Description of a flexible cell for in situ X-ray and far-IR characterization of the surface of powdered materials

Lamberti, Carlo; Prestipino, Carmelo; Bordiga, Silvia; Berlier, Gloria; Spoto, G.; Zecchina, Adriano; Laloni, A.; Manna, F.; D’Anca, F.; Felici, Roberto; d’Acapito, Francesco; Roy, P.

doi:10.1016/s0168-583x(02)01719-6

Cited by 57 publications

(58 citation statements)

References 33 publications

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“…Ionization chambers measuring I 0 and I 1 were optimized to have, at 18 keV, an absorption efficiency of 15 and 50%, respectively. UiO-67, in the form of self-supported pellets of optimized thickness, was located inside an ad hoc conceived cell 76 and measured in its desolvated form.…”

Section: Atrmentioning

confidence: 99%

H₂storage in isostructural UiO-67 and UiO-66 MOFs

Chavan

Vitillo

Gianolio

et al. 2012

Phys. Chem. Chem. Phys.

451

356

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The recently discovered UiO-66/67/68 class of isostructural metallorganic frameworks (MOFs) [J. H. Cavka et al. J. Am. Chem. Soc., 2008, 130, 13850] has attracted great interest because of its remarkable stability at high temperatures, high pressures and in the presence of different solvents, acids and bases [L. Valenzano et al. Chem. Mater., 2011, 23, 1700]. UiO-66 is obtained by connecting Zr(6)O(4)(OH)(4) inorganic cornerstones with 1,4-benzene-dicarboxylate (BDC) as linker resulting in a cubic MOF, which has already been successfully reproduced in several laboratories. Here we report the first complete structural, vibrational and electronic characterization of the isostructural UiO-67 material, obtained using the longer 4,4'-biphenyl-dicarboxylate (BPDC) linker, by combining laboratory XRPD, Zr K-edge EXAFS, TGA, FTIR, and UV-Vis studies. Comparison between experimental and periodic calculations performed at the B3LYP level of theory allows a full understanding of the structural, vibrational and electronic properties of the material. Both materials have been tested for molecular hydrogen storage at high pressures and at liquid nitrogen temperature. In this regard, the use of a longer ligand has a double benefit: (i) it reduces the density of the material and (ii) it increases the Langmuir surface area from 1281 to 2483 m(2) g(-1) and the micropore volume from 0.43 to 0.85 cm(3) g(-1). As a consequence, the H(2) uptake at 38 bar and 77 K increases from 2.4 mass% for UiO-66 up to 4.6 mass% for the new UiO-67 material. This value is among the highest values reported so far but is lower than those reported for MIL-101, IRMOF-20 and MOF-177 under similar pressure and temperature conditions (6.1, 6.2 and 7.0 mass%, respectively) [A. G. Wong-Foy et al. J. Am. Chem. Soc., 2006, 128, 3494; M. Dinca and J. R. Long. Angew. Chem., Int. Ed., 2008, 47, 6766]. Nevertheless the remarkable chemical and thermal stability of UiO-67 and the absence of Cr in its structure would make this material competitive.

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Section: Atrmentioning

confidence: 99%

H₂storage in isostructural UiO-67 and UiO-66 MOFs

Chavan

Vitillo

Gianolio

et al. 2012

Phys. Chem. Chem. Phys.

451

356

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“…All XAS spectra were measured employing a home-made cell allowing sample activation in temperature and gas dosage under in situ or operando conditions, 97 monitoring the evolution of the XAS features while controlling the temperature and gas feed. The XAS data reduction and EXAFS extraction procedure was performed using the Athena codes.…”

Section: Pt L 3 -And Cu K-edge Xas Data Collections Exafs Data Analysismentioning

confidence: 99%

Tuning Pt and Cu sites population inside functionalized UiO-67 MOF by controlling activation conditions

et al. 2017

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The exceptional thermal and chemical stability of the UiO-66, -67 and -68 classes of isostructural MOFs [J. Am. Chem. Soc., 2008, 130, 13850] makes them ideal materials for functionalization purposes aimed at introducing active centres for potential application in heterogeneous catalysis. We previously demonstrated that a small fraction (up to 10%) of the linkers in the UiO-67 MOF can be replaced by bipyridine-dicarboxylate (bpydc) moieties exhibiting metal-chelating ability and enabling the grafting of Pt(ii) and Pt(iv) ions in the MOF framework [Chem. Mater., 2015, 27, 1042] upon interaction with PtCl or PtCl precursors. Herein we extend this functionalization approach in two directions. First, we show that by controlling the activation of the UiO-67-Pt we can move from a material hosting isolated Pt(ii) sites anchored to the MOF framework with Pt(ii) exhibiting two coordination vacancies (potentially interesting for C-H bond activation) to the formation of very small Pt nanoparticles hosted inside the MOF cavities (potentially interesting for hydrogenation reactions). The second direction consists of the extension of the approach to the insertion of Cu(ii), obtained via interaction with CuCl, and exhibiting interesting redox properties. All materials have been characterized by in situ X-ray absorption spectroscopy at the Pt L- and Cu K-edges.

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“…Nowadays, third generation sources allow acquisition time on the (sub)second scale, opening a brand-new range of possibilities for multi-scale time-resolved characterization. A variety of complex sample environments and in situ cells can be employed to "penetrate the black box" [76,318,535,536] in which the reaction is evolving. Synchrotron SAXS setups developed for time-dependent studies [291,537] allowed for instance to monitor crystallizations processes [288,289,291,538] and self-assembly phenomena [539], and to determine transient intermediates in biomolecules folding [540].…”

Section: X-ray Scattering Techniques Applied To Disordered and Partiamentioning

confidence: 99%

Determination of the electronic and structural configuration of coordination compounds by synchrotron-radiation techniques

Garino

Borfecchia

Gobetto

et al. 2014

Coordination Chemistry Reviews

102

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Description of a flexible cell for in situ X-ray and far-IR characterization of the surface of powdered materials

Cited by 57 publications

References 33 publications

H₂storage in isostructural UiO-67 and UiO-66 MOFs

H₂storage in isostructural UiO-67 and UiO-66 MOFs

Tuning Pt and Cu sites population inside functionalized UiO-67 MOF by controlling activation conditions

Determination of the electronic and structural configuration of coordination compounds by synchrotron-radiation techniques

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Description of a flexible cell for in situ X-ray and far-IR characterization of the surface of powdered materials

Cited by 57 publications

References 33 publications

H2storage in isostructural UiO-67 and UiO-66 MOFs

H2storage in isostructural UiO-67 and UiO-66 MOFs

Tuning Pt and Cu sites population inside functionalized UiO-67 MOF by controlling activation conditions

Determination of the electronic and structural configuration of coordination compounds by synchrotron-radiation techniques

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Product

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H₂storage in isostructural UiO-67 and UiO-66 MOFs

H₂storage in isostructural UiO-67 and UiO-66 MOFs