本文關(guān)鍵詞： 激光剝蝕-電感耦合等離子體質(zhì)譜法(LA-ICP-MS) 固態(tài)電遷移 統(tǒng)計分布分析 稀土材料 鏑　出處：《冶金分析》2017年05期 　論文類型：期刊論文

【摘要】：高效、高靈敏度的原位微區(qū)分析技術(shù)開發(fā)對于固態(tài)電遷移等稀土提純工藝具有重要意義。實驗以固態(tài)電遷移提純后金屬鏑棒為研究對象,將激光剝蝕-電感耦合等離子體質(zhì)譜法(LA-ICP-MS)應(yīng)用于高純稀土金屬的微區(qū)分布分析。研究了激光剝蝕速率對樣品覆蓋率和分析時間的影響,確定了剝蝕速率為50μm/s;考察了剝蝕池及ICP-MS載氣流量對待測元素信號強度、氧化物產(chǎn)率及元素分餾效應(yīng)的影響,確定了載氣流量分別為0.60L/min(He)和1.0L/min(Ar)。采用線掃描方式,以基體元素~(158)Dy為內(nèi)標(biāo),獲得了不同電遷移區(qū)域各雜質(zhì)元素的二維相對強度分布圖,初步探究了各雜質(zhì)元素的遷移規(guī)律。結(jié)果顯示:在電遷移過程中,Al、Si、Ti、Fe、Mo、W元素從陰極向陽極遷移;Ni、Cu元素從中間區(qū)域向兩極遷移。這一遷移趨勢與輝光放電質(zhì)譜法(GD-MS)分析結(jié)果相一致。同時,LA-ICP-MS還得到更豐富的微區(qū)統(tǒng)計分布信息。不同電遷移區(qū)域各雜質(zhì)元素最大偏析度、相對標(biāo)準(zhǔn)偏差(RSD)值及最大偏析位置進(jìn)一步揭示了各元素的遷移狀態(tài),可能與固態(tài)電遷移工藝相聯(lián)系。因此,LA-ICPMS有望為稀土金屬提純工藝解析及優(yōu)化提供一種新的有效分析手段。
[Abstract]:The development of high efficiency and high sensitivity in situ microanalysis technology is of great significance for the solid state electromigration and other rare earth purification processes. The laser denudation-inductively coupled plasma-mass spectrometry (LICP-MS) was applied to analyze the microdistribution of high purity rare earth metals. The effect of laser denudation rate on sample coverage and analysis time was studied. The denudation rate was determined to be 50 渭 m / s, and the effects of denudation tank and ICP-MS carrier gas flow rate on signal intensity, oxide yield and elemental fractionation effect were investigated. The carrier gas flow rates were 0.60 L 路min ~ (-1) and 1.0 L ~ (-1) 路min ~ (-1) 路min ~ (-1), respectively. The two-dimensional relative strength distribution of impurity elements in different electromigration regions has been obtained by using the matrix element, 158Dy, as the internal standard, and the relative strength distribution of the impurity elements in different electromigration regions has been obtained. The migration rules of various impurity elements were preliminarily investigated. The results showed that the elements of AlAlSiSiTiTiFeMoMoW migrated from cathode to anode from the middle region to the two poles. This migration trend and GD-MSanalysis by Glow discharge Mass Spectrometry (GD-MS) showed that the Cu element was transferred from the cathode to the anode. The results are consistent. At the same time, LA-ICP-MS also gets more information of statistical distribution of microregions. The maximum segregation degree of impurity elements in different electromigration regions is also obtained. The relative standard deviation (RSD) value and the maximum segregation position further reveal the migration state of each element, which may be related to the solid state electromigration process. Therefore, LA-ICPMS is expected to provide a new and effective analytical method for the analysis and optimization of rare earth metal purification process.
【作者單位】： 鋼鐵研究總院金屬材料表征北京市重點實驗室;北京有色金屬研究總院稀土材料國家工程研究中心;
【基金】：國家重點研發(fā)計劃材料基因工程關(guān)鍵技術(shù)與支撐平臺專項(2016YFB0700302)
【分類號】：TG115.33

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本文編號：1519535