li><li> 고 에너지는 아르곤 국립 연구소 (Argonne National Laboratory)의 고급 광자 소스에서 45-47 XANES 작동합니다. </li></ol></li><li> ATR-FTIR에 대한 표본 <ol><li> 전에 측정 한 후 다이아몬드 감쇠 전반사 (ATR) 장치를 청소합니다. </li><li> 관심있는 모든 샘플에 대한 다이아몬드 장치에 시료를 넣어. </li><li> 수행 ATR-FTIR 분석. 48, 49 </li></ol></li><li> 라만 스펙트럼에 대한 표본 <ol><li> 평평한 기판 상에 시료를 넣고 (유리, 스테인레스 스틸, 등.). </li><li> 커버 슬라이드 표본을 커버. </li><li> 공기에 민감한 샘플 세트를 밀봉합니다. </li><li> 라만 분광법을 수행합니다. 50, 51 </li></ol></li></ol>

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The authors have nothing to disclose.

공기 리튬 O 2 전지 시스템의 감도, 특히 이산화탄소 및 수분을 고려하여, 프로토콜의 단계는 많은 간섭 물질을 감소시키고 부반응을 방지하기 위해 필요하다. 예를 들어,은 Swagelok 형 셀이 O &lt;0.5 ppm을 H 2 O &lt;0.5 ppm으로 Ar에로 채워진 글로브 박스에 조립되고 모든 양극 활물질, 전해액 용매 및 염, 유리 섬유는 Swagelok 부 및 유리 챔버는 수분 오염을 감소시키기 위?...

1996 년 아브라함 지앙 1은 다공질 탄소 양극, 유기 전해질과 리튬 금속 음극으로 이루어진 제 가역 비 수계 리튬 전지 O 2를보고 하였다. 그 이후로 인해 다른 기존의 에너지 저장 시스템의 초과의 매우 높은 이론 에너지 밀도로, 양극에서 리튬의 산화에 의해 전류의 흐름과 캐소드에서 산소의 환원 (유도 리튬 O 2 배터리 전체 반응 리튬 + + O 2 + 전자 - ↔ 리튬 2 O 2), 최근에 상당한 관심을 받고있다 1-8. 다음과 같은 요구 사항이있는 음극 재료는 리튬 O의 고성능의 요구에 대한 수용 할 수있을 것 2 배터리 (1) 빠른 산소 확산; (2) 우수한 전기 전도도를; (3) 높은 비 표면적 (4) 안정성. 두 양극의 표면적 및 다공도가 중요하다. 리튬 O 2 배터리 전기 성능 9-12 다공성 구조는 O 2 리튬 양이온의 반응으로부터 생성 된 고체 방전 생성물의 증착을 허용; 큰 표면적은 전기 화학 반응을 촉진 전기 촉매 입자를 수용하기 위해 더 많은 활성 부위를 제공한다. 이러한 전극 촉매는 13-17. 기판의 원래 다공성 표면 구조의 보존과, 기판과 촉매 입자를 잘 제어 강한 접착을 제공하는 소정의 증착 방법에 의해 양극 재료에 첨가하는 것과 같이 제조 된 물질은 시험 프로톤 리튬 O이 전지의 음극으로는 Swagelok 형 셀이다. 그러나, 전지의 성능뿐만 아니라 캐소드 물질의 성질에 의존하지만, 또한, 비 양성 자성 전해질 18-22 및 리튬 금속 애노드의 유형. 23-26 더 영향 양과 물질의 농도 및 포함 피충전 / 방전 시험에 사용 rocedure. 적절한 조건으로 프로토콜 최적화 전지 재료의 전체적인 성능을 향상시킬 것이다. 전기 화학적 시험 결과뿐만 아니라, 전지 성능은 깨끗한 물질 및 반응 생성물의 특성을 평가할 수있다. 27-33 주사 전자 현미경 (SEM)을 양극 재료 및 형태의 표면 미세 구조를 조사하기 위해 사용 방전 제품의 진화. 투과 전자 현미경 (TEM) 에지 구조 (XANES) 근처의 X 선 흡수, 및 X 선 광전자 분광법 (XPS)은 특히 나노 촉매 입자의 위해 요소의 미세 구조, 화학적 상태 및 구성을 결정하는데 사용될 수있다. 고 에너지의 X 선 회절 (XRD)을 직접 토출 성 제품을 식별하기 위해 사용된다. 가능한 전해질 분해 감쇄 전반사 푸리에 변환에 의해 결정될 수 변환적외선 (ATR-FTIR) 라만 스펙트럼. 이 문서에서는 자연 그대로의 재료와 반응 생성물의 전지 재료 및 부속품의 제조, 전기 화학적 성능 테스트 및 특성화를 포함한 비 양성 자성 리튬 O 2 배터리의 일상적인 시험의 체계적이고 효율적인 배치를 보여주는 프로토콜입니다. 자세한 비디오 프로토콜 분야의 새로운 실무자 리튬 O 2 배터리의 성능 테스트 및 특성화와 관련된 많은 일반적인 함정을 방지하기위한 것입니다.

