用脉冲电沉积方法制备了纳米晶Ni-Co-Fe-P合金镀层.采用X射线衍射(XRD)、透射电镜(TEM)、能谱分析(EDS)、差示扫描量热法(DSC)以及显微硬度计等测试方法研究合金镀层的微观结构、显微硬度和热稳定性.结果表明,纳米晶Ni-40.41%Co-6.16%Fe-1.63%P合金镀层的晶体结构为单一面心立方结构,其平均晶粒尺寸仅为8.8 nm,并具有(111)织构.该镀层的显微硬度随着退火温度的升高而上升,在300和450℃之间达到最大值,之后随退火温度的继续提高而逐步降低.在450℃退火后,晶粒长大到35.1 nm;600℃退火后,晶粒长大到160.8 nm,达亚微米级.在晶粒长大过程中伴有结构的转变,镀层由(111)织构向(200)织构转变.在升温速率为20 K/min的DSC曲线中,该镀层在474.4℃开始放热,并出现明显的放热峰,峰值温度为499.1℃,放热焓为9.086 J/g;通过Kissinger方程式求出该镀层晶粒长大的激活能为369.3 kJ/mol,具有很好的热稳定性.
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