Solvothermal synthesis of new metal organic framework structures in the zinc–terephthalic acid–dimethyl formamide system

Clausen, Henrik F.; Poulsen, Rasmus D.; Bond, Andrew D.; Chevallier, Marie-Agnes; Iversen, Bo B.

doi:10.1016/j.jssc.2005.08.013

Cited by 135 publications

(95 citation statements)

References 22 publications

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“…However, in MOF-2, the square-grid layers are held together by hydrogen bonding between water and two adjacent paddlewheels, with the oxygen of H 2 O bound to the Zn atom and the H of the same H 2 O molecule bound to the carboxylate oxygen of the adjacent paddlewheel structure. 80,81 The XRD data of Zn(bdc)(ted) 0.5 shown in Fig. 8 clearly shows that the frameworks transform into MOF-2 after hydration.…”

Section: Zn(bdc)(ted) 05mentioning

confidence: 97%

Stability and Hydrolyzation of Metal Organic Frameworks with Paddle-Wheel SBUs upon Hydration

et al. 2012

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Instability of most prototypical metal organic frameworks (MOFs) in the presence of moisture is always a limitation for industrial scale development. In this work, we examine the dissociation mechanism of microporous paddle wheel frameworks M(bdc)(ted) 0.5 [M=Cu, Zn, Ni, Co; bdc= 1,4-benzenedicarboxylate; ted= triethylenediamine] in controlled humidity environments. Combined in-situ IR spectroscopy, Raman, and Powder x-ray diffraction measurements show that the stability and modification of isostructual M(bdc)(ted) 0.5 compounds upon exposure to water vapor critically depend on the central metal ion. A hydrolysis reaction of water molecules with Cu-O-C is observed in the case of Cu(bdc)(ted) 0.5 . Displacement reactions of ted linkers by water molecules are identified with Zn(bdc)(ted) 0.5 and Co(bdc)(ted) 0.5 . In contrast, . Ni(bdc)(ted) 0.5 is less susceptible to reaction with water vapors than the other three compounds. In addition, the condensation of water vapors into the framework is necessary to initiate the dissociation reaction. These findings, supported by supported by first principles theoretical van der Waals density functional (vdW-DF) calculations of overall reaction enthalpies, provide the necessary information for determining operation conditions of this class of MOFs with paddle wheel secondary building units and guidance for developing more robust units.

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Section: Zn(bdc)(ted) 05mentioning

confidence: 97%

Stability and Hydrolyzation of Metal Organic Frameworks with Paddle-Wheel SBUs upon Hydration

et al. 2012

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“…24 DMF is a solvent commonly used in liquid phase synthesis of MOFs. 1,7 In order to recrystallize the unknown phase into IRMOF-8, the films were placed in an autoclave with DMF. After 120 min at 150 C, GIXRD revealed a structure matching to IRMOF-8 (Fig.…”

Section: A121-mentioning

confidence: 99%

“…[1][2][3][4][5][6] The most common method for synthetizing MOFs in the bulk form has been solvothermal growth in mother solution containing the precursors. 1,7 However, depositing MOFs in thin film form creates new challenges for the growth methods. Thin films could open up new application areas for MOFs, including electronics, magnetics, and optics.…”

Section: Introductionmentioning

confidence: 99%

Studies on atomic layer deposition of IRMOF-8 thin films

Salmi

Heikkilä

Vehkamäki

et al. 2014

Journal of Vacuum Science &Amp; Technology A: Vacuum, Surfaces, and Films

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Deposition of IRMOF-8 thin films by atomic layer deposition was studied at 260–320 °C. Zinc acetate and 2,6-naphthalenedicarboxylic acid were used as the precursors. The as-deposited amorphous films were crystallized in 70% relative humidity at room temperature resulting in an unknown phase with a large unit cell. An autoclave with dimethylformamide as the solvent was used to recrystallize the films into IRMOF-8 as confirmed by grazing incidence x-ray diffraction. The films were further characterized by high temperature x-ray diffraction (HTXRD), field emission scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), time-of-flight elastic recoil detection analysis (TOF-ERDA), nanoindentation, and energy-dispersive x-ray spectroscopy. HTXRD measurements revealed similar behavior to bulk IRMOF-8. According to TOF-ERDA and FTIR, composition of the films was similar to IRMOF-8. Through-porosity was confirmed by loading the films with palladium using Pd(thd)2 (thd = 2,2,6,6-tetramethyl-3,5-heptanedionato) as the precursor.

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“…[15] Other groups have used electrochemical methods to speed up the synthesis. [16] Although the structure of MOF-2 and some of the associated polymorphs are well studied, [17,18] we know of no equivalent high-throughput syntheses for the isostructural copper terephthalate. Along similar lines to that used for MOF-2, we have used dmf at elevated temperatures to carry out the reaction shown in Equation (1).…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Structure Characterization of Copper Terephthalate Metal–Organic Frameworks

et al. 2009

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In this paper, we report on a high‐throughput (gram quantities) solvothermal method for the synthesis of copper terephthalate metal–organic frameworks in dmf. While the structure of MOF‐2 and some of the associated polymorphs are well known, we know of no equivalent structural studies for the isostructural copper terephthalate (Cu–tpa). The material we have made crystallizes in the C2/m space group. Cu–tpa also exhibits reversible solvent‐exchange properties. These properties make this material useful for potential applications in gas storage and catalysis applications. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)

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Solvothermal synthesis of new metal organic framework structures in the zinc–terephthalic acid–dimethyl formamide system

Cited by 135 publications

References 22 publications

Stability and Hydrolyzation of Metal Organic Frameworks with Paddle-Wheel SBUs upon Hydration

Stability and Hydrolyzation of Metal Organic Frameworks with Paddle-Wheel SBUs upon Hydration

Studies on atomic layer deposition of IRMOF-8 thin films

Synthesis and Structure Characterization of Copper Terephthalate Metal–Organic Frameworks

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