冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2007年
6期
1-7
,共7页
钕铁硼%氧氮分析仪%X射线衍射%背散射扫描电镜%电解提取%光电子能谱
釹鐵硼%氧氮分析儀%X射線衍射%揹散射掃描電鏡%電解提取%光電子能譜
녀철붕%양담분석의%X사선연사%배산사소묘전경%전해제취%광전자능보
NdFeB%oxygen & nitrogen analyzer%X-ray diffraction%SEM%electroextraction%X-ray photoelectron spectroscopy
钕铁硼磁体中氧含量偏高是影响其大工业生产、造成钕铁硼磁体性能偏低的主要原因之一,因此合理地控制氧在钕铁硼中含量及其存在状态,为分析工作提出了重要研究课题.依据样品中不同状态氧与碳的结合能不同的特点,本文使用惰气熔融红外吸收法对钕铁硼材料样品中不同状态氧进行了定性和定量的方法研究.首先通过斜率加热模式,确定钕铁硼样品在不同分析加热电流下存在着两种状态氧化物.根据斜率加热模式下得到的每种状态氧化物对应的释放条件,使用分段加热模式,完全分离两种状态氧的释放峰.对原始样品和第一段加热后的中间产物分别进行X射线衍射、背散射扫描电镜、电解提取氧化物和光电子能谱分析,得到两种状态氧的定性分析结果:第一段加热电流下得到氧的释放峰为钕铁氧的复合物分解释放产物,第二段加热电流下得到的氧的释放峰来源于氧化钕的分解还原.根据文中研究得到的定性分析及定量分离方法,选取相应标准物质对两种氧化物释放峰进行分别标定,得到钕铁硼样品中两种状态氧化物的准确定量结果.
釹鐵硼磁體中氧含量偏高是影響其大工業生產、造成釹鐵硼磁體性能偏低的主要原因之一,因此閤理地控製氧在釹鐵硼中含量及其存在狀態,為分析工作提齣瞭重要研究課題.依據樣品中不同狀態氧與碳的結閤能不同的特點,本文使用惰氣鎔融紅外吸收法對釹鐵硼材料樣品中不同狀態氧進行瞭定性和定量的方法研究.首先通過斜率加熱模式,確定釹鐵硼樣品在不同分析加熱電流下存在著兩種狀態氧化物.根據斜率加熱模式下得到的每種狀態氧化物對應的釋放條件,使用分段加熱模式,完全分離兩種狀態氧的釋放峰.對原始樣品和第一段加熱後的中間產物分彆進行X射線衍射、揹散射掃描電鏡、電解提取氧化物和光電子能譜分析,得到兩種狀態氧的定性分析結果:第一段加熱電流下得到氧的釋放峰為釹鐵氧的複閤物分解釋放產物,第二段加熱電流下得到的氧的釋放峰來源于氧化釹的分解還原.根據文中研究得到的定性分析及定量分離方法,選取相應標準物質對兩種氧化物釋放峰進行分彆標定,得到釹鐵硼樣品中兩種狀態氧化物的準確定量結果.
녀철붕자체중양함량편고시영향기대공업생산、조성녀철붕자체성능편저적주요원인지일,인차합리지공제양재녀철붕중함량급기존재상태,위분석공작제출료중요연구과제.의거양품중불동상태양여탄적결합능불동적특점,본문사용타기용융홍외흡수법대녀철붕재료양품중불동상태양진행료정성화정량적방법연구.수선통과사솔가열모식,학정녀철붕양품재불동분석가열전류하존재착량충상태양화물.근거사솔가열모식하득도적매충상태양화물대응적석방조건,사용분단가열모식,완전분리량충상태양적석방봉.대원시양품화제일단가열후적중간산물분별진행X사선연사、배산사소묘전경、전해제취양화물화광전자능보분석,득도량충상태양적정성분석결과:제일단가열전류하득도양적석방봉위녀철양적복합물분해석방산물,제이단가열전류하득도적양적석방봉래원우양화녀적분해환원.근거문중연구득도적정성분석급정량분리방법,선취상응표준물질대량충양화물석방봉진행분별표정,득도녀철붕양품중량충상태양화물적준학정량결과.
High content of oxygen in NdFeB magnet is one of the essential factors that hinder its large-scale industry production and cause its low grade in magnetism performance. Therefore, how to control the total oxygen content and oxygen states in NdFeB becomes an important issue brought to analysts. Based on different binding energies of oxides with graphite in the sample, releasing behaviors of different oxides in NdFeB were investigated by both qualitative and quantitative methods in this article. Inert gas fusion infrared absorption method was used in the article. As verified by ramp heating mode, two kinds of oxides were found to exist in Nd2 Fe14 B under different analyzing heating powers. Based on releasing conditions derived from ramp heating mode, two releasing peaks of different oxides obtained from segmented heating mode were completely separated. Then, X-ray diffraction, SEM, Electrolyte distillation and Photoelectron Spectroscopy were used on Nd2Fe14B sample and the 1st- stepheated sample individually. Qualitative analysis results were obtained. The first peak was released from deoxidization of NdxFeyOz compound. The second one was released from Nd2O3 deoxidization. Based on the above results, seriatim calibrated method was used to calibrate the two peaks respectively. Accurate quantitative results of them were obtained.
