| LI Lianchi,WU Aimin,SONG Xinyi,LIU Yanling,WANG Yanan,HUANG Hao.Preparation Process of LiNi0.8Co0.1Mn0.1O2 Thin Film by Magnetron Sputtering[J],53(6):190-197 |
| Preparation Process of LiNi0.8Co0.1Mn0.1O2 Thin Film by Magnetron Sputtering |
| Received:February 11, 2023 Revised:June 01, 2023 |
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| DOI：10.16490/j.cnki.issn.1001-3660.2024.06.017 |
| KeyWord:solid state thin film battery NCM cathode thin film orthogonal experiment magnetron sputtering electrochemical performance |
| Author | Institution |
| LI Lianchi |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
| WU Aimin |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
| SONG Xinyi |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
| LIU Yanling |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
| WANG Yanan |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
| HUANG Hao |
Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian , China |
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| Abstract: |
| Magnetron sputtering is the most commonly used method for preparing NCM thin films, which has the advantages of fast sputtering speed, dense film and good film substrate bonding. The existing problem is that the composition of the films prepared by magnetron sputtering may deviate from the target material, and it is difficult to prepare the stoichiometric NCM811 films. NCM811 materials need to be sintered at high temperature (800-1 000 ℃) or annealed at high temperature (600-800 ℃) for a long time to obtain layered materials with good cycling performance and high capacity. The work aims to prepare NCM811 thin films at lower temperature by optimizing the process and eliminating annealing steps and obtain the optimal preparation process conditions for NCM811 thin film material with excellent comprehensive performance. The surface impurities on the polished stainless steel substrate were removed by sonicating the substrate in acetone, anhydrous ethanol, and deionized water for 15 min. Then, the sample was blown to be dry in one direction with an ear wash ball and fixed on the sample table. When the background vacuum was better than 6×10−4 Pa, the air pressure in the vacuum chamber was adjusted to reach the ignition pressure (2 Pa), and the ignition power was set to 30 W. After light up, the air pressure was adjusted to the working air pressure (1 Pa), the sputtering power was increased to 60 W, pre sputtering was conducted, and glow cleaning was carried out on the target surface. After 15 minutes of pre sputtering, the sputtering power was adjusted to officially sputter for 5 hours. The power, substrate temperature, and argon oxygen ratio during sputtering were set according to the orthogonal test table. The structure was analyzed by an X-ray diffractometer (D8 Advance) and the cross-sectional and surface morphology of the samples were observed by scanning electron microscope (SUPARR 55). The composition of thin films was tested by EDS and ICP (Agilent 5110). The cycling performance of the batteries was tested by battery testing system (LAND CT2001A). According to the range analysis method, the order of factors affecting the retention rate of the first 50 cycles of discharge capacity was temperature > power > argon oxygen ratio. Power and temperature had a significant impact on cycle performance, with range value of 18.45 and 26.79, respectively. The argon oxygen ratio had a small impact on the cycle performance, with a range R value of 3.17. Increasing the sputtering power and substrate heating temperature, as well as increasing the argon content in the argon oxygen ratio, was beneficial for the preparation of NCM811 thin films with stoichiometric ratios. The orthogonal experimental results dthat the optimal process conditions for thin film preparation were:sputtering power as 110 W, substrate temperature as 650 ℃ and Ar:O2=2∶1 (Volume flow ratio). NCM811 thin films with good cyclic performance and stoichiometric ratio can be prepared under optimal process parameters. The stable structure is the main reason for the better cycling stability of NCM811 thin films. The increase in sputtering power and substrate temperature results in good crystallinity, good layered structure, crack free, denser, and more stable structure of thin film. |
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