宋俊,蒋明杰,楚晓婉,万驰,李会洁,张琦,陈宇慧,吴学红,刘娟芳.冷喷涂制备纯硅负极结合特性对电极性能的影响[J].表面技术,2023,52(5):288-297.
SONG Jun,JIANG Ming-jie,CHU Xiao-wan,WAN Chi,LI Hui-jie,ZHANG Qi,CHEN Yu-hui,WU Xue-hong,LIU Juan-fang.Effect of Bonding Characteristics of Pure Silicon Anode Prepared by Cold Spraying on Electrode Performance[J].Surface Technology,2023,52(5):288-297 |
| 冷喷涂制备纯硅负极结合特性对电极性能的影响 |
| Effect of Bonding Characteristics of Pure Silicon Anode Prepared by Cold Spraying on Electrode Performance |
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| DOI：10.16490/j.cnki.issn.1001-3660.2023.05.028 |
| 中文关键词: 锂离子电池 硅基电极 冷喷涂 结合特性 循环性能 |
| 英文关键词:lithium-ion battery silicon-based electrode cold spraying bonding characteristics cycle performance |
| 基金项目:国家自然科学基金(51906229，51906230，51776027);河南省高等学校重点科研项目(21B470013);河南省科技攻关项目(212102210235) |
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| Author | Institution |
| SONG Jun | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| JIANG Ming-jie | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| CHU Xiao-wan | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| WAN Chi | a.School of Energy and Power Engineering, b.Key Laboratory of Low-grade Energy Utilization Technologies and Systems, Ministry of Education of China, Chongqing University, Chongqing 400044, China |
| LI Hui-jie | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| ZHANG Qi | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| CHEN Yu-hui | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| WU Xue-hong | College of Energy and Power Engineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China |
| LIU Juan-fang | a.School of Energy and Power Engineering, b.Key Laboratory of Low-grade Energy Utilization Technologies and Systems, Ministry of Education of China, Chongqing University, Chongqing 400044, China |
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| 中文摘要: |
| 目的 提高冷喷涂制备锂离子电池硅(Si)基负极的电化学性能，探究冷喷涂制备硅基负极结合特性对电极性能的影响。方法 通过涂覆和冷喷涂制备硅基负极，利用剥离强度试验测试活性材料与集流体的结合强度。通过扫描电镜表征充放电前后电极表面及断面形貌，分析2种电极的结构稳定性。通过观察单颗粒子沉积形貌，研究硅颗粒的沉积特性。采用恒流充放电、循环伏安法、交流阻抗法分别研究电极的循环性能和动力学特性。结果 在相同剥离条件下，Si–喷涂样品结合强度高，且剥离现象出现较晚，Si–喷涂样品的平均载荷为2.04 N，大于Si–涂覆样品的平均载荷(1.51 N)。Si–涂覆电极材料与集流体的贴合度较差，铜箔与涂层以及涂层材料内部均存在大量的孔隙结构，Si–喷涂电极活性材料均匀沉积于铜箔表面簇状的缝隙中，涂层较薄，未能覆盖簇状凸起。硅颗粒无法连续沉积形成较厚的涂层，仅以嵌入的方式沉积于铜箔表面。Si–涂覆电极循环200次后，容量仅剩51 mAh/g，而Si–喷涂电极循环200次后，容量高达240 mAh/g。Si–喷涂电极的Rct比Si–涂覆小，说明Si–喷涂电极的嵌入式结构利于电荷的转移。Si–涂覆电极的锂离子扩散系数在1~200次嵌锂后，始终比Si–喷涂电极高出1个数量级。结论 冷喷涂制备的硅基负极具有更高的结合强度。Si–喷涂电极活性材料均匀沉积于铜箔表面簇状凸起缝隙之中，有利于缓解体积效应，提高了结构的稳定性，显示出更好的循环性能和容量性能。相比于Si–涂覆电极，Si–喷涂电极具有较小的电荷转移阻抗和较大的离子扩散阻抗。 |
| 英文摘要: |
| The cold spray method has great potential to prepare lithium ion battery electrode coatings. This paper compares the characteristics of the coating method and the cold spray method to prepare silicon-based anodes. It is proposed that the bonding characteristics of the cold spray method are beneficial to improve the cycle performance and capacity performance of silicon-based anodes. With 10 μm Si powder as active material and sodium carboxymethyl cellulose (CMC) as binder, the active material, conductive agent, and binder were mixed according to the mass ratio of Si∶Super P∶CMC=6∶2∶2. An appropriate amount of deionized water was added as a solvent. It was stirred evenly, and then applied on 50 μm thick single-sided copper foil. All the sprayed samples were prepared by self-developed spraying equipment. 