Engineering Papers⌕ Search

Engineering topics

Wang, Timothy C.

Publications and source records attributed to Wang, Timothy C..

At least 19 records

Surviving Under Pressure: The Role of Solvent, Crystal Size, and Morphology During Pelletization of Metal–Organic Frameworks

As metal–organic frameworks (MOFs) gain traction for applications, such as hydrogen storage, it is essential to form the as-synthesized powder materials into shaped bodies with high packing densities to maximize their volumetric performance. Mechanical compaction, which involves compressing the materials at high pressure, has been reported to yield high monolith density but often results in a significant loss in accessible porosity. Herein, we sought to systematically control (1) crystal size, (2) solvation, and (3) compacting pressure in the pelletization process to achieve high packing density without compromising the porosity that makes MOFs functional. It was determined that solvation is the most critical factor among the three factors examined. Solvation that exceeds the pore volume prevents the framework from collapsing, allowing for porosity to be maintained through pelletization. Higher pelletization pressure results in higher packing density, with extensive loss of porosity being observed at a higher pressure if the solvation is below the pore volume. Lastly, we observed that the morphology and size of the MOF particles result in variation in the highest achievable packing efficiency, but these numbers (75%) are still greater than many existing techniques used to form MOFs. Furthermore, we concluded that the application of pressure through pelletization is a suitable and widely applicable technique for forming high-density MOF-monoliths.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Charge Transport in Zirconium-Based Metal–Organic Frameworks

Metal–organic frameworks (MOFs) are a class of crystalline porous materials characterized by inorganic nodes and multitopic organic linkers. Because of their molecular-scale porosity and periodic intraframework chemical functionality, MOFs are attractive scaffolds for supporting and/or organizing catalysts, photocatalysts, chemical-sensing elements, small enzymes, and numerous other functional-property-imparting, nanometer-scale objects. Notably, these objects can be installed after the synthesis of the MOF, eliminating the need for chemical and thermal compatibility of the objects with the synthesis milieu. Thus, postsynthetically functionalized MOFs can present three-dimensional arrays of high-density, yet well-separated, active sites. Depending on the application and corresponding morphological requirements, MOF materials can be prepared in thin-film form, pelletized form, isolated single-crystal form, polycrystalline powder form, mixed-matrix membrane form, or other forms. For certain applications, most obviously catalytic hydrolysis and electro- or photocatalytic water splitting, but also many others, an additional requirement is water stability. MOFs featuring hexa-zirconium(IV)-oxy nodes satisfy this requirement. For applications involving electrocatalysis, charge storage, photoelectrochemical energy conversion, and chemiresistive sensing, a further requirement is electrical conductivity, as embodied in electron or hole transport. As most MOFs, under most conditions, are electrically insulating, imparting controllable charge-transport behavior is both a chemically intriguing and chemically compelling challenge. Herein, we describe three strategies to render zirconium-based metal–organic frameworks (MOFs) tunably electrically conductive and, therefore, capable of transporting charge on the few nanometers (i.e., several molecular units) to few micrometers (i.e., typical dimensions for MOF microcrystallites) scale. The first strategy centers on redox-hopping between periodically arranged, chemically equivalent sites, essentially repetitive electron (or hole) self-exchange. Zirconium nodes are electrically insulating, but they can function as grafting sites for (a) redox-active inorganic clusters or (b) molecular redox couples. Alternatively, charge hopping based on linker redox properties can be exploited. Marcus’s theory of electron transfer has proven useful for understanding/predicting trends in redox-hopping based conductivity, most notably, in accounting for variations as great as 3000-fold depending on the direction of charge propagation through structurally anisotropic MOFs. In MOF environments, propagation of electronic charge via redox hopping is necessarily accompanied by movement of charge-compensating ions. Consequently, rates of redox hopping can depend on both the identity and concentration of ions permeating the MOF. In the context of electrocatalysis, an important goal is to transport electronic charge fast enough to match or exceed the inherent activity of MOF-based or MOF-immobilized catalysts. Bandlike electronic conductivity is the focus of an alternative strategy: one based on the introduction of molecular guests capable of forming donor–acceptor charge transfer complexes with the host framework. Theory again can be applied predictively to alter conductivity. A third strategy similarly emphasizes electronic conductivity, but it makes use of added bridges in the form of molecular oligomers or inorganic clusters that can then be linked to span the length of a MOF crystallite. For all strategies, retention of molecular-scale porosity is emphasized, as this property is key to many applications. Lastly, while our focus is on Zr-MOFs, the described approaches clearly are extendable to other MOF compositions, as has already been demonstrated, in part, in studies by others.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Imaging the Phase Evolution of the Li-N-H Hydrogen Storage System