<table><tbody><tr><td>1-Methyl-2-pyrrolidinone (NMP), 99.5%</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>Battery test system</td><td>MACCOR</td><td>Series 4000 Automated Test System</td><td></td></tr><tr><td>Dimethyl carbonate (DMC), &amp;ge;99%</td><td>Sigma-Aldrich</td><td>517127</td><td></td></tr><tr><td>Ethyl alcohol, &amp;ge;99.5%</td><td>Sigma-Aldrich</td><td>459844</td><td></td></tr><tr><td>Formaldehyde solution, 37 wt. % in H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>252549</td><td></td></tr><tr><td>Graphitized Carbon black, &gt;99.95%</td><td>Sigma-Aldrich</td><td>699632</td><td></td></tr><tr><td>Iron(III) chloride (FeCl&lt;sub&gt;3&lt;/sub&gt;), 97%</td><td>Sigma-Aldrich</td><td>157740</td><td></td></tr><tr><td>Kapton polyimide tubing</td><td>Cole-Parmer</td><td>EW-95820-09</td><td></td></tr><tr><td>Kapton polymide tape</td><td>Cole-Parmer</td><td>EW-08277-80</td><td></td></tr><tr><td>Kapton window film</td><td>SPEX Sample Prep</td><td>3511</td><td></td></tr><tr><td>Lithium Chip (99.9% Lithium)</td><td>MTI Corporation</td><td>EQ-Lib-LiC25</td><td></td></tr><tr><td>Lithium trifluoromethanesulfonate (LiCF&lt;sub&gt;3&lt;/sub&gt;SO&lt;sub&gt;3&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>481548</td><td></td></tr><tr><td>Palladium hexafluoroacetylacetonate (Pd(hfac)&lt;sub&gt;2&lt;/sub&gt;), 99.9%</td><td>Aldrich</td><td>401471</td><td></td></tr><tr><td>Poly(vinylidene fluoride) (PVDF)</td><td>Aldrich</td><td>182702</td><td></td></tr><tr><td>Potassium permanganate (KMnO&lt;sub&gt;4&lt;/sub&gt;), &amp;ge;99.0%&amp;nbsp;</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Sodium hydroxide (NaOH), &amp;ge;97.0%</td><td>Sigma-Aldrich</td><td>221465</td><td></td></tr><tr><td>Tetraethylene glycol dimethyl ether (TEGDME), &amp;ge;99%</td><td>Aldrich</td><td>172405</td><td></td></tr><tr><td>Toray 030 carbon paper</td><td>ElectroChem Inc.</td><td>590637</td><td></td></tr></tbody></table>

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.

