[논문]증착 기법을 이용한 리튬이차전지용 초박막 세라믹 코팅 분리막 기술

김우철; 노영준; 최승엽; 이용민

doi:10.5229/jkes.2022.25.4.134

증착 기법을 이용한 리튬이차전지용 초박막 세라믹 코팅 분리막 기술
A Review on Ultrathin Ceramic-Coated Separators for Lithium Secondary Batteries using Deposition Processes 원문보기

전기화학회지 = Journal of the Korean Electrochemical Society, v.25 no.4, 2022년, pp.134 - 153

김우철 (대구경북과학기술원 에너지공학과) , 노영준 (대구경북과학기술원 에너지공학과) , 최승엽 (대구경북과학기술원 에너지공학과) , (대구경북과학기술원 에너지공학과) , 이용민 (대구경북과학기술원 에너지공학과)

초록
AI-Helper

리튬이온전지의 에너지밀도가 지속적으로 높아지고 사용환경이 가혹해지고 있지만, 전지의 안전성은 타협할 수 있는 특성이 아니다. 특히, 더 높은 에너지밀도 확보를 위해 고용량 전극 소재 개발과 함께 분리막 원단 뿐만 아니라 세라믹 코팅층의 두께 및 무게의 박막화와 경량화가 동시에 요구되고 있다. 그 중, 기존 슬러리 코팅 방식을 증착 방식으로 대체하는 기술이 주목받고 있으며, 분리막의 내열성 확보를 위해 도입된 수 ㎛ 수준의 세라믹 코팅층을 nm 수준으로 박막/경량화 하면서도 동등의 내열성을 확보하는 시도가 진행되고 있다. 증착법으로 제조된 세라믹 코팅 분리막은 리튬이온전지 에너지밀도를 크게 증가시킬 수 있는 효율적인 방법이지만, 균일한 물성의 세라믹 코팅 분리막을 제작하기 위해서는 증착 공정 중 온도를 제어해야 하며, 생산속도와 공정비용을 기존 슬러리 코팅 수준으로 떨어뜨려야 하는 현실적 문제가 존재한다. 그럼에도 불구하고, 분리막 원단 대비 두께 및 무게 증가가 거의 없다는 점에서는 전지의 고에너지밀도 달성에 필요한 매력적인 접근법임은 분명하다. 본 총설에서는 세라믹 증착 코팅에 사용되고 있는 세 가지 방법인 1) 화학적 기상 증착법, 2) 원자층 증착법, 그리고 3) 물리적 기상 증착법으로 제조된 세라믹 코팅 분리막을 소개하고자 한다. 각 증착법의 원리와 장/단점을 설명하고, 제조된 세라믹 코팅 분리막의 물리적, 전기화학적 특성 및 전지의 성능 변화를 비교 분석하였다. 또한, 소재 관점에서 금속 또는 유기물질이 코팅된 초박막 코팅 분리막의 기술 동향도 소개하였다.

Abstract ▼ AI-Helper

Regardless of a trade-off relationship between energy density and safety, it is essential to improve both properties for future lithium secondary batteries. Especially, to improve the energy density of batteries further, not only thickness but also weight of separators including ceramic coating layers should be reduced continuously apart from the development of high-capacity electrode active materials. For this purpose, an attempt to replace conventional slurry coating methods with a deposition one has attracted much attention for securing comparable thermal stability while minimizing the thickness and weight of ceramic coating layer in the separator. This review introduces state-of-the-art technology on ceramic-coated separators (CCSs) manufactured by the deposition method. There are three representative processes to form a ceramic coating layer as follows: chemical vapor deposition (CVD), atomic layer deposition (ALD), and physical vapor deposition (PVD). Herein, we summarized the principle and advantages/disadvantages of each deposition method. Furthermore, each CCS was analyzed and compared in terms of its mechanical and thermal properties, air permeability, ionic conductivity, and electrochemical performance.