10 μm Si powder and conductive carbon black (Super P) were mixed in a mass ratio of 3∶1 and then put into a ball mill for 2 h to obtain composite powder. The copper foil was cut into 10 cm×10 cm and fixed on the cold spray sample stage. At spraying temperature:300 ℃, spraying pressure:1 MPa, spraying distance:5 cm, spraying pass:1 time, powder feeding rate:3.3 g/min, and with powder carrier gas as the air, the deposition of single particle was achieved by reducing the powder feeding rate and increasing the substrate moving speed. The microscopic morphologies of the samples were characterized by a field emission scanning electron microscope (FESEM, Nova400). Elemental analyses were performed on an energy dispersive spectrometer (EDS) attached to the field emission scanning electron microscope. The bonding strength between the electrode coating and the substrate copper foil was tested with an electronic universal testing machine of model E1000. The electrode samples were cut into the same size, a 3M tape was adhered to its surface with the same sticking area, the electrode sample was fixed on the upper part of the testing machine, and the unaffixed end of the tape was fixed on the lower part, at a stripping angle relative to the sticking position of the tape:180°, stripping speed:15 mm/min. Its test was continued under load until the 3M tape was separated from the electrode sample, and a force-displacement curve was obtained. The constant current charge-discharge test was carried out in an incubator with LAND test system (LAND-CT3001AU) in the voltage range of 0.05-2 V. The electrode specific capacity was calculated based on the total weight of Si. The cyclic voltammetry curve (current-voltage) was tested by electrochemical workstation (CHI604E) in 0-2 V and at 0.1 mV/s. Under the same stripping conditions, the Si-sprayed samples had high bonding strength and the stripping phenomenon appeared later. The average load of the Si-sprayed samples was 2.04 N, which was larger than that of the Si-coated samples (1.51 N). The adhesion between the Si-coated electrode material and the current collector was poor, and there were a large number of pore structures between the copper foil and the coating and inside the coating material. The Si-sprayed electrode active material was uniformly deposited in the cluster bulges gaps on the surface of the copper foil. The thin coating did not cover the cluster bulges. The silicon particles could not be deposited continuously to form a thicker coating, and were only deposited on the surface of the copper foil in an embedded manner. The capacity of the Si-sprayed electrode was only 51 mAh/g after 200 cycles, while the capacity of the Si-sprayed electrode was as high as 240 mAh/g after 200 cycles. The Rct of the Si-sprayed electrode was smaller than that of the Si-coated electrode. The lithium ion diffusion coefficient of the Si-coated electrode was always one order of magnitude higher than that of the Si-sprayed electrode from the 1st to the 200th lithium-intercalation. The silicon-based anode prepared by cold spraying has higher bonding strength. The Si-sprayed electrode active material is uniformly deposited in the cluster bulges gaps on the surface of the copper foil, which is beneficial to alleviate the volume effect, improve the structural stability, and show better cycle performance and capacity performance. Compared with Si-coated electrodes, Si-sprayed electrodes have smaller charge transfer resistance and larger lithium ion diffusion resistance. |
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