铜锡合金电镀层锡含量的几种测试方法比较  

Comparative Analysis on Several Test Methods of Tin Content in Copper/Tin Plating Coating

作　　者：孙文涛 周立峰 方磊 钟庆富 徐国强[4] 齐建涛[1] SUN Wen-tao;ZHOU Li-feng;FANG Lei;ZHONG Qing-fu;XU Guo-qiang;QI Jian-tao(College of New Energy,China University of Petroleum(East China),Qingdao 266580,China;PetroChina Liaohe Engineering Co.,Ltd.,Panjin 124000,China;Shandong Mining Machinery Huaneng Manufacturing Co.,Ltd.,Weifang 261200,China;College of Pipeline and Civil Engineering,China University of Petroleum(East China),Qingdao 266580,China)

机构地区：[1]中国石油大学(华东)新能源学院,山东青岛266580 [2]中油辽河工程有限公司,辽宁盘锦124000 [3]山东矿机华能制造有限公司,山东潍坊261200 [4]中国石油大学(华东)储运与建筑工程学院,山东青岛266580

出　　处：《材料保护》2022年第11期184-187,共4页Materials Protection

基　　金：注水井油管适用性评价(30200006-21-ZC0613-0031);中国石油大学(华东)大学生自主创新项目;中央高校基本科研业务费专项资金(18CX02128A)资助。

摘　　要：采用碘酸钾滴定法,电感耦合等离子体原子发射光谱法(ICP-AES),扫描电子显微镜(SEM/EDS),X-射线能谱仪(EDX),对液压油缸表面铜锡镀层主要成分的含量进行对比分析。结果表明:碘酸钾滴定法,ICP-AES,SEM/EDS,EDX 4种方法测试的锡含量分别为(7.30±0.17)%,(7.07±0.15)%,(4.33±0.47)%和(16.69±2.71)%。ICP-AES是基于铜锡镀层溶解液的光谱分析,与碘酸钾滴定法成分测试结果相近,可代表镀层成分准确含量;SEM/EDS是针对镀层表面分析方法,测试结果相对较低,反映出镀层内外锡含量不均匀;EDX能谱仪因无法聚焦和难以校准,虽测试快速,但误差较大,测试精度在于能谱仪校准和样品表面聚焦。通过对比不同的测试方法得出碘酸钾滴定法、ICP-AES、SEM/EDS均使用于铜镀层中锡含量的检测,3种方法中ICP-AES在准确度较高,SEM/EDS测试速度较快,碘酸钾滴定法成本较低,结果准确。为现场测试提供测试依据。In this paper, the contents of main components of copper/tin plating coating on the surface of hydraulic cylinder were compared and analyzed by potassium iodate titration method, inductively coupled plasma atomic emission spectrometry(ICP-AES), scanning electron microscope(SEM/EDS) and X-ray energy spectrometer(EDX). Results showed that the tin contents measured by potassium iodate titration, ICP-AES, SEM/EDS and EDX were(7.30±0.17)%,(7.07±0.15)%,(4.33±0.47)% and(16.69±2.71)% respectively. ICP-AES was based on the spectral analysis of copper/tin plating coating solution, and its test result was similar to the component test result of potassium iodate titration method, which could represent the accurate content of plating coating components;SEM/EDS was a surface analysis method for the plating coating, and the test results were relatively low, reflecting the uneven tin content inside and outside the coating;EDX energy spectrometer was unable to focus and difficult to calibrate. Although the test was fast, the error was large. The test accuracy relied on the calibration of energy spectrometer and the focusing of sample surface. By comparing different test methods, it could be concluded that potassium iodate titration method, ICP-AES and SEM/EDS were all feasible to detect tin content in copper plating coating. Among the three methods, ICP-AES had highest accuracy, SEM/EDS had fastest test speed, potassium iodate titration method had lowest cost and accurate results. This work would provide test basis for field test.

关 键 词：电镀 铜锡镀层 锡含量测定 ICP-AES 碘酸钾滴定 SEM/EDS EDX 

分 类 号：X781.1[环境科学与工程—环境工程]