주제어

표/그림 (20)

그림 Fig. 1. Classification and characteristics of thin film deposition process
그림 Fig. 2. Schematic diagrams of the key steps during (a) chemical vapor deposition (CVD). Reproduced with permission.²⁰⁾ Copyright 2003, Elsevier. and (b) atomic layer deposition (ALD) processes. Reproduced with permission.²²⁾ Copyright 2018, AIP Publishing.
그림 Fig. 4. Schematic diagrams for evaporation and sputtering processes. (a) Thermal evaporation (b) electron beam evaporation (c) direct current (DC) sputtering (d) radio frequency (RF) sputtering, and (e) magnetron DC or RF sputtering. Reproduced with permission.²⁵⁾ Copyright 2012, Elsevier.
그림 Fig. 3. Schematic diagrams of physical vapor deposition (PVD) processes. (a) Evaporation and (b) sputtering processes. Reproduced with permission.²⁴⁾ Copyright 2000, Elsevier.
그림 Fig. 5. (a) Schematic diagram of the SiO₂ thin film coated separator by CVD process and (b) its corresponding thermal shrinkage for various cycle numbers of CVD after storage at 150 °C for 20 min. Reproduced with permission.⁴⁷⁾ Copyright 2012, Elsevier.
그림 Fig. 6. (a) Schematic diagram of pHVDS thin film coated PE separator by iCVD process. (b[i]) SEM images of pristine and pHVDS-coated PE separators (b[ii]) their thermal shrinkage and (b[iii]) corresponding SEM images after storage at 140 °C for 30 min. (c) Rate performance tests for the cells with and without the pHVDS coating. (d) electrolyte wettability tests of the pristine separator and pHVDS-40 min PE. Reproduced with permission.⁴⁸⁾ Copyright 2015, American Chemical Society.
그림 Fig. 7. (a) Schematic diagram of Al₂O₃ thin film coated separator by ALD process and (b) photographs of bare and Al₂O₃ thin film coated separator s contacted with PC solvent and 1 M LiPF₆/PC. Reproduced with permission.⁵⁴⁾ Copyright 2012, John Wiley and Sons.
그림 Fig. 8. (a) Schematic diagram of the PE/Al₂O₃/PDA thin film separator. (b) SEM images of the surfaces and the corresponding cross-sectional views of bare PE, PE/Al₂O₃, and PE/Al₂O₃/PDA separators. Electrochemical measurements of the cells using the bare PE, PE/Al₂O₃, PE/PDA, and PE/Al₂O₃/PDA separators. (c) Comparison of the rate performance (0.2~5 C), Nyquist plots after the (d) 1^st cycle and (e) 200^th cycle. Reproduced with permission.⁵⁸⁾ Copyright 2019, Elsevier.
그림 Fig. 9. (a) Schematic diagram of Al₂O₃ R2R ALD process. (b) Cross section SEM image of Al₂O₃ film coated separator. (c) Tensile strength curves of Pristine (Celgard) and Al₂O₃ thin film coated (ALD-Celgard) separators. Reproduced with permission.⁵⁹⁾ Copyright 2020, John Wiley and Sons.
그림 Fig. 10. (a) Schematic diagram of TiO₂ R2R ALD process (b) TiO₂ thin film coated separators according to line speed (c) comparison of discharge capacity for TiO₂ thin film coated (ALD-T3) and pristine separators. Reproduced with permission.⁶⁰⁾ Copyright 2021, Elsevier.
그림 Fig. 11. (a) Schematic diagram and characteristics of Al₂O₃ thin film coated PVDF-HFP separator by ALD process and (b) galvanostatic cycling curves of Li/Li symmetric cells. Reproduced with permission.⁶³⁾ Copyright 2019, American Chemical Society.
그림 Fig. 12. SEM images of (a) bare and Al₂O₃ thin film coated PE separators after (b) 10 min (c) 40 min, and (d) 70 min sputtering and (e) their corresponding thermal shrinkage after storage at 150 °C for 30 min. Reproduced with permission.⁶⁴⁾ Copyright 2014, Springer Nature.
그림 Fig. 15. Characteristics of Al₂O₃ thin film coated separator by EB-evaporation process. (a) SEM images of PE, EB-PVD Al₂O₃-PE, commercial Al₂O₃-PE, and Al₂O₃-PI. Shutdown and breakdown behavior test: (b) In situ impedance measurement and (c) Post-mortem SEM images. Reproduced with permission.⁷²⁾ Copyright 2021, American Chemical Society.
