倾斜溅射沉积法制备SnO_2基纳米结构阵列的研究
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摘要
磁控溅射作为最广泛使用的镀膜方法之一，具有样品均匀性和可重复性较好、可方便掺杂以调节薄膜成分等许多优点。另一方面，倾斜沉积法（GLAD）通过束流大角度地倾斜入射引起阴影效应，从而对薄膜的形貌进行调控，制备出特殊形貌的纳米结构。本文将磁控溅射和倾斜沉积相结合，制备出形貌和成分可控的SnO_2基纳米结构阵列，并对其光学、表面浸润、磁学性能进行研究。和光刻等方法相比，倾斜溅射沉积法具有步骤简单、成本较低的优点，在器件应用领域表现出了巨大的潜力。
首先，通过倾斜溅射沉积法在密排的聚苯乙烯（polystyrene, PS）微球模板上制备出Ti_xSn_(1-x)O_2纳米结构阵列。通过调节Ti靶的溅射功率和PS微球模板的大小控制Ti_xSn_(1-x)O_2纳米结构的形貌，并进一步调控薄膜的反射率。退火后的薄膜晶化为TiO2和SnO_2的复合纳米结构，形貌和抗反射性能均保持良好的热稳定性。
其次，对Ti_xSn_(1-x)O_2纳米结构阵列的表面浸润性进行了研究。以200nm直径聚苯乙烯微球为模板制备出的形貌各向异性的纳米片结构呈现出宏观的各向异性润湿现象，并通过三相接触线的结构进行研究。另一方面，以1μm直径聚苯乙烯微球为模板制备的“球壳”结构在可见光照和黑暗环境中能够发生可逆的超亲水-疏水转变。Ti_xSn_(1-x)O_2纳米结构阵列同时实现了抗反射性能和特殊浸润性，可应用于表面的抗反射、自清洁和防雾层。
最后，通过倾斜溅射沉积法制备Fe_xSn_(1-x)O_2纳米结构阵列。和Fe_xSn_(1-x)O_2平膜相比，Fe_xSn_(1-x)O_2纳米结构阵列具有更大的饱和原子磁矩，并且同时具有垂直磁各向异性和面内磁各向异性。对不同的Fe含量下氧空位的EPR信号强度和饱和原子磁矩的变化趋势进行了研究，表明氧空位是Fe_xSn_(1-x)O_2薄膜磁性的重要因素。
As the most popular fabrication method of films, magnetron sputter deposition hasadvantages in its good homogeneity and reproducibility, and the ease and flexibility ofdoping, which is extensively used to adjust the composition. On the other hand, themorphology of films can be tuned by Glancing Angle Deposition (GLAD) technique,in which the oblique incident vapor flux causes atomic shadow effects and thus resultsin special morphological nanostructures. With GLAD and magnetron sputter depositioncombined, periodic arrays of SnO_2-based nanostructures with modulated compositionsand morphology were fabricated. The glancing angle sputter deposition technique ismuch simpler and cheaper compared to lithography techniques, and thus shows greatpotentials in device applications.
First, regular arrays of Ti_xSn_(1-x)O_2nanostructures were prepared by glancing anglesputter deposition onto self-assembled close-packed arrays of polystyrene microspheres.The morphology of the nanostructures could be modulated by the variation of thesputtering power of Ti target and the size of polystyrene microspheres templates.Accordingly, the performance of reflection which was dependent on the morphology ofnanostructures could be tuned by optimizing the parameters. After annealing in air, thefilms were crystallized to TiO2/SnO_2composite and maintained good thermal stabilityin the morphology and antireflection property.
Secondly, the wetting behaviors of Ti_xSn_(1-x)O_2nanostructures were studied. Theanisotropic nanoflakes grown on200-nm-diameter polystyrene microspheres exhibitedmacroscopic-wetting anisotropy, which is ascribed to the difference of the three-phasecontact line structure in different directions, resulting from the anisotropic topography.On the other hand, it was shown that the “spheric shells” deposited on1-μm-diameterpolystyrene microspheres can be reversibly switched between hydrophobicity andsuperhydrophilicity by alternating visible light illumination and dark storage. Therealization of special wettability on antireflective films is of great significance and canbe employed to develop coatings for various substrates with simultaneous antireflective,self-cleaning and antifogging behavior.
