Mo-W-containing tetragonal tungsten bronzes through isomorphic substitution of molybdenum by tungsten

Mixed metal oxides based in Mo(W)–Nb–V–Te with tetragonal tungsten bronze (TTB) structure have been synthesized by a hydrothermal method from aqueous solutions of the corresponding Keggin-type heteropolyacids and further heat-treatment in N2 at 700 ◦ C. The materials have been characterized by several physico-chemical techniques, i.e. XRD, Raman, FTIR, SEM-EDS, and TEM. This procedure allows controlling the chemical species to be distributed in the different interstices of the TTB skeleton, which is a key factor to regulate the catalytic properties of the final solid. In this sense, the isomorphic replacement of Mo by W results in lattice parameter and crystal morphology variation, although…

Use of alkylarsonium directing agents for the synthesis and study of zeolites

[EN] Expanding the previously known family of -onium (ammonium, phosphonium, and sulfonium) organic structure-directing agents (OSDAs) for the synthesis of zeolite MFI, a new member, the arsonium cation, is used for the first time. The new group of tetraalkylarsonium cations has allowed the synthesis of the zeolite ZSM-5 with several different chemical compositions, opening a route for the synthesis of zeolites with a new series of OSDA. Moreover, the use of As replacing N in the OSDA allows the introduction of probe atoms that facilitate the study of these molecules by powder X-ray diffraction (PXRD), solid-state nuclear magnetic resonance (MAS NMR), and X-ray absorption spectroscopy (XAS)…

Meltable, Glass-Forming, Iron Zeolitic Imidazolate Frameworks

An Ultrahigh CO2-Loaded Silicalite-1 Zeolite: Structural Stability and Physical Properties at High Pressures and Temperatures

[EN] We report the formation of an ultrahigh CO2-loaded pure-SiO2, silicalite-1 structure at high pressure (0.7 GPa) from the interaction of empty zeolite and fluid CO, medium. The CO2-filled structure was characterized in situ by means of synchrotron powder X-ray diffraction. Rietveld refinements and Fourier recycling allowed the location of 16 guest carbon dioxide molecules per unit cell within the straight and sinusoidal channels of the porous framework to be analyzed. The complete filling of pores by CO, molecules favors structural stability under compression, avoiding pressure-induced amorphization below 20 GPa, and significantly reduces the compressibility of the system compared to th…

Insights into the formation of metal carbon nanocomposites for energy storage using hybrid NiFe layered double hydroxides as precursors

[EN] NiFe-carbon magnetic nanocomposites prepared using hybrid sebacate intercalated layered double hydroxides (LDHs) as precursors are shown to be of interest as supercapacitors. Here, the low-temperature formation mechanism of these materials has been deciphered by means of a combined study using complementaryin situ(temperature-dependent) techniques. Specifically, studies involving X-ray powder diffraction, thermogravimetry coupled to mass spectrometry (TG-MS), statistical Raman spectroscopy (SRS), aberration-corrected scanning transmission electron microscopy (STEM) and electron energy-loss spectroscopy (EELS) have been carried out. The experimental results confirm the early formation o…

Cobalt Metal-Organic Framework based on two dinuclear secondary building units for electrocatalytic oxygen evolution

[EN] The synthesis of a new microporous metal-organic framework (MOF) based on two secondary building units, with dinuclear cobalt centers, has been developed. The employment of a well-defined cobalt cluster results in an unusual topology of the Co-2-MOF, where one of the cobalt centers has three open coordination positions, which has no precedent in MOF materials based on cobalt. Adsorption isotherms have revealed that Co-2-MOF is in the range of best CO2 adsorbents among the carbon materials, with very high CO2/CH4 selectivity. On the other hand, dispersion of Co-2-MOF in an alcoholic solution of Nafion gives rise to a composite (Co-2-MOF@Nafion) with great resistance to hydrolysis in aqu…

Stimuli-responsive hybrid materials: breathing in magnetic layered double hydroxides induced by a thermoresponsive molecule

