Cryo-focused ion beam preparation of perovskite based solar cells for atom probe tomography.,PLOS ONE

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Cryo-focused ion beam preparation of perovskite based solar cells for atom probe tomography.
PLOS ONE ( IF 2.9 ) Pub Date : 2020-01-16 , DOI: 10.1371/journal.pone.0227920
Nicolás Alfonso Rivas _{1,

2,

3} , Aslihan Babayigit _{1,

2} , Bert Conings _{1,

2} , Torsten Schwarz ₃ , Andreas Sturm ₃ , Alba Garzón Manjón ₃ , Oana Cojocaru-Mirédin ₄ , Baptiste Gault _{3,

5} , Frank Uwe Renner ₁

Affiliation

Focused-ion beam lift-out and annular milling is the most common method used for obtaining site specific specimens for atom probe tomography (APT) experiments and transmission electron microscopy. However, one of the main limitations of this technique comes from the structural damage as well as chemical degradation caused by the beam of high-energy ions. These aspects are especially critical in highly-sensitive specimens. In this regard, ion beam milling under cryogenic conditions has been an established technique for damage mitigation. Here, we implement a cryo-focused ion beam approach to prepare specimens for APT measurements from a quadruple cation perovskite-based solar cell device with 19.7% efficiency. As opposed to room temperature FIB milling we found that cryo-milling considerably improved APT results in terms of yield and composition measurement, i.e. halide loss, both related to less defects within the APT specimen. Based on our approach we discuss the prospects of reliable atom probe measurements of perovskite based solar cell materials. An insight into the field evaporation behavior of the organic-inorganic molecules that compose the perovskite material is also given with the aim of expanding the applicability of APT experiments towards nano-characterization of complex organo-metal materials.

中文翻译：

基于钙钛矿的太阳能电池的低温聚焦离子束制备，用于原子探针层析成像。

聚焦离子束抬起和环形铣削是获取原子探针层析成像（APT）实验和透射电子显微镜的特定位置标本的最常用方法。然而，该技术的主要局限性之一是由于高能离子束引起的结构破坏以及化学降解。这些方面对于高度敏感的标本尤其重要。在这方面，在低温条件下进行离子束铣削已成为减轻损害的既定技术。在这里，我们实现了一种低温聚焦离子束方法，以效率为19.7％的四倍钙钛矿型太阳能电池装置为APT测量准备了样品。与室温FIB研磨相反，我们发现冷冻研磨在产率和成分测量方面显着改善了APT结果，即卤化物损失，这两者都与APT样品中较少的缺陷有关。基于我们的方法，我们讨论了钙钛矿基太阳能电池材料可靠的原子探针测量的前景。为了扩大APT实验向复杂有机金属材料的纳米表征的适用性，还对构成钙钛矿材料的有机无机分子的蒸发行为进行了深入研究。

更新日期：2020-01-17

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