氮氩流量比与基底温度对射频溅射TiN薄膜性能的影响

Effects of N_(2)/Ar flow ratio and substrate temperature on properties of RF-sputtered TiN film

采用射频磁控溅射技术,以纯钛为靶材,氮气为反应气体,通过改变氮氩流量比与基底温度在304不锈钢及玻璃表面制备了不同的TiN薄膜。利用能谱仪、扫描电镜、台阶仪、四探针仪、划痕仪和纳米压痕仪对制备的所制薄膜的氮钛原子比、表面形貌、沉积速率、方块电阻、膜基结合力和纳米硬度进行表征。结果表明:随着氮氩流量比的增大,TiN的形貌先由四面锥体凸起结构逐渐过渡至柱状晶体堆积结构,然后转变为稀疏的液滴状颗粒结构,直至平整光滑,致密均匀。在氮气和氩气的流量分别为5.0 mL/min和50.0 mL/min的条件下,基底温度25~400℃范围内制备的TiN薄膜的结合力介于135.4 mN与210.2 mN之间。当基底温度为300℃时,薄膜的沉积速率最大,颜色最接近金黄色,氮钛原子比最接近1,结合力和纳米硬度也都最大。随着基底温度的升高,氮钛原子比逐渐降低,方块电阻不断下降,400℃时达到最小的9.87Ω。

TiN films were prepared on 304 stainless steel or glass by radio frequency(RF)magnetron sputtering with pure Ti as target and N_(2) as reaction gas under different N_(2)/Ar flow ratios and substrate temperatures.The N/Ti atomic ratio,surface morphology,deposition rate,sheet resistance,film/substrate interface adhesion,and nanohardness of the TiN film were characterized by using energy-dispersive spectroscope,scanning electron microscope,profilometer,four-probe apparatus,scratch tester,and nanoindenter.The results showed that as the N2/Ar flow ratio is increased,the morphology of TiN gradually transits from a tetrahedral convex structure to a columnar crystal packing structure,then to a sparse drop-shaped particle structure,and finally becomes smooth,compact,and uniform.When the flow rates of N2 and Ar are 5.0 mL/min and 50.0 mL/min respectively,the adhesion forces of the TiN films sputtered at substrate temperature ranging from 25℃to 400℃are 135.4-210.2 mN.The TiN film sputtered at a substrate temperature of 300℃has the maximum deposition rate,adhesion force,and nanohardness with a N/Ti atomic ratio closest to 1,and its color is almost golden yellow.As the substrate temperature is increased,the N/Ti atomic ratio of TiN film is gradually decreased,and its sheet resistance also shows a descending trend,reaching the minimum value of 9.87Ωat 400℃.