采用ZrW2O8陶瓷靶材,以射频磁控溅射法在单晶硅基片上沉积制备了ZrW2O8薄膜。用X射线衍射仪和热膨胀仪分析了靶材的成分和热膨胀性能;用X射线光电子能谱仪和扫描电子显微镜分析了薄膜的组分及其表面形貌;用表面粗糙轮廓仪和薄膜应力分布测试仪测量了薄膜的厚度和应力。实验结果表明:制备的ZrW2O8靶材纯度高且具有良好的负热膨胀性能,磁控溅射沉积制备的ZrW2O8薄膜和靶材保持良好的化学成分一致性,且表面平滑、致密,在750℃热处理3 min后薄膜表面晶粒明显长大,并出现孔洞缺陷;衬底未加热时沉积制备的ZrW2O8薄膜选区应力差最小,应力分布最均匀,随着热处理温度和衬底温度的提高,由于薄膜和衬底的热膨胀系数的差异较大,薄膜选区内的应力差增加,薄膜应力分布不均性增大。
The ZrW2O8 Films with a negative thermal expansion property were deposited by RF magnetron sputtering on Si substrates.The impacts of the deposition conditions,purity of target materials,annealing temperatures and sputtering power,on film quality were evaluated.The microstructures and mechanical properties of the films were characterized with X-ray diffraction,X-ray photoelectron spectroscopy,scanning electron microscopy and conventional surface probes.The results show that the annealing temperature strongly affects the surface stress distribution of the fairly smooth,compact films with good negative thermal expansion.For example,annealed at 750℃ for 3 min,bigger grains with increased pores were observed.The stress uniformly distributes with little variations in the as-deposited films.As the substrate and annealing temperatures increased,the stress,1.613 GPa at least,its uniform stress distribution deteriorated with an increased bigger stress difference,possibly because of the mismatch of thermal expansion coefficients at the interface of the film and the substrate.