Determination of nitrogen in titanium, aluminum, silicon, hafnium nitrides and compositions on their base using a Metavak-AK analyzer

N. V. Chapysheva, O. M. Miloserdova
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Abstract

Methods for determining nitrogen in the products of self-propagating high-temperature synthesis (SHS), i.e., titanium, aluminum, silicon, and hafnium nitrides using a Metavak-AK gas analyzer have been developed. The optimal modes of analysis have been selected: the time and temperature of degassing of the crucible with flux in the furnace, the time and temperature of purging the extraction chamber with the sample, the time of automatic dumping of the sample from the loading chamber into the crucible, the time and temperature of purging the chamber after loading, the time of removal of gaseous products of reduction melting and registration of nitrogen signals. Furnace operating programs were compiled to determine the nitrogen content in TiN, AlN, Si3N4, HfN. Reduction melting of the samples took place in a helium flow at a furnace temperature of 2700°C for TiN, AlN, HfN, and 2500°C for Si3N4. To speed up the process and complete nitrogen extraction, a metal bath was used: nickel grit in the case of titanium and hafnium nitrides, and combined Sn/Ni flux for aluminum and silicon nitrides. The nitrogen content in the studied samples was determined in the range from 0.12 up to 39.3 %wt., the relative standard deviation was 0.6 – 3.6%. The accuracy of the results obtained on a Metavak-AK gas analyzer is confirmed by the Kjeldahl and Dumas reference methods.
使用 Metavak-AK 分析仪测定钛、铝、硅、氮化铪及其基底成分中的氮含量
已开发出使用 Metavak-AK 气体分析仪测定自推进高温合成(SHS)产物(即钛、铝、硅和氮化铪)中氮含量的方法。选择了最佳分析模式:坩埚与熔剂在炉内脱气的时间和温度、用样品吹扫萃取室的时间和温度、样品从装载室自动倾倒到坩埚的时间、装载后吹扫萃取室的时间和温度、去除还原熔化的气体产物的时间以及氮气信号的记录。编制了熔炉运行程序,以确定 TiN、AlN、Si3N4 和 HfN 中的氮含量。样品的还原熔化在氦气流中进行,TiN、AlN、HfN 的炉温为 2700°C,Si3N4 为 2500°C。为了加快这一过程并完成氮的提取,使用了金属浴:钛和铪氮化物使用镍砂,铝和硅氮化物使用锡/镍联合助熔剂。研究样品中氮含量的测定范围为 0.12% 至 39.3%(重量百分比),相对标准偏差为 0.6 - 3.6%。用 Metavak-AK 气体分析仪得出的结果的准确性得到了凯氏定氮法和杜马斯参考方法的证实。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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