Ma Yibo, Zhang Xiaofeng, Liu Weiming, Wei Youxiu, Fu Ziyi, Li Jiuyong, Zhang Xuan, Peng Jingjing, Yan Yue
Beijing Engineering Research Center of Advanced Structural Transparencies for the Modern Traffic System, Beijing Institute of Aeronautical Materials, Beijing 100095, China.
Materials (Basel). 2021 Apr 6;14(7):1803. doi: 10.3390/ma14071803.
A batch of Sn oxides was fabricated by pulse direct current reactive magnetron sputtering (pDC-RMS) using different Ar/O flow ratios at 0.3 Pa; the influence of stoichiometry on the physical and electrochemical properties of the films was evaluated by the characterization of scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray reflection (XRR), X-ray photoelectron spectroscopy (XPS) and more. The results were as follows. First, the film surface transitioned from a particle morphology (roughness of 50.0 nm) to a smooth state (roughness of 3.7 nm) when Ar/O flow ratios changed from 30/0 to 23/7; second, all SnO films were in an amorphous state, some samples deposited with low O flow ratios (≤2 sccm) still included metallic Sn grains. Therefore, the stoichiometry of SnO calculated by XPS spectra increased linearly from SnO to SnO as the O flow ratios increased, and the oxidation degree was further calibrated by the average valence method and SnO standard material. Finally, the electrochemical performance was confirmed to be improved with the increase in oxidation degree (x) in SnO, and the SnO film deposited with Ar/O = 23/7 possessed the best cycle performance, reversible capacity of 396.1 mAh/g and a capacity retention ratio of 75.4% after 50 cycles at a constant current density of 44 μA/cm.
采用脉冲直流反应磁控溅射(pDC-RMS)在0.3 Pa的压强下,以不同的氩/氧流量比制备了一批氧化锡;通过扫描电子显微镜(SEM)、X射线衍射(XRD)、X射线反射(XRR)、X射线光电子能谱(XPS)等表征手段,评估了化学计量比对薄膜物理和电化学性能的影响。结果如下。首先,当氩/氧流量比从30/0变为23/7时,薄膜表面从颗粒形态(粗糙度为50.0 nm)转变为光滑状态(粗糙度为3.7 nm);其次,所有的氧化锡薄膜均为非晶态,一些低氧流量比(≤2 sccm)沉积的样品仍含有金属锡颗粒。因此,通过XPS光谱计算得到的氧化锡化学计量比随氧流量比的增加从SnO线性增加到SnO,并且通过平均价态法和SnO标准物质进一步校准了氧化程度。最后,证实随着氧化锡中氧化程度(x)的增加,电化学性能得到改善,在44 μA/cm的恒定电流密度下,氩/氧=23/7沉积的氧化锡薄膜具有最佳的循环性能,可逆容量为396.1 mAh/g,50次循环后的容量保持率为75.4%。