<br>原始 MXene：使用 HCl+LiF 溶液进行 MAX 相蚀刻的原位 XRD 研究,Advanced Science

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原始 MXene：使用 HCl+LiF 溶液进行 MAX 相蚀刻的原位 XRD 研究
Advanced Science ( IF 14.3 ) Pub Date : 2024-10-30 , DOI: 10.1002/advs.202408448
Bartosz Gurzęda ₁ , Nicolas Boulanger ₁ , Andreas Nordenström ₁ , Catherine Dejoie ₂ , Alexandr V Talyzin ₁

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Ti-MXene 有许多应用，激发了人们对通过基于溶液的方法合成 Ti₃C₂T_x 的浓厚兴趣。然而，到目前为止，仅进行了合成的异位研究，主要是由于难以处理基于 HF 的溶液。在这里，报道了直接在 HF 溶液中使用塑料毛细管大小的反应池进行的 MXene 合成的首次时间分辨原位同步辐射 X 射线衍射研究。本研究首次报告了 Ti₃AlC₂ 与 LiF + HCl 刻蚀形成的“原始 MXene”结构。术语“原始”是指直接在 HF 溶液中发现的 MXene 结构。通过比较原始 MXene （≈13.5 Å）、无溶剂锂嵌入 MXene （≈12.2 Å）和无锂 MXene （≈10.7 Å）的层间距离，可以得出结论，在铝蚀刻过程中由端接 MX 层形成的“狭缝孔”的宽度不超过 ≈3 Å。这些狭缝孔隙的宽度是层内 Al 的 HF 蚀刻的关键因素。这种空间限制解释了基于 HF 的合成方法中 MXene 形成的缓慢动力学。没有观察到中间相，表明结晶 MXene 相是由 Al 的同时刻蚀和 Ti₃C₂ 层终止形成的。

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Pristine MXene: In Situ XRD Study of MAX Phase Etching with HCl+LiF Solution

Many applications are suggested for Ti-MXene motivating strong interest in studies of Ti₃C₂T_x synthesis by solution-based methods. However, so far only ex situ studies of the synthesis are performed, mostly due to the difficulty of handling HF-based solutions. Here the first time-resolved in situ synchrotron radiation X-ray Diffraction study of MXene synthesis performed using a plastic capillary-size reaction cell directly in HF solution is reported. This study provides the first report on the structure of “pristine MXene” formed by Ti₃AlC₂ etching with LiF+HCl. The term “pristine” refers to the MXene structure found directly in HF solution. By comparing the interlayer distances of pristine MXene (≈13.5 Å), solvent-free Li-intercalated MXene (≈12.2 Å), and Li-free MXene (≈10.7 Å), it can be concluded that the width of “slit pores” formed by terminated MX layers during the Al etching does not exceed ≈3 Å. The width of these slit pores is a key factor for HF etching of Al within the interlayers. This space constraint explains the slow kinetics of MXene formation in HF-based synthesis methods. No intermediate phases are observed, suggesting that the crystalline MXene phase is formed by the simultaneous etching of Al and termination of Ti₃C₂ layers.

更新日期：2024-10-30

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