Fast Nucleation and Growth of ZIF‐8 Nanocrystals Monitored by Time‐Resolved In Situ Small‐Angle and Wide‐Angle X‐Ray Scattering

Cravillon, Janosch; Schröder, Christian; Nayuk, Roman; Gummel, Jérémie; Huber, Klaus; Wiebcke, Michael

doi:10.1002/ange.201102071

Cited by 61 publications

(41 citation statements)

References 54 publications

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“…The growth of ZIF-8 particles was successfully monitored by Patterson et al [16] in a careful in-situ liquid cell transmission electron microscopy (LC-TEM) study. It was demonstrated that particle growth is not a coalescence process, confirming the results of earlier in-situ small-angle and wide-angle X-ray scattering (SAXS/WAXS) experiments [17], and that particle growth is surface-reaction limited and not diffusion limited. The topotactic transformation of a layered zinc 2-methylimidazolate (ZIF-L) into ZIF-8 was investigated using various ex-situ methods as well as in-situ liquid-state 1 H NMR spectroscopy by Low et al [18].…”

Section: Introductionsupporting

confidence: 82%

The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms

Springer

Heidenreich

Stock

et al. 2016

Zeitschrift Für Kristallographie - Crystalline Materials

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Abstract:In this report, we summarize our theoretical and experimental investigations on the zeolitic imidazolate framework (ZIF) system [Zn(dcim) 2 ] (dcim = 4,5-dichloroimidazolate) that have been published recently. These comprise: (1) a theoretical study on hypothetical conformational [Zn(dcm) 2 ]-SOD polymorphs with the same underlying sodalite (SOD) topology but distinct dcim linker orientations, (2) a synthetic work that resulted in the experimental realization of the most stable predicted (trigonal) SOD-type framework conformer and improved synthetic protocols for a previously discovered cubic SOD-type material, (3) a detailed structural analysis of the trigonal and cubic SOD-type materials, (4) a comparative characterization of the SOD-type materials by gas physisorption measurements, (5) a synthetic work that resulted in the discovery of a complete series of intermediate frameworks with the trigonal and cubic SOD-type materials as the end members, and (6) time-resolved insitu light and stopped-flow synchrotron small-angle and wide-angle X-ray scattering experiments on the rapid crystallization of the RHO-type polymorph (ZIF-71). In addition, we report as yet unpublished work, concerning time-resolved in-situ angular-dispersive synchrotron X-ray diffraction experiments on RHO-/SOD-type phase selection via the coordination modulation approach during competitive formation of the RHO-type and SOD-type materials.

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Section: Introductionsupporting

confidence: 82%

The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms

Springer

Heidenreich

Stock

et al. 2016

Zeitschrift Für Kristallographie - Crystalline Materials

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“…2c and d for ZIF-8_A10 and ZIF-8_A30, respectively. This trend can be attributed to continuous growth of the existing nanoparticles through the attachment of monomers in the presence of an organic amine template [29]. In addition, we note that the mesoporous structures of ZIF-8_A1 and ZIF-8_A5 primarily result from interparticle void space, whereas the crystals of ZIF-8_A10 and ZIF-8_A30 are intrinsically mesoporous.…”

Section: Morphologies Of Hierarchical Porous Zif-8mentioning

confidence: 74%

“…In the initial stages, the organic amines act as protonation agents that deprotonate the organic ligands (e.g., 2-Im and methylimidazole (Im)), a key step in forming ZIFs rapidly [29]. Meanwhile, the protonated organic amines interact strongly with the ZIF ligands [7].…”

Section: Science China Materialsmentioning

confidence: 99%

Rapid room-temperature synthesis of hierarchical porous zeolitic imidazolate frameworks with high space-time yield

Duan

Xiao

et al. 2017

Sci. China Mater.

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Hierarchical porous zeolitic imidazolate frameworks (ZIFs) have potential for adsorption, catalysis and chemical sensing applications. Ultrafast synthesis of ZIFs at room temperature and pressure is particularly desirable for large-scale industrial production. Here, we developed a green and versatile method using organic amines as supramolecular templates (organic amine-template) to rapidly synthesize hierarchical porous ZIFs (ZIF-8, ZIF-61 and ZIF-90) at room temperature and pressure. The synthesis time was reduced dramatically to within 1 min, and the resulting ZIFs had multimodal hierarchical porous structures with mesopores/ macropores interconnected with micropores. Notably, the space-time yield (STY) of hierarchical porous ZIF-8 was up to 1.29×10 4 kg m -3 d -1 , which is more than three times higher than that reported using other methods. Furthermore, the morphologies and porosities of the produced ZIFs could be readily tuned by controlling the synthesis time or type of organic amine. The organic amine played two roles in the synthesis: (1) a protonation agent to deprotonate organic ligands, facilitating the formation of ZIF crystals, and (2) an structure directing agent to direct mesopore/macropore formation. The resulting hierarchical porous ZIF-8 exhibited enhanced uptake capacities and diffusion rates for guest molecules relative to its microporous counterpart. This work provides a new direction for the green and efficient synthesis of various hierarchical porous ZIFs with high STYs for a wide range of applications.

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“…This primary particle formation is characterized by a persistent nucleation of new particles and fast individual growth to a certain size (R g E 20 nm for ZIF-8, R g E 60 nm for ZIF-zni) which depends on the ZIF system and probably also on the particular synthesis conditions. As shown for ZIF-8 by in situ synchrotron SAXS/WAXS, 17 the primary particle nucleation and growth processes run on a time scale of seconds (or even faster) and involve transient formation of small prenucleation nanoclusters. Crystalline ZIF-8 domains are generated rapidly within about 20-35 s revealing the great propensity of this ZIF system to crystallize as confirmed by a number of further ex situ studies, 36 one of which indicated the transient coexistence of an amorphous phase.…”

Section: 20mentioning

confidence: 95%

In situ static and dynamic light scattering and scanning electron microscopy study on the crystallization of the dense zinc imidazolate framework ZIF-zni

Hikov

Schröder

Cravillon

et al. 2012

Phys. Chem. Chem. Phys.

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The kinetics and mechanism of crystallization of the dense zinc imidazolate framework with zni topology, from comparatively dilute methanol solutions containing Zn(NO 3 )Á6H 2 O and imidazole with variation of the zinc-to-imidazole ratio, were followed in situ by time-resolved static and dynamic light scattering. The light scattering data revealed that metastable primary particles of about 100 nm in diameter form rapidly upon mixing the component solutions. After a lag time that is dependent on the imidazole concentration, the primary particles aggregate into secondary particles by a monomer addition mechanism with the primary particles as the monomers. Complementary scanning electron microscopy revealed that further evolution of the secondary particles is a complex process involving polycrystalline intermediates, the non-spherical morphologies of which depend on the initial zinc-to-imidazole ratio. Time and location of the first appearance of crystalline order could so far not be established. The pure-phase ZIF-zni crystals obtained after 240 min are twins. The aspect ratio of the tetragonal crystals can be controlled via the zinc-to-imidazole ratio.

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Fast Nucleation and Growth of ZIF‐8 Nanocrystals Monitored by Time‐Resolved In Situ Small‐Angle and Wide‐Angle X‐Ray Scattering

Cited by 61 publications

References 54 publications

The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms

The ZIF system zinc(II) 4,5-dichoroimidazolate: theoretical and experimental investigations of the polymorphism and crystallization mechanisms

Rapid room-temperature synthesis of hierarchical porous zeolitic imidazolate frameworks with high space-time yield

In situ static and dynamic light scattering and scanning electron microscopy study on the crystallization of the dense zinc imidazolate framework ZIF-zni

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