期刊
ADVANCED MATERIALS INTERFACES
卷 10, 期 12, 页码 -出版社
WILEY
DOI: 10.1002/admi.202202461
关键词
chemical vapor deposition; Heavy Atom Method; metal-organic frameworks; Patterson functions; polymorphism
Chemical vapor deposition is used to prepare thin films of a copper-isonicotinate (Cu-INA) metal-organic framework (MOF). The crystalline order of the precursor layer strongly influences the texture of Cu-INA thin films. A novel methodology combining synchrotron grazing incidence X-ray diffraction (GIXRD) data with Patterson functions is introduced to determine the structure of an unknown thin-film MOF polymorph.
The preparation of thin films is often associated with the appearance of unknown polymorphs, as both the substrate and deposition method can heavily influence crystallization processes. Here, chemical vapor deposition is used to obtain thin films of a copper-isonicotinate (Cu-INA) metal-organic framework (MOF). Starting from copper-based precursor layers (copper oxide and hydroxide), a solid-vapor conversion with vaporized isonicotinic acid in either a dry or humidified atmosphere, yields a new Cu-INA MOF polymorph. It is found that the crystalline order of the precursor layer has a strong impact on the texture of Cu-INA thin films. Furthermore, a novel methodology is introduced to determine the structure of a previously unknown thin-film phase of Cu-INA. Although only a few diffraction peaks are found via synchrotron grazing incidence X-ray diffraction (GIXRD), a triclinic unit cell can be determined, and Patterson functions can be calculated. The latter reveals the position of the copper atoms within the unit cell and the alignment of the INA linkers defining the coordination network structure. This work introduces how the combination of GIXRD data with Patterson functions can be used to identify the structure of an unknown thin-film MOF polymorph.
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