Open-porous alumina foams with additional strut porosity are fabricated by a two-step sponge-replication based manufacturing process. As the first step, open cellular ceramic foams are prepared following the Schwarzwalder sponge replication technique. Therefore, organic foam templates are coated with different aqueous alumina slurries with a solid load between 20 and 40 vol% In a second step, an additional porosity is generated inside the foam struts by freezing of the foams at temperatures between À196 and À20 C and subsequent sublimation drying. The hierarchical structure of both, cell pores and strut pores in the freeze-dried material remains intact after drying, template removal, and sintering. Size, connectivity, and morphology of the strut pores strongly depend on the solid load of the alumina slurry and on the freezing temperature. Cellular structures with a strut porosity between 50% and 60% and a total porosity exceeding 90% are prepared, which show a compressive strength in between 0.4 to 0.6 MPa. Due to the additional strut porosity, the specific surface area of freeze-dried replica foams increases from 70 cm 2 g À1 for conventionally prepared foams to 200 cm 2 g À1 for freeze-dried foams, respectively.
Fine-pored, 45 ppi (pores per linear inch) alumina foams are prepared from ceramic slurries with varying contents of additives (deflocculant, binder) and solid loading following a standardized procedure. Rheological key parameters (yield stress, high-shear viscosity) of the respective slurries are determined by approximation of the experimental flow curves with appropriate rheological models. The resulting ceramic foams are characterized by computed tomography (CT) followed by a morphometric analysis of the reconstruction volume data. The main scope of the work involves the development of a procedure to reliably define the binarization threshold during these morphometric calculations, which is based on the analysis of the differential course of the total porosity results from calculations performed at varying binarization threshold values ("differential thresholding"). A very good match of the CT porosity results with experimental data is achieved, despite the unfavorable CT voxel resolution to foam structure fineness relation. The CT evaluation results are finally correlated to the rheological properties of the respective slurries used in foam manufacturing. The dominant slurry composition parameters are the weight fraction of the ceramic powder and the binder concentration. Increasing binder and solid content result in an increased yield stress and viscosity of the respective dispersion and consequently in a decreased porosity and cell size of the finally manufactured cellular ceramic.
Reticulated ceramic foams are used in a wide range of applications such as filters, catalyst supports, lightweight materials, energy absorptions materials, or as scaffolds for tissue engineering as the most common ones. Based on gaseous foaming processes of polymers, a stochastic distribution of closed pores is obtained. By reticulation processing thin foam windows are removed between cells turning a closed cell into an open cell structure. These foams are used as template for porous ceramics manufacturing: With different processing approaches, for example, with dip coating of a ceramic slurry and a subsequent (multistep) thermal treatment ceramic reticulate foams are obtained. A variety of material properties strongly depend on the cell and strut size, as well on material composition. Functionalization of ceramic foam surfaces (outer surface functionalization), for example, with zeolites or nanosized aggregates lead to an increase of the specific surface area or provides catalytic or heat storage functionality. Filling of struts (inner surface functionalization) may lead to improved mechanical stability or may provide functionalities such as electric conductivity. The present work summarizes the processing steps from the template foam to the final cellular ceramic, functionalization strategies, and the most common characterization techniques.
Pores, on several orders of magnitude in size, control the properties of a solid material to a large extent. This is just as true for materials containing pores in the sub‐nanometer range like zeolites as for cellular foam structures with pores of several millimeters in size. All these porous materials have their distinct potential application ranging from heterogeneous catalysis to metal melt filtration. In many cases, the (hierarchical) combination of pores with different size regimes can improve the performance of the respective porous material or can lead to entirely new properties and applications. This review addresses the preparation and properties of microporous‐macroporous composite materials based on cellular foam supports (ceramic, metal, polymer) with a coating of a microporous compound (zeolite, zeotype framework, metal‐organic framework). The manufacturing of these materials can either be performed by dispersion‐based techniques, where the microporous coating is applied from a dispersion onto the cellular support (ex situ), or in situ by crystallization of the microporous compound directly onto the struts of the foam structure. In both cases, the general procedure can be modified by a pretreatment of the cellular support in order to improve the coating layer adherence, the overall amount of deposited material, or to control of the crystal morphology of the microporous compound.
The sulfates Nb(2)O(2)(SO(4))(3), MoO(2)(SO(4)), WO(SO(4))(2,) and two modifications of Re(2)O(5)(SO(4))(2) have been synthesized by the solvothermal reaction of NbCl(5), WOCl(4), Re(2)O(7)(H(2)O)(2), and MoO(3) with sulfuric acid/SO(3) mixtures at temperatures between 200 and 300 °C. Besides the X-ray crystal structure determination of all compounds, the thermal behavior was investigated using thermogravimetric studies. WO(SO(4))(2) (monoclinic, P2(1)/n, a = 7.453(1) Å, b = 11.8232(8) Å, c = 7.881(1) Å, β = 107.92(2)°, V = 660.7(1) Å(3), Z = 4) and both modifications of Re(2)O(5)(SO(4))(2) (I: orthorhombic, Pba2, a = 9.649(1) Å, b = 8.4260(8) Å, c = 5.9075(7) Å, V = 480.27(9) Å(3), Z = 2; II: orthorhombic, Pbcm, a = 7.1544(3) Å, b = 7.1619(3) Å, c = 16.8551(7) Å, V = 863.64(6) Å(3), Z = 4) are the first structurally characterized examples of tungsten and rhenium oxide sulfates. Their crystal structure contains layers of sulfate connected [W═O] moieties or [Re(2)O(5)] units, respectively. The cohesion between layers is realized through weak M-O contacts (343-380 pm). Nb(2)O(2)(SO(4))(3) (orthorhombic, Pna2(1), a = 9.9589(7) Å, b = 11.7983(7) Å, c = 8.6065(5) Å, V = 1011.3(1) Å(3), Z = 4) represents a new sulfate-richer niobium oxide sulfate. The crystal structure contains a three-dimensional network of sulfate connected [Nb═O] moieties. In MoO(2)(SO(4)) (monoclinic, I2/a, a = 8.5922(6) Å, b = 12.2951(6) Å, c = 25.671(2) Å, β = 94.567(9)°, V = 2703.4(3) Å(3), Z = 24) [MoO(2)] units are connected through sulfate ions to a three-dimensional network, which is pervaded by channels along [100] accommodating the terminal oxide ligands. In all compounds except WO(SO(4))(2), the metal ions are octahedrally coordinated by monodentate sulfate ions and oxide ligands forming short M═O bonds. In WO(SO(4))(2), the oxide ligand and two monodentate and two bidentate sulfate ions build a pentagonal bipyramid around W. The thermal stability of the sulfates decreases in the order Nb > Mo > W > Re; the residues formed during the decomposition are the corresponding oxides.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.
hi@scite.ai
10624 S. Eastern Ave., Ste. A-614
Henderson, NV 89052, USA
Copyright © 2024 scite LLC. All rights reserved.
Made with 💙 for researchers
Part of the Research Solutions Family.