摘要
采用X射线荧光光谱法测定高性能陶瓷中的硅元素含量,系统研究了熔剂、稀释比、脱模剂、熔融温度与时间对测定结果的影响,并分析了产生这些影响的机理。结果表明,当无水四硼酸锂、碳酸锂、样品三者质量比(m(无水四硼酸锂)∶m(碳酸锂)∶m(样品))=8.0∶1.5∶0.2时,在1 050℃下先预熔5min、再摇摆熔融10min,可以获得高质量的熔片。硅的质量浓度在55%～70%时,相关系数为0.9997,方法检出限为0.81%。硅元素的加标质量为0.02g时,加标回收率为98.5%～99.0%。此方法已应用到日常陶瓷样品的检测。
Method for the determination of silicon in high performance ceramic was established by X-ray fluorescence spectrometry(XRF).Several influencing factors were studied,including the flux for fusion sample preparation,the dilution ratio between flux and sample,the mold release,the fusion temperature and time.Besides,the mechanism of the factors wasalso discussed.It was found that the sample could be well prepared under the following conditions:the mass ratio of anhydrous lithium tetraborate,lithium carbonate and sample was 8.0∶1.5∶0.2,the fusion temperature was 1 050℃,the prefusion time was 5 min and the fusion time was 10 min.The developed method was linear over the range assayed with determination coefficient of 0.9997,when the mass concentration of silicon was between 55%and 70%.The detection limit of the method was 0.81%.Recovery study was performed at 0.02 g for silicon,and the recoveries ranged from 98.5%to 99.0%.The method has been applied to the detection of daily ceramic samples.
作者
陈美瑜
兰琳
CHEN Meiyu;LAN Lin(College of Materials, Key Laboratory of High Performance Ceramic Fibers,Ministry of Education, Xiamen University, Xiamen 361005,China)
出处
《功能材料》
EI
CAS
CSCD
北大核心
2018年第12期12217-12220,共4页
Journal of Functional Materials
关键词
X射线荧光光谱法
硅
陶瓷
先驱体转化法
氟硅酸钾滴定
X-ray fluorescence spectrometry(XRF)
silicon
ceramic
precursor infiltration pyrolysis
K 2SiF 6 titration
