We report herein the upscaled synthesis and shaping of UiO66-COOH for NH3 air purification. The synthesis of the zirconium-based MOF was carried out in a batch reactor in an aqueous suspension with a yield of 89% and a spacetime yield of 350 kg/day/m 3. Neither toxic chemicals nor organic solvents were used, allowing this MOF to be employed in individual or collective air purification devices. Freeze-granulation and extrusion shaping techniques were investigated. The NH3 air purification performances of UiO66-COOH in bead, tablet and extrudate forms were compared to those of commercial carbon based materials (type K adsorbents from3M and Norit). Testing conditions were chosen to reflect current standards for ammonia concentration (600-1200 ppm) and velocity. In addition, the breakthrough measurements were carried out at three different relative humidity levels (0%, 40% and 70%). Pellets and extrudates of UiO66-COOH outperformed commercial benchmark adsorbents in all conditions, especially in dry conditions, for which the commercial adsorbents suffered impaired ammonia uptake and shortened service life. Extrudates of UiO66-COOH also withstood attrition after intensive shaking.
The authors report on the manufacturing of mechanically stable β-tricalcium phosphate (β-TCP) structural hybrid scaffolds via the combination of additive manufacturing (CerAM VPP) and Freeze Foaming for engineering a potential bone replacement. In the first step, load bearing support structures were designed via FE simulation and 3D printed by CerAM VPP. In the second step, structures were foamed-in with a porous and degradable calcium phosphate (CaP) ceramic that mimics porous spongiosa. For this purpose, Fraunhofer IKTS used a process known as Freeze Foaming, which allows the foaming of any powdery material and the foaming-in into near-net-shape structures. Using a joint heat treatment, both structural components fused to form a structural hybrid. This bone construct had a 25-fold increased compressive strength compared to the pure CaP Freeze Foam and excellent biocompatibility with human osteoblastic MG-63 cells when compared to a bone grafting Curasan material for benchmark.
Freeze foaming is a method to manufacture cellular ceramic scaffolds with a hierarchical porous structure. These so-called freeze foams are predestined for the use as bone replacement material because of their internal bone-like structure and biocompatibility. On the one hand, they consist of macrostructural foam cells which are formed by the expansion of gas inside the starting suspension. On the other hand, a porous microstructure inside the foam struts is formed during freezing and subsequent freeze drying of the foamed suspension. The aim of this work is to investigate for the first time the formation of macrostructure and microstructure separately depending on the composition of the suspension and the pressure reduction rate, by means of appropriate characterization methods for the different pore size ranges. Moreover, the foaming behavior itself was characterized by in-situ radiographical and computed tomography (CT) evaluation. As a result, it could be shown that it is possible to tune the macro- and microstructure separately with porosities of 49–74% related to the foam cells and 10–37% inside the struts.
Freeze Foaming is a direct foaming method that aims at manufacturing ceramic cellular scaffolds for diverse applications. Next to porous structures for a potential use as refractories, the focus lies on potential bone replacement material. The main challenge of this foaming method is to achieve a homogeneous and predictable pore morphology. That is why, in a current project, the authors report on the pore morphology formation and evolution of the foaming process by means of nondestructive testing. This contribution primarily compares the effect of the suspension’s temperature on the resulting foam structure (foaming at 5 and 40 °C). As a basis for computed tomographic analysis, a stable and reproducible model suspension was developed that resulted in reproducible foam structures. Characterized by viscosity, foam structure analyses and foaming rate, the resulting Freeze Foams became adjustable with regards to their porosity and pore shape/size. Under certain conditions, we succeeded in achieving a relatively homogeneous pore structure, as proven by computed tomography-derived quantitative analysis.
Living building materials (LBM) are gaining interest in the field of sustainable alternative construction materials to reduce the significant impact of the construction industry on global CO2 emissions. This study investigated the process of three-dimensional bioprinting to create LBM incorporating the cyanobacterium Synechococcus sp. strain PCC 7002, which is capable of producing calcium carbonate (CaCO3) as a biocement. Rheology and printability of biomaterial inks based on alginate-methylcellulose hydrogels containing up to 50 wt% sea sand were examined. PCC 7002 was incorporated into the bioinks and cell viability and growth was characterized by fluorescence microscopy and chlorophyll extraction after the printing process. Biomineralization was induced in liquid culture and in the bioprinted LBM and observed by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and through mechanical characterization. Cell viability in the bioprinted scaffolds was confirmed over 14 days of cultivation, demonstrating that the cells were able to withstand shear stress and pressure during the extrusion process and remain viable in the immobilized state. CaCO3 mineralization of PCC 7002 was observed in both liquid culture and bioprinted LBM. In comparison to cell-free scaffolds, LBM containing live cyanobacteria had a higher compressive strength. Therefore, bioprinted LBM containing photosynthetically active, mineralizing microorganisms could be proved to be beneficial for designing environmentally friendly construction materials.
With a novel Freeze Foaming method, it is possible to manufacture porous cellular components whose structure and composition also enables them for application as artificial bones, among others. To tune the foam properties to our needs, we have to understand the principles of the foaming process and how the relevant process parameters and the foam’s structure are linked. Using in situ analysis methods, like X-ray microcomputed tomography (µCT), the foam structure and its development can be observed and correlated to its properties. For this purpose, a device was designed at the Institute of Lightweight Engineering and Polymer Technology (ILK). Due to varying suspension temperature and the rate of pressure decrease it was possible to analyze the foam’s developmental stages for the first time. After successfully identifying the mechanism of foam creation and cell structure formation, process routes for tailored foams can be developed in future.
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