Cleaning of tungsten tips for subsequent use as cold field emitters or STM probes

Zuzana Košelová, Lenka Horáková, D. Burda, Mohammad M. Allaham, A. Knápek, Z. Fohlerova
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Abstract

This study investigates the crucial process of cleaning cold field emission electron emitters and scanning tunnel microscopy (STM) probes, particularly focusing on tungsten tips. The cleanliness of these tips is essential for maintaining optimal cathode properties, preventing impurities that can significantly affect the emission process. Various cleaning methods, including macroetching, ammonia cleaning, and hydrofluoric acid (HF) cleaning were explored and compared by scanning electron microscopy. The macroetching method, involving a mixture of hydrochloric acid, nitric acid, and hydrogen fluoride, proved to be too reactive, causing significant material removal and altering the tip’s structure. Ammonia cleaning did not significantly improve or harm the samples. However, oxide islands appeared in some areas, suggesting the potential formation of ammonium tungsten oxide. HF cleaning, specifically at 20% and 50% concentrations, demonstrated effectiveness in removing tungsten oxides without damaging the tip. Pre-cleaning with water and ethanol proved beneficial for subsequent HF refinement. Results suggest that HF is the most suitable method for oxide removal but a rinse with water is essential for removing residual sodium hydroxide. To maintain optimal properties, it is crucial to apply a less reactive layer quickly or transfer the tips to a water/ethanol bath to prevent oxidation.
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清洗钨针尖,以便随后用作冷场发射器或 STM 探针
本研究探讨了清洁冷场发射电子发射器和扫描隧道显微镜(STM)探针的关键过程,尤其是钨针尖的清洁。这些针尖的清洁度对于保持最佳阴极性能、防止杂质严重影响发射过程至关重要。我们通过扫描电子显微镜探索并比较了各种清洁方法,包括宏观蚀刻、氨水清洁和氢氟酸(HF)清洁。宏蚀刻法涉及盐酸、硝酸和氟化氢的混合物,被证明反应性太强,会导致大量材料脱落并改变针尖的结构。氨水清洗没有明显改善或损害样品。不过,某些区域出现了氧化物岛,表明可能形成了氧化钨铵。高频清洗,特别是浓度为 20% 和 50% 的高频清洗,在去除钨氧化物的同时不会损坏针尖。事实证明,用水和乙醇进行预清洁有利于随后的高频细化。结果表明,高频是去除氧化物的最合适方法,但用水冲洗对去除残留氢氧化钠至关重要。为了保持最佳性能,必须快速涂抹活性较低的涂层,或将针尖转移到水/乙醇浴中,以防止氧化。
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