Optimization of the deposition process of ZrN and TiN thin films on Si(1 0 0) using design of experiment method
Optimization of the deposition process of ZrN and TiN thin films on Si(1 0 0) using design of experiment method
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DOI：
10.1016/s0254-0584(03)00209-8
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发表时间：
2003-09
影响因子：
4.6
通讯作者：
W. Chou;Chunting Sun;G. Yu;Jia-Hong Huang
中科院分区：
文献类型：
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作者：
W. Chou;Chunting Sun;G. Yu;Jia-Hong Huang
分别采用空心阴极放电离子镀（HCD-IP）和非平衡磁控溅射（UBM）方法在Si（100）衬底上制备了氮化锆（ZrN）和氮化钛（TiN）薄膜。实验设计（DOE）一直被认为是一种有效的方法来优化复杂的工业过程。本研究的目的是验证DOE方法在PVD工艺中应用的可行性和可靠性，优化沉积工艺参数，并确定影响薄膜性能的敏感参数。对于HCD-IP方法，选择了四个参数，包括衬底温度，衬底偏压，Ar分压，和N2分压，对于UBM方法，直流功率，N2流量，靶-靶距离，和试样高度被选择为操作参数。沉积后，通过X射线衍射（XRD）和高分辨率扫描电子显微镜（SEM）对薄膜结构进行表征。用纳米压痕法测定了ZrN和TiN薄膜的硬度。用四探针法测量了薄膜的电阻率。通过原子力显微镜（AFM）获得的膜的粗糙度。采用均数分析和方差分析对各敏感参数进行评价，并预测最佳条件。根据统计分析，HCD-IP工艺中最敏感的参数是衬底偏压和N2分压，UBM工艺中最敏感的参数是直流功率和样品高度。并获得了各体系的最佳沉积条件。
Zirconium nitride (ZrN) and titanium nitride (TiN) thin films were deposited on Si(100) substrates using hollow cathode discharge ion-plating (HCD-IP) and unbalanced magnetron (UBM) sputtering methods, respectively. Design of experiment (DOE) has long been recognized as a powerful method to optimize a complex process in industry. The purposes of present study were to verify the feasibility and reliability of the application of DOE method on PVD processes and optimize the processing parameters for the deposition process, in which the sensitive parameters that affected the film properties were also identified. For HCD-IP method, four parameters, including substrate temperature, substrate bias, Ar partial pressure, and N2partial pressure, were selected; for the UBM method, dc power, N2flow rate, specimen–target distance, and specimen height were chosen to be the operating parameters. After deposition, the thin film structure was characterized by X-ray diffraction (XRD), and high-resolution scanning electron microscopy (SEM). The hardness of the ZrN and TiN films was determined by nanoindentation. The resistivity of thin films was measured by a four-point probe. The roughness of the film was obtained by atomic force microscopy (AFM). The analysis of mean (ANOM) and analysis of variance (ANOVA) were conducted to assess the sensitive parameters and predict the optimum conditions. Based on the statistical analysis, the most sensitive parameters in the HCD-IP process were the substrate bias and the N2partial pressure and in the UBM process were the dc power and the specimen height. The optimum deposition conditions in each system were also acquired.