Complex metal hydrides provide high-density hydrogen storage, which is essential for vehicular applications. However, the utility of these materials has been limited by thermodynamic and kinetic barriers present during the dehydrogenation and rehydrogenation processes as new phases form inside parent phases. Better understanding of the mixed-phase mesostructures and their interfaces may assist in improving cyclability. In this work, the evolution of the phases during hydrogenation of lithium nitride and dehydrogenation of lithium amide with lithium hydride are probed with scanning-transmission X-ray microscopy at the nitrogen K edge. With this technique, intriguing core-shell structures were observed in particles of both partially hydrogenated Li 3 N and partially dehydrogenated LiNH 2 + 2 LiH. The potential contributions of both internal hydrogen mobility and interfacial energies on the generation of these structures are discussed.

08 HYDROGEN↗

Design Rules for Metal‐Organic Framework Stability in High‐Pressure Hydrogen Environments

Abstract Stability of metal‐organic frameworks (MOFs) under hydrogen is of particular importance for a diverse range of applications, including catalysis, gas separations, and hydrogen storage. Hydrogen in gaseous form is known to be a strong reducing agent and can potentially react with the secondary building units of a MOF and decompose the porous framework structure. Moreover, rapid pressure swings expected in vehicular hydrogen storage could create significant mechanical stresses within MOF crystals that cause partial or complete pore collapse. In this work, we examined the stability of a structurally representative suite of MOFs by testing them under both static (70 MPa) and dynamic hydrogen exposure (0.5 to 10 MPa, 1000 pressure cycles) at room temperature. We aim to provide stability information for development of near room‐temperature hydrogen storage media based on MOFs and suggest framework design rules to avoid materials unstable for hydrogen storage under relevant technical conditions.

Wang, Timothy C.↗

Electrolyte-Assisted Hydrogen Storage Reactions

Use of electrolytes, in the form of LiBH 4 /KBH 4 and LiI/KI/CsI eutectics, is shown to significantly improve (by more than a factor of 10) both the dehydrogenation and full rehydrogenation of the MgH 2 /Sn destabilized hydride system and the hydrogenation of MgB 2 to Mg(BH 4 ) 2 . The improvement revealed that interparticle transport of atoms heavier than hydrogen can be an important rate-limiting step during hydrogen cycling in hydrogen storage materials consisting of multiple phases in powder form. Electrolytes enable solubilizing heavy ions into a liquid environment and thereby facilitate the reaction over full surface areas of interacting particles. In conclusion, the examples presented suggest that use of electrolytes in the form of eutectics, ionic liquids, or solvents containing dissolved salts may be generally applicable for increasing reaction rates in complex and destabilized hydride materials.

08 HYDROGEN↗

Inorganic “Conductive Glass” Approach to Rendering Mesoporous Metal–Organic Frameworks Electronically Conductive and Chemically Responsive

A representative mesoporous metal–organic-framework (MOF) material, NU-1000, has been rendered electronically conductive via a robust inorganic approach that permits retention of MOF crystallinity and porosity. The approach is based on condensed-phase grafting of molecular tin species onto the MOF nodes via irreversible reaction with hydroxyl and aqua ligands presented at the node surface, a self-limiting process termed solvothermal installation (of metal ions) in MOFs (SIM, a solution-phase analog of atomic layer deposition in MOFs). Treatment of the modified MOF with aerated steam at 120 °C converts the grafted tin molecules to tetratin(IV)oxy clusters, with the clusters being sited between insulating pairs of zirconia-like nodes (the zirconium component being key to endowing the parent material with requisite chemical and thermal stability). By introducing new O–H presenting ligands on the modified-MOF node, the high-temperature steam step additionally serves to reset the material to reactive form, thus enabling a second self-limiting tin-grafting step to be run (and after further steam treatment, enabling a third). Difference-envelop-density (DED) analyses of synchrotron-derived X-ray scattering data, with and without installed tin species, show that the clusters formed after one cycle are spatially isolated, but that repetitive SIM cycling adds metal and oxygen ions in a way that enshrouds nodes, links clusters, and yields continuous one-dimensional strands of oxy-tin(IV), oriented exclusively along the c axis of the MOF. Two-probe conductivity measurements show that the parent MOF and the version containing isolated oxy-tin(IV) clusters are electrically insulating, but that the versions featuring continuous strands show an electrical conductivity of 1.8 × 10–7 S/cm after three Sn-SIM cycles. When combined with interdigitated microelectrodes, the solvent-free and conductive-glass-modified material (three Sn-SIM cycles) displays a substantial and persistent increase in electrical conductivity during exposure to 5% H2, indicating a role for dissociated H2 as an electronic dopant. The increase can be repetitively reversed by alternating H2 with air, illustrating the ability of the conductive MOF to function as a resistive sensor for H2 and suggesting further potential applications that may capitalize on the combination of high volumetric surface area, high mesoporosity, high chemical and thermal stability, and significant electrical conductivity.