Thirdly, periodic arrays of Fe_xSn_(1-x)O_2nanostructures were fabricated by glancingangle sputter deposition. Compared with Fe_xSn_(1-x)O_2flat films, arrays of Fe_xSn_(1-x)O_2 nanostructures processed larger saturation magnetic moment, and exhibited bothperpendicular magnetic anisotropy and in-plane magnetic anisotropy. The EPR signaloriginating from the oxygen vacancies significantly varied with the Fe concentrationand reached the strongest at x=0.059, which is consistent with the saturationmagnetization. It demonstrates that the oxygen vacancies are an important factor forthe ferromagnetism of Fe_xSn_(1-x)O_2films.
首先，通过倾斜溅射沉积法在密排的聚苯乙烯（polystyrene, PS）微球模板上制备出Ti_xSn_(1-x)O_2纳米结构阵列。通过调节Ti靶的溅射功率和PS微球模板的大小控制Ti_xSn_(1-x)O_2纳米结构的形貌，并进一步调控薄膜的反射率。退火后的薄膜晶化为TiO2和SnO_2的复合纳米结构，形貌和抗反射性能均保持良好的热稳定性。
其次，对Ti_xSn_(1-x)O_2纳米结构阵列的表面浸润性进行了研究。以200nm直径聚苯乙烯微球为模板制备出的形貌各向异性的纳米片结构呈现出宏观的各向异性润湿现象，并通过三相接触线的结构进行研究。另一方面，以1μm直径聚苯乙烯微球为模板制备的“球壳”结构在可见光照和黑暗环境中能够发生可逆的超亲水-疏水转变。Ti_xSn_(1-x)O_2纳米结构阵列同时实现了抗反射性能和特殊浸润性，可应用于表面的抗反射、自清洁和防雾层。
最后，通过倾斜溅射沉积法制备Fe_xSn_(1-x)O_2纳米结构阵列。和Fe_xSn_(1-x)O_2平膜相比，Fe_xSn_(1-x)O_2纳米结构阵列具有更大的饱和原子磁矩，并且同时具有垂直磁各向异性和面内磁各向异性。对不同的Fe含量下氧空位的EPR信号强度和饱和原子磁矩的变化趋势进行了研究，表明氧空位是Fe_xSn_(1-x)O_2薄膜磁性的重要因素。
As the most popular fabrication method of films, magnetron sputter deposition hasadvantages in its good homogeneity and reproducibility, and the ease and flexibility ofdoping, which is extensively used to adjust the composition. On the other hand, themorphology of films can be tuned by Glancing Angle Deposition (GLAD) technique,in which the oblique incident vapor flux causes atomic shadow effects and thus resultsin special morphological nanostructures. With GLAD and magnetron sputter depositioncombined, periodic arrays of SnO_2-based nanostructures with modulated compositionsand morphology were fabricated. The glancing angle sputter deposition technique ismuch simpler and cheaper compared to lithography techniques, and thus shows greatpotentials in device applications.
First, regular arrays of Ti_xSn_(1-x)O_2nanostructures were prepared by glancing anglesputter deposition onto self-assembled close-packed arrays of polystyrene microspheres.The morphology of the nanostructures could be modulated by the variation of thesputtering power of Ti target and the size of polystyrene microspheres templates.Accordingly, the performance of reflection which was dependent on the morphology ofnanostructures could be tuned by optimizing the parameters. After annealing in air, thefilms were crystallized to TiO2/SnO_2composite and maintained good thermal stabilityin the morphology and antireflection property.
Secondly, the wetting behaviors of Ti_xSn_(1-x)O_2nanostructures were studied. Theanisotropic nanoflakes grown on200-nm-diameter polystyrene microspheres exhibitedmacroscopic-wetting anisotropy, which is ascribed to the difference of the three-phasecontact line structure in different directions, resulting from the anisotropic topography.On the other hand, it was shown that the “spheric shells” deposited on1-μm-diameterpolystyrene microspheres can be reversibly switched between hydrophobicity andsuperhydrophilicity by alternating visible light illumination and dark storage. Therealization of special wettability on antireflective films is of great significance and canbe employed to develop coatings for various substrates with simultaneous antireflective,self-cleaning and antifogging behavior.
Thirdly, periodic arrays of Fe_xSn_(1-x)O_2nanostructures were fabricated by glancingangle sputter deposition. Compared with Fe_xSn_(1-x)O_2flat films, arrays of Fe_xSn_(1-x)O_2 nanostructures processed larger saturation magnetic moment, and exhibited bothperpendicular magnetic anisotropy and in-plane magnetic anisotropy. The EPR signaloriginating from the oxygen vacancies significantly varied with the Fe concentrationand reached the strongest at x=0.059, which is consistent with the saturationmagnetization. It demonstrates that the oxygen vacancies are an important factor forthe ferromagnetism of Fe_xSn_(1-x)O_2films.
引文
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