[EN] A hybrid magnetic multilayer material of micrometric size, with highly crystalline hexagonal crystals consisting of CoAl-LDH ferromagnetic layers intercalated with thermoresponsive 4-(4-anilinophenylazo)benzenesulfonate (AO5) molecules diluted (ratio 9 : 1) with a flexible sodium dodecylsulphate (SDS) surfactant has been obtained. The resulting material exhibits thermochromism attributable to the isomerization between the azo (prevalent at room temperature) and the hydrazone (favoured at higher temperatures) tautomers, leading to a thermomechanical response. In fact, these crystals exhibited thermally induced motion triggering remarkable changes in the crystal morphology and volume. In…

Synthesis and Structure Determination of the Hierarchical Meso-Microporous Zeolite ITQ-43

[EN] The formation of mesopores in microporous zeolites is generally performed by postsynthesis acid, basic, and steam treatments. The hierarchical pore systems thus formed allow better adsorption, diffusion, and reactivity of these materials. By combining organic and inorganic structure-directing agents and high-throughput methodologies, we were able to synthesize a zeolite with a hierarchical system of micropores and mesopores, with channel openings delimited by 28 tetrahedral atoms. Its complex crystalline structure was solved with the use of automated diffraction tomography.

Synthesis of a novel zeolite through a pressure-induced reconstructive phase transition process

et al.

Photo-switching in a hybrid material made of magnetic layered double hydroxides intercalated with azobenzene molecules.

Financial support from the EU (Projects HINTS FP7-263104-2 and SpinMol Advanced Grant ERC-2009-AdG-20090325), the Spanish Ministerio de Economia y Competitividad (Projects with FEDER cofinancing MAT 2009-14528-C02-01, MAT2011-22785, MAT2012-38567-C02-01, CTQ-2011-26507, Consolider-Ingenio in Molecular Nanoscience CSD2007-00010, Consolider-Ingenio 2010-Multicat CSD2009-00050, and Severo Ochoa Program SEV-2012-0267), Generalitat Valenciana (PROMETEO and ISIC-Nano programs), and VLC/Campus Microcluster "Functional Nanomaterials and Nanodevices" is gratefully acknowledged. C. M. G. thanks the Spanish MINECO for a Ramon y Cajal Fellowship (RYC-2012-10894). We also acknowledge P. Atienzar and J. …

Structural evolution of CO2 filled pure silica LTA zeolite under high-pressure high-temperature conditions

[EN] The crystal structure of CO2-filled pure-SiO2 LTA zeolite has been studied at high pressures and temperatures using synchrotron-based X-ray powder diffraction. Its structure consists of 13 CO2 guest molecules, 12 of them accommodated in the large alpha-cages and one in the beta-cages, giving a SiO2/CO2 stoichiometric ratio smaller than 2. The structure remains stable under pressure up to 20 GPa with a slight pressure-dependent rhombohedral distortion, indicating that pressure-induced amorphization is prevented by the insertion of guest species in this open framework. The ambient temperature lattice compressibility has been determined. In situ high-pressure resistive-heating experiments…

Correspondence: Strongly-driven Re+CO2 redox reaction at high-pressure and high-temperature.

Correspondence: Strongly-driven Re+CO 2 redox reaction at high-pressure and high-temperature

Gas confinement in compartmentalized coordination polymers for highly selective sorption

Discrimination between different gases is an essential aspect for industrial and environmental applications involving sensing and separation. Several classes of porous materials have been used in this context, including zeolites and more recently MOFs. However, to reach high selectivities for the separation of gas mixtures is a challenging task that often requires the understanding of the specific interactions established between the porous framework and the gases. Here we propose an approach to obtain an enhanced selectivity based on the use of compartmentalized coordination polymers, named CCP-1 and CCP-2, which are crystalline materials comprising isolated discrete cavities. These compar…

CCDC 1473649: Experimental Crystal Structure Determination

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CCDC 1473650: Experimental Crystal Structure Determination

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CCDC 1439097: Experimental Crystal Structure Determination

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CCDC 1439096: Experimental Crystal Structure Determination

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CCDC 1473652: Experimental Crystal Structure Determination

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CCDC 1473653: Experimental Crystal Structure Determination

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