bio-inspired↗

Catalytic chemoselective functionalization of methane in a metal-organic framework

Methane constitutes the largest fraction of natural gas reserves and is a low-cost abundant starting material for the synthesis of value-added chemicals and fuel. Selective catalytic functionalization of methane remains a vital goal in the chemical sciences due to its low intrinsic reactivity. Borylation has recently emerged as a promising route for the catalytic functionalization of methane. A major challenge in this regard is selective borylation towards the monoborylated product that is more active than methane and can easily lead to over-functionalization. Herein, we report a highly selective microporous metal-organic framework- supported iridium(III) catalyst for methane borylation that exhibits a chemoselectivity of > 99% (mono versus bis at 19.5% yield; turnover number = 67) for monoborylated methane, with bis(pinacolborane) as the borylation reagent in dodecane, at 150 °C and 34 atm of methane, employing as little as 1.8 wt% of iridium. The preference for the monoborylated product is ascribed to the shape-selective effect of the metal-organic framework pore structures.

Zhang, Xuan (ORCID:0000000182147265)↗

Tunable Crystallinity and Charge Transfer in Two‐Dimensional G‐Quadruplex Organic Frameworks

Abstract DNA G‐quadruplex structures were recently discovered to provide reliable scaffolding for two‐dimensional organic frameworks due to the strong hydrogen‐bonding ability of guanine. Herein, 2,7‐diaryl pyrene building blocks with high HOMO energies and large optical gaps are incorporated into G‐quadruplex organic frameworks. The adjustable substitution on the aryl groups provides an opportunity to elucidate the framework formation mechanism; molecular non‐planarity is found to be beneficial for restricting interlayer slippage, and the framework crystallinity is highest when intermolecular interaction and non‐planarity strike a fine balance. When guanine‐functionalized pyrenes are co‐crystallized with naphthalene diimide, charge‐transfer (CT) complexes are obtained. The photophysical properties of the pyrene‐only and CT frameworks are characterized by UV/Vis and steady‐state and time‐resolved photoluminescence spectroscopies, and by EPR spectroscopy for the CT complex frameworks.

Wu, Yi‐Lin↗

Extending the Compositional Range of Nanocasting in the Oxozirconium Cluster-Based Metal–Organic Framework NU-1000—A Comparative Structural Analysis

Here, the process of nanocasting in metal-organic frameworks (MOFs) is a versatile approach to modify these porous materials by introducing supporting scaffolds. The nanocast scaffolds can stabilize metal-oxo clusters in MOFs at high temperatures and modulate their chemical environments. Here we demonstrate a range of nanocasting approaches in the MOF NU-1000, which contains hexanuclear oxozirconium clusters (denoted as Zr 6 clusters) that are suitable for modification with other metals. We developed methods for introducing SiO 2 , TiO 2 , polymeric, and carbon scaffolds into the NU-1000 structure. The responses of NU-1000 towards different scaffold precursors were studied, including the effects on morphology, precursor distribution, and porosity after nanocasting. Upon removal of organic linkers in the MOF by calcination/pyrolysis at 500 °C or above, the Zr 6 clusters remained accessible and maintained their Lewis acidity in SiO 2 nanocast samples, whereas additional treatment was necessary for Zr 6 clusters to become accessible in carbon nanocast samples. Aggregation of Zr 6 clusters was largely prevented with SiO 2 or carbon scaffolds even after thermal treatment at 500 °C or above. In the case of titania nanocasting, NU- 1000 crystals underwent a pseudomorphic transformation, in which Zr 6 clusters reacted with titania to form small oxaggregates of a Zr/Ti mixed oxide with a local structure resembling that of ZrTi 2 O 6 . In conclusion, the ability to maintain high densities of discrete Lewis acidic Zr 6 clusters on SiO 2 or carbon supports at high temperatures provides a starting point for designing new thermally stable catalysts.

