在镀液成分、pH值、沉积电流密度和脉冲占空比等工艺参数不变的条件下,利用脉冲电沉积技术在镀液温度分别为30,50和80℃时制备了包含高密度纳米孪晶片层结构的纳米晶Ni薄膜.利用SEM,XRD和TEM研究了镀液温度对纳米孪晶Ni薄膜的沉积速率、择优取向、晶粒尺寸、孪晶片层特征尺寸(长度和厚度)以及生长规律的影响;利用HRTEM揭示了纳米孪晶Ni的孪晶界面微观结构特征,利用纳米压痕技术研究了温度对Ni薄膜纳米压痕硬度的影响.研究结果表明:脉冲电沉积纳米孪晶Ni薄膜的生长速率在20-30 nm/s之间,镀液温度为30和50℃时Ni薄膜沿(220)面择优生长,80℃时转变为沿(200)面择优生长;随着镀液温度的升高,Ni薄膜的平均晶粒尺寸由900 nm减小到300 nm,晶粒内部孪晶片层的厚度由60 nm降低到28 nm; 50℃时纳米孪晶Ni薄膜的纳米压痕硬度平均值最高,达3.75 GPa.
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