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Further reports on shaping ZIF-8 via DIW include the work by Lefevere et al., 112 who managed to formulate the MOF with a blend of inorganic and organic binders. The former was added to improve the mechanical stability of the shaped objects, and the latter to enhance the rheological properties of the paste. Typically, the parent ZIF-8 powder (66.7 wt%) was mixed with bentonite (16.7 wt%) and methylcellulose (16.7 wt%) with a subsequent addition of water and mixing to form a homogeneous printable paste. Once homogenized, it was further loaded into a 50 mL syringe and extruded through 250 and 600 μm diameter nozzles in a layer-by-layer fashion at room temperature ( Fig. 11g and h). N. Heymans, S. Vaesen and G. De Weireld, A complete procedure for acidic gas separation by adsorption on MIL-53 (Al), Microporous Mesoporous Mater., 2012, 154, 93–99, DOI: 10.1016/j.micromeso.2011.10.020. As in the case of extrusion, the paste formulation is a crucial step in 3D printing and should yield a final composition with appropriate rheological properties. Apart from the parent powder and a liquid, the paste is also composed of a binder and a plasticizer. The former provides adequate mechanical resistance to the final 3D objects, while the latter improves the flowability and plasticity of the paste to be printed. One of the major differences is the printing nozzle: while the die in extruders can reach sizes up to a few centimeters, in 3D printers the nozzle (or needle) is typically smaller than millimeters in diameter. Such a thin nozzle allows designing objects with complex geometries that would be challenging to obtain via a conventional method.

Two step, continuous flow spray-drying method, dense structures Garzon-Tovar et al. 138 also reported the spray-drying of a series of MOFs with high-nuclearity. To do so, they combined continuous flow and spray-drying methods ( Fig. 16b and c). As in the case of Mitsuka et al., 137 the former is beneficial to initiate the nucleation step, while the latter favors the crystal growth. Thus, the so-called spray-drying continuous flow-assisted synthesis was applied to produce spherical microbeads of UiO-66 and its derivatives.Extrusion is another classical technique which is especially used to produce extrudates and honeycombs for catalytic converters. When it is applied to MOFs, limited impact on the structural and textural properties can be observed for most MOFs, due to lower pressures and shear forces applied. Extrusion requires, however, finely controlling the formulation and related rheological properties of the extruded paste. Advantageously, extrusion can also be used for the direct preparation of MOF objects starting from precursors (reactive extrusion). The latter is of particular interest as it allows limiting or avoiding completely the toxic solvents traditionally used for the synthesis of MOF powders. At the same time, reactive extrusion implies a continuous process with high potential space time yields. While this approach might not be applicable to all MOF structures, the reactive extrusion presents several advantages over more conventional methods such as solvo/hydrothermal or microwave-assisted syntheses of MOFs. On the other hand, these conventional methods remain better in terms of obtained crystallinity and surface area for most MOF structures. Y. Ming, J. Purewal, J. Yang, C. Xu, R. Soltis, J. Warner, M. Veenstra, M. Gaab, U. Mu and D. J. Siegel, Kinetic Stability of MOF-5 in Humid Environments: Impact of Powder Densification, Humidity Level, and Exposure Time, Langmuir, 2015, 31, 4988–4995, DOI: 10.1021/acs.langmuir.5b00833. A mixture of PVA and PVB was used as a binder in the study by Chanut et al. 71 The authors first mixed 5 g of MOF powder with a 3 wt% polymer blend, followed by periodical spraying of ethanol for a total of 50 mL to cause primary particle agglomeration. Upon sieving, a fraction with sizes between 1.3 and 1.7 mm ( Fig. 5h) was rounded using a rolling device to achieve the final shape. Eventually, the spheres were dried at 110 °C for 12 h to remove the residual ethanol. Fig. 9 Schematic representation of the 3D printing process via the Direct Ink Writing (DIW) method.