도 1a는 리튬 전지 O이 시험은 Swagelok 형 전지의 구성도이다. 리튬 필름의 한 조각 애노드 단부에 스테인리스 스틸 막대 상에 배치된다. 다공성 음극 알루미늄 튜브를 통해 순수한 O 2 열려 있습니다. 유리 섬유 세퍼레이터 및 비 양성 자성 전해질의 흡수제로 사용된다; 알 메쉬는 전류 집 전체로 사용된다. 전체는 Swagelok 형 셀은 초 고순도 산소?...

Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

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 ...

protocol-electrochemical-test-characterization-aprotic-li-o2

Universidad San Sebastian

Research

JoVE Journal

Engineering

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

11.4K 조회수.  Argonne National Laboratory. 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. 

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

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

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. ...

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 ...

A Protocol for Electrochemical Evaluations and State of Charge Diagnostics of a Symmetric Organic Redox Flow Battery

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid and deployment of renewable energy technologies. Among the many flow battery chemistries, non-aqueous flow batteries have the potential to achieve high energy density because of the broad voltage windows of non-aqueous electrolytes. However, significant technical hurdles exist currently limiting non-aqueous flow batteries to demonstrate their full potential, such as low redox concentrations, low operating currents, under-explored battery status monitoring, etc. In an attempt to address these limitations, we recently reported a non-aqueous flow battery based on a highly soluble, redox-active organic nitronyl nitroxide radical compound, 2-phenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (PTIO). This redox material exhibits an ambipolar electrochemical property, and therefore can serve as both anolyte and catholyte redox materials to form a symmetric flow battery chemistry. Moreover, we demonstrated that Fourier transform infrared (FTIR) spectroscopy could measure the PTIO concentrations during the PTIO flow battery cycling and offer reasonably accurate detection of the battery state of charge (SOC), as cross-validated by electron spin resonance (ESR) measurements. Herein we present a video protocol for the electrochemical evaluation and SOC diagnosis of the PTIO symmetric flow battery. With a detailed description, we experimentally demonstrated the route to achieve such purposes. This protocol aims to spark more interests and insights on the safety and reliability in the field of non-aqueous redox flow batteries.

We present the protocols for electrochemically evaluating a symmetric non-aqueous organic redox flow battery and for diagnosing its state of charge using FTIR.

전기 평가 및 대칭 유기 산화 환원 흐름 배터리의 충전 진단의 상태에 대한 프로토콜

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid ...

화학

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 ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

집중 된 이온 빔 제작 현장에서 테스트 LiPON 기반 고체 리튬-이온 Nanobatteries

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

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 ...

The Effect of Charging and Discharging Lithium Iron Phosphate-graphite Cells at Different Temperatures on Degradation

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. The degradation of the cells is assessed by using 10 charging and discharging temperature permutations ranging from -20 &#176;C to 30 &#176;C. This allows an analysis of the effect of charge and discharge temperatures on aging, and their associations. A total of 100 charge/discharge cycles were carried out. Every 25 cycles a reference cycle was performed to assess the reversible and irreversible capacity degradation. A multi-factor analysis of variance was used, and the experimental results were fitted showing: i) a quadratic relationship between the rate of degradation and the temperature of charge, ii) a linear relationship with the temperature of discharge, and iii) a correlation between the temperature of charge and discharge. It was found that the temperature combination for charging at +30 &#176;C and discharging at -5 &#176;C led to the highest rate of degradation. On the other hand, the cycling in a temperature range from -20 &#176;C to 15 &#176;C (with various combinations of temperatures of charge and discharge), led to a much lower degradation. Additionally, when the temperature of charge is 15 &#176;C, it was found that the degradation rate is nondependent on the temperature of discharge.

This article describes the effect of dissimilar charging/discharging temperatures on the degradation of lithium iron phosphate-graphite pouch cells, aiming at simulating close to real case scenarios. In total, 10 temperature combinations are investigated in the range -20 to 30 &#176;C in order to analyze the impact of temperature on degradation.

충전 및 방전 리튬 철 인산 염-흑연 셀 저하에 다른 온도에서 효과

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. ...

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 ...

비 양성 자성 리튬 O의 전기 시험 프로토콜 및 특성

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