细铜丝电子背散射衍射试样的制备

为了解决细铜丝电子背散射衍射（Electron Back-Scattered Diffraction,EBSD）试样制备的难题,将电化学镀镍技术引入到EBSD试样制备过程中,并对电化学镀镍过程的工艺参数进行了研究.同时,电解抛光过程对EBSD试样表面质量影响显著,文中讨论了抛光电压和抛光时间对EBSD试样表面质量的影响.研究结果表明,当电镀液为硫酸镍280g/L、氯化镍45g/L、硼酸30g/L、十二烷基硫酸镍0.05g/L,在室温下,电压为1V、pH=3时细铜丝上能够获得很好的镀层;当电解抛光配方为蒸馏水500mL＋磷酸250mL＋乙醇250mL＋丙醇50mL＋尿素5g,温度为-15℃～-20℃,电压为3V,时间90～120s,试样抛光效果较佳;采用上述两种过程处理后,真应变为8.42的EBSD试样的标定率可达80%以上.

Study on Preparation of EBSD Sample of the Fine Copper

In order to prepare the EBSD samples of the fine copper wire,a method of EBSD sample preparation was put forward and the technology parameters of electrochemical nickel plating have been investigated.Meanwhile,The electrolytic polishing has a significant influence on surface quality of samples,electrolytic polishing time and voltage have been investigated.The results show that electrolytic plating solution of the fine copper wire,at room temperature,was comprised of nickel sulfate 280g/L,nickel chloride 45 g/L,boric acid 30 g/L and lauryl sodium sulfate 0.05 g/L.When the voltage is 1 V and pH=3,good plating surface was obtained.A good polishing effect has been received in a solution of 500 mL distilled water,250 mL HPO3,250 mL ethanol,50 mL propanol and 5 g urea.The process is of temperature-15 ℃~-20 ℃,voltage 3 V and polishing time 90~120 s.Indexing rate of samples,with large strain,prepared by the above method was up to 80%.