李镰池,吴爱民,宋欣忆,刘延领,王亚楠,黄昊.磁控溅射制备LiNi0.8Co0.1Mn0.1O2薄膜工艺研究[J].表面技术,2024,53(6):190-197.
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].Surface Technology,2024,53(6):190-197 |
| 磁控溅射制备LiNi0.8Co0.1Mn0.1O2薄膜工艺研究 |
| Preparation Process of LiNi0.8Co0.1Mn0.1O2 Thin Film by Magnetron Sputtering |
| 投稿时间：2023-02-11 修订日期：2023-06-01 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.06.017 |
| 中文关键词: 固态薄膜电池 NCM正极薄膜 正交试验 磁控溅射 电化学性能 |
| 英文关键词:solid state thin film battery NCM cathode thin film orthogonal experiment magnetron sputtering electrochemical performance |
| 基金项目:中央高校基础研究基金项目(DUT20LAB123，DUT20LAB307) |
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| 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 116024, China |
| WU Aimin | Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China |
| SONG Xinyi | Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China |
| LIU Yanling | Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China |
| WANG Yanan | Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China |
| HUANG Hao | Key Laboratory of Energy Materials and Device Liaoning Province, School of Materials Science and Engineering, Dalian University of Technology, Liaoning Dalian 116024, China |
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| 中文摘要: |
| 目的 探究了磁控溅射法制备符合化学计量比且循环性能良好的LiNi0.8Co0.1Mn0.1O2(NCM811)薄膜工艺，有利于进一步提高全固态薄膜电池能量密度。方法 从溅射功率、氩氧比、衬底温度中各选取3个水平组成L9(34)正交试验，在不锈钢衬底上沉积制备NCM811薄膜。利用X射线衍射仪和扫描电子显微镜对薄膜进行表征。利用EDS和ICP对薄膜成分进行分析。利用蓝电测试系统对以NCM811为正极的电池进行循环曲线测试。结果 根据极差分析结果发现，影响前50圈放电容量保持率的因素从大到小依次为:温度>功率>氩氧比。其中功率和温度对循环性能有很大的影响，极差R值分别为18.45和26.79;氩氧比对循环性能影响较小，极差R值为3.17。增大溅射功率、提高衬底加热温度、增加氩氧比中氩气的含量有利于制备出符合化学计量比的NCM811薄膜。随着溅射功率的提升，NCM811薄膜的结晶度增强，材料中Ni2+/Li+阳离子的混排程度降低;随着衬底温度升高，薄膜由非晶逐渐转化为晶态，表面由无序非晶形貌过渡到小三角片状晶粒，厚度变薄，且更加致密。薄膜的循环性能也随着功率和衬底温度的增加有着明显的提升。结论 正交试验结果表明，薄膜制备的最优工艺条件为:溅射功率110 W，衬底温度650 ℃，Ar∶O2=2∶1(体积流量比)，验证试验表明NCM811薄膜中主元素原子数占比Ni∶Co∶Mn=79.9∶10.2∶9.9，接近理想原子数占比8∶1∶1，且前50圈放电容量保持率达到72.33%。 |
| 英文摘要: |
| 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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