그림 Fig. 14. (a) Schematic diagram of Al₂O₃/SiO₂ co-sputtering deposition setup and (b) electrochemical impedance spectroscopy (EIS) profiles of ME-PVDF, Al₂O₃/SiO₂/PVDF, Al₂O₃/PVDF, SiO₂/PVDF, and PE separators. Reproduced with permission.⁷¹⁾ Copyright 2019, American Chemical Society.
그림 Fig. 15. Characteristics of Al₂O₃ thin film coated separator by EB-evaporation process. (a) SEM images of PE, EB-PVD Al₂O₃-PE, commercial Al₂O₃-PE, and Al₂O₃-PI. Shutdown and breakdown behavior test: (b) In situ impedance measurement and (c) Post-mortem SEM images. Reproduced with permission.⁷²⁾ Copyright 2021, American Chemical Society.
그림 Fig. 16. Schematic diagram and characteristics of Cu thin film separator by sputtering process. Surface SEM images of (a) Bare PE and (b) PE/CuTF separator. (c) Cross-sectional SEM image of the as prepared PE/CuTF separator and (d) corresponding EDX mapping of the dotted square in panel (c). (e) Schematic diagram of Li metal deposition mechanism with the [i] bare PE and [ii] PE/CuTF separators. Cross-sectional SEM images of passivation layer (Li/Cu cells @30 cycles) for (f) bare PE and (g) PE/CuTF separators. Reproduced with permission.⁷³⁾ Copyright 2017, John Wiley and Sons.
그림 Fig. 17. Characteristics of Pt thin film coated separator by sputtering process. Galvanostatic cycling performance of Li/ Li symmetric cells using bare PP and PP@Pt separators at (a) 1 mA cm^-2 and (b) 2 mA cm^-2. SEM images of Li anode surface cycled for 500 hours using (c) PP and (d) PP@Pt separators. Reproduced with permission.⁷⁴⁾ Copyright 2018, American Chemical Society.
그림 Fig. 18. Electrochemical characteristics of Nb thin film coated separator by sputtering process. CV measurements of Li/S cells containing composite sulfur cathode with (a) PP and (b) Nb-PP separators at 0.1 mV s^-1. Voltage profiles of Li/S cells with (c) PP and (d) Nb-PP separators. Cycle performance of Li/S cells with (e) PP and (f) Nb-PP separators. Reproduced with permission.⁷⁵⁾ Copyright 2019, Springer Nature.
그림 Fig. 19. Characteristics of diamond-like carbon (DLC) coated PP separator by sputtering process. Surface SEM images of (a) pristine PP and (b) DLC/PP-5h separators (c) Cross-sectional SEM image of DLC/PP-5h separator. (d) Young's modulus results of pristine PP, DLC/PP-5h, and DLC/PP-10h separators. A microscopic particle diffusion model for Liions passing through the (e) pristine PP and (f) DLC/PP (DLC thickness with 300 nm) separators. Voltage profiles of Li/ Li symmetric cells having the pristine PP and DLC/PP-5h separators at (g) 3 mA cm^-2 and (h) 5 mA cm^-2. Reproduced with permission.⁷⁵⁾ Copyright 2021, John Wiley and Sons.
그림 Fig. 20. Schematic diagram and characteristics of Mg thin film coated separator by sputtering process. SEM images of (a) Bare (Celgard) and (b) Mg coated separators (Inset is Mg 1s XPS data). (c) Schematic diagram of electrodeposition with Mg coated separator. SEM images of the separators and Li anodes retrieved from Li/LCO full cells after 200 cycles: A top view of (d) Li anode surface and (e) the corresponding Mg-coated separator, A top view of (f) Li anode surface and (g) the corresponding bare separator after cycling. (h) Cycling performance of the Li/LCO full cells using the bare and Mg coated separators at 2 C rate. Reproduced with permission.⁷⁷⁾ Copyright 2019, Elsevier.

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저자의 다른 논문 :

표제어: PCR

동의어: Packet Collision Rate

용어 설명 출처 목록 (6)

용어 설명: PCR은 세균 특이성이 있는 primer를 이용하여 적은 수의 세균이 있을지라도 쉽게 검출할 수 있는 유용한 방법이며, 이를 이용하여 구강 내 치면세균막이나 타액에서 직접 세균을 검출할 수 있게 되었다[8].

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