For those outside of France, the hospitality industry, or both, the initials MOF may not ring a bell, but those three letters hold an incredible amount of significance. To be a “Meilleur Ouvrier de France” or "Best Craftsman of France" as you'll soon discover, is a very prestigious title indeed. Here's how it happens. Peterson et al. 47 performed another study on HKUST-1 to examine the evolution of its physical and chemical properties. Thus, the authors applied pressures of 1000 psi (∼7 MPa) and 10 000 psi (∼69 MPa). While the crystal structure was globally preserved, compressed HKUST-1 exhibited broader reflections as well as high signal-to-noise ratios on the XRD patterns. This suggests partial framework damage. Consequently, there was a certain decrease in BET surface area, from 1698 m 2 g −1 for the powder to 892 m 2 g −1 for the pellets made at ∼69 MPa. These values are somewhat different from the ones reported by Kim et al., 48 who stated that above 10 MPa the HKUST-1 framework underwent structural degradation. At the same time, Dhainaut et al. 49 reported a low (15%) loss in BET surface area for HKUST-1, reaching 1091 m 2 g −1 upon densification at 121 MPa. Besides, they showed that addition of 2 wt% of a binder (graphite) slightly improved the mechanical stability of HKUST-1 pellets without significant loss of BET surface area. They explained this relatively small loss as due to the presence of the remaining solvent within the framework, acting as a scaffold during compression, as well as the slow compression speed applied to the powder bed. Y. H. Hu and L. Zhang, Amorphization of metal–organic framework MOF-5 at unusually low applied pressure, Phys. Rev. B: Condens. Matter Mater. Phys., 2010, 81, 174103, DOI: 10.1103/PhysRevB.81.174103. V. Finsy, H. Verelst, L. Alaerts, D. E. De Vos, P. A. Jacobs, G. V. Baron and J. F. M. Denayer, Pore-Filling-Dependent Selectivity Effects in the Vapor-Phase Separation of Xylene Isomers on the Metal−Organic Framework MIL-47, J. Am. Chem. Soc., 2008, 130, 7110–7118, DOI: 10.1021/ja800686c. Granulation is the last industrially-mature technology reviewed herein, and allows producing millimeter-sized grains. Two types of granulation techniques are typically discussed: wet granulation, when powders are aggregated in a high-shear rate mixer in the presence of a solvent; and dry granulation, when grains are obtained from a previously shaped object either mildly crushed and sieved, or spheronized. Due to higher stresses applied, the dry granulation implies more severe losses in the initial physicochemical properties of the MOFs, while the wet granulation has a less pronounced effect and therefore might be more adequate. Especially, replacing water with another solvent with a lower surface tension is highly beneficial.The XRD patterns of the monoliths were found to be comparable to those of their powder analogues, suggesting that the crystal structure was retained upon shaping. The intensities however experienced a certain decrease, which was attributed to the presence of PVA. Further analyses revealed pronounced textural properties for Ni(bdc)(ted) 0.5 as given by N 2 physisorption. Its monolithic form exhibited a S BET of 1325 m 2 g −1, while its powder form presented a S BET of 1802 m 2 g −1. The difference was 27%, a value which agrees well with the initial MOF content in the paste (80 wt%). The corresponding values for ZIF-7 were 16 and 40 m 2 g −1, respectively, for its powder and printed forms. Its porosity is inaccessible to N 2 and the slightly higher available surface area was attributed to the silica binder in the printed composition. Interestingly, conventional compression tests revealed an excellent mechanical stability of up to 1.7 MPa for Ni(bdc)(ted) 0.5 due to the high content of binder (20 wt%), which provided considerably strong bonding of particles. At the same time, ZIF-7 monoliths withstood compression up to 0.8 MPa, showing that silica might be less appropriate than PVA for strongly bonding MOF particles. When probed for ethane/ethylene adsorption, Ni(bdc)(ted) 0.5 monoliths showed total uptakes of 4.1 and 2.9 mmol g −1, respectively. These values were found to be proportional to the MOF content. Notably, ZIF-7 monoliths showed total uptakes of 1.8 and 2.5 mmol g −1, respectively. Both isotherms exhibited an S-shape, revealing the pore-opening feature of this MOF upon increasing pressure. C. Wang, Y. V. Kaneti, Y. Bando, J. Lin, C. Liu, J. Li and Y. Yamauchi, Metal–organic framework-derived one-dimensional porous or hollow carbon-based nanofibers for energy storage and conversion, Mater. Horiz., 2018, 5, 394–407, 10.1039/C8MH00133B. S. S.-Y. Chui, S. M.-F. Lo, J. P. H. Charmant, A. G. Orpen and I. D. Williams, A Chemically Functionalizable Nanoporous Material [Cu 3(TMA) 2(H 2O) 3]n, Science, 1999, 283, 1148–1151, DOI: 10.1126/science.283.5405.1148.