Insight and Control of the Crystal Growth of Zeolitic Imidazolate Framework ZIF-67 by Atomic Force Microscopy and Mass Spectrometry,Crystal Growth & Design

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Insight and Control of the Crystal Growth of Zeolitic Imidazolate Framework ZIF-67 by Atomic Force Microscopy and Mass Spectrometry
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2018-01-08 00:00:00 , DOI: 10.1021/acs.cgd.7b01058
Raghidah Wagia ₁ , Ilya Strashnov ₁ , Michael W. Anderson ₁ , Martin P. Attfield ₁

Affiliation

Combination of electrospray ionization mass spectrometry (ESI-MS) and in situ atomic force microscopy (AFM) are applied to provide the first nanoscopic study of the crystal growth of zeolitic imidazolate framework ZIF-67. ZIF-67 is found to form through a process of nucleation and spreading of metastable unenclosed substeps to form stable surface steps of the enclosed framework structure and demonstrates that isostructural MOFs, ZIF-67 and ZIF-8, undergo identical crystal growth mechanisms. The information on the crystal growth species obtained from the AFM experiments correlates well with the solution species identified by ESI-MS indicating that the species involved in the growth under low supersaturation conditions are methylimidazole/methylimidazolate, monomeric nonmethylimidazole/methylimidazolate complexed Co²⁺ ions and monomeric complexed [Co(methylimidazole/methylimidazolate)_1-2] ions. Combination of the use of low supersaturation growth solutions and in situ AFM has also allowed the successful extraction of the synthetic conditions necessary for formation of ZIF-67 nanodots that possesses a maximum vertical dimension of 1.2 nm which is the smallest dimension reported for a stable ZIF-67 entity. This methodology may be expanded to understand the formation of, and to form, complex crystal forms of other MOFs for new or improved functionality.

中文翻译：

原子力显微镜和质谱对沸石咪唑盐骨架ZIF-67晶体生长的了解和控制

电喷雾电离质谱（ESI-MS）和原位原子力显微镜（AFM）的结合用于对沸石咪唑酸盐骨架ZIF-67的晶体生长进行首次纳米研究。发现ZIF-67是通过亚稳的非封闭子步骤的成核和扩散过程形成的，以形成封闭框架结构的稳定表面台阶，并证明同构MOF，ZIF-67和ZIF-8经历相同的晶体生长机制。从AFM实验获得的晶体生长物种的信息与通过ESI-MS鉴定的溶液物种非常相关，这表明在低过饱和条件下参与生长的物种是甲基咪唑/甲基咪唑化物，单体非甲基咪唑/甲基咪唑化物络合的Co ²⁺离子和单体络合的[Co（甲基咪唑/甲基咪唑酸酯）_1-2 ]离子。低过饱和度生长溶液的使用和原位原子力显微镜的结合还可以成功提取形成ZIF-67纳米点所需的合成条件，该纳米点的最大垂直尺寸为1.2 nm，这是稳定的ZIF所报道的最小尺寸-67实体。可以扩展此方法以了解其他MOF的形成和形成，以形成新的或改进的功能。

更新日期：2018-01-08

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