36 MATERIALS SCIENCE↗

Tuning the properties of metal–organic framework nodes as supports of single-site iridium catalysts: node modification by atomic layer deposition of aluminium

The metal–organic framework NU-1000, with Zr 6 -oxo, hydroxo, and aqua nodes, was modified by incorporation of hydroxylated Al( iii ) ions by ALD-like chemistry with [Al(CH 3 ) 2 (iso-propoxide)] 2 followed by steam (ALD = atomic layer deposition). Al ions were installed to the extent of approximately 7 per node. Single-site iridium diethylene complexes were anchored to the nodes of the modified and unmodified MOFs by reaction with Ir(C 2 H 4 ) 2 (acac) (acac = acetylacetonate) and converted to Ir(CO) 2 complexes by treatment with CO. Infrared spectra of these supported complexes show that incorporation of Al weakened the electron donor tendency of the MOF. Correspondingly, the catalytic activity of the initial supported iridium complexes for ethylene hydrogenation increased, as did the selectivity for ethylene dimerization. The results of density functional theory calculations with a simplified model of the nodes incorporating Al( iii ) ions are in qualitative agreement with some catalyst performance data.

catalysis (heterogeneous), materials and chemistry↗

Stable metal–organic framework-supported niobium catalysts

In this study by developing structurally well-defined, supported oxide catalysts remains a significant challenge. Here, we report the grafting of Nb(V) oxide sites onto the nodes of the Zr-based metal organic framework (MOF) NU-1000 as a stable, well-defined catalyst support. Nb(V) oxide was deposited with loadings up to 1.6 mmol/g via two post-synthetic methods: atomic layer deposition in a MOF (AIM), and solution-phase grafting in a MOF (SIM). Difference envelope density (DED) measurements indicated that the two synthetic methods resulted in different local structures of the Nb(V) ions within NU-1000. Despite their high Nb(V) loadings, which were equivalent to >60% surface coverage, nearly all Nb(V) sites of the MOF-supported catalysts were active sites for alkene epoxidation, as confirmed by phenylphosphonic acid titration. The MOF-supported catalysts were more selective than the control Nb-ZrO 2 catalyst for cyclohexene epoxidation with aqueous H 2 O 2 , and were far more active on a gravimetric basis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Best Practices for the Synthesis, Activation, and Characterization of Metal–Organic Frameworks

Metal–organic frameworks (MOFs) are structurally diverse materials comprised of inorganic and organic components. As the rapidly expanding field of MOF research has demonstrated, these materials are being explored for a wide variety of potential applications. In this tutorial review, we give an overview of the current best practices associated with the synthesis, activation, and characterization of MOFs. Methods described include supercritical CO 2 activation, single crystal X-ray diffraction (XRD), powder X-ray diffraction (PXRD), nitrogen adsorption/desorption isotherms, surface area calculations, aqueous stability tests, scanning electron microscopy (SEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), nuclear magnetic resonance spectroscopy (NMR), and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). A variety of different MOFs are presented to aid in the discussion of relevant techniques. In addition, some sections are accompanied by instructional videos to give further insight into the techniques, including tips, tricks, and suggestions only those at the bench could describe.

36 MATERIALS SCIENCE↗

Installing heterobimetallic cobalt–aluminum single sites on a metal organic framework support

Here, a heterobimetallic cobalt-aluminum complex was immobilized onto the metal organic framework NU-1000 using a simple solution-based deposition procedure. Characterization data are consistent with a maximum loading of a single Co-Al complex per Zr 6 node of NU-1000. Furthermore, the data support that the Co-Al bimetallic complex is evenly distributed throughout the NU-1000 particle, binds covalently to the Zr6 nodes, and occupies the NU-1000 apertures with the shortest internode distances (~8.5 Å). Heating the anchored Co-Al complex on NU-1000 at 300 °C for 1 h in air completely removes the organic ligand of the complex without affecting the structural integrity of the MOF support. We propose that a Co-Al oxide cluster is formed in place of the anchored complex in NU-1000 during heating. Collectively, the results suggest that well-defined heterobimetallic complexes can be effective precursors for installing two different metals simultaneously onto a MOF support. The CoAl-functionalized NU-1000 samples catalyze the oxidation of benzyl alcohol to benzaldehyde with tert -butyl hydroperoxide as a stoichiometric oxidant. Density functional theory calculations were performed to elucidate the detailed structures of the Co-Al active sites on the Zr 6 -nodes, and a Co-mediated catalytic mechanism is proposed.

36 MATERIALS SCIENCE↗