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21 pages, 6827 KiB

Open AccessArticle

Porous Alumina Ceramics with Multimodal Pore Size Distributions

by Jonas Biggemann, Martin Stumpf and Tobias Fey

Materials 2021, 14(12), 3294; https://doi.org/10.3390/ma14123294 - 14 Jun 2021

Cited by 21 | Viewed by 3830

Pore networks with multimodal pore size distributions combining advantages from isotropic and anisotropic shaped pores of different sizes are highly attractive to optimize the physical properties of porous ceramics. Multimodal porous Al₂O₃ ceramics were manufactured using pyrolyzed cellulose fibers (l [...] Read more.

Pore networks with multimodal pore size distributions combining advantages from isotropic and anisotropic shaped pores of different sizes are highly attractive to optimize the physical properties of porous ceramics. Multimodal porous Al₂O₃ ceramics were manufactured using pyrolyzed cellulose fibers (l = 150 µm, d = 8 µm) and two types of isotropic phenolic resin spheres (d = 30 and 300 µm) as sacrificial templates. The sacrificial templates were homogeneously distributed in the Al₂O₃ matrix, compacted by uniaxial pressing and extracted by a burnout and sintering process up to 1700 °C in air. The amount of sacrificial templates was varied up to a volume content of 67 Vol% to form pore networks with porosities of 0–60 Vol%. The mechanical and thermal properties were measured by 4-point-bending and laser flash analysis (LFA) resulting in bending strengths of 173 MPa to 14 MPa and heat conductivities of 22.5 Wm⁻¹K⁻¹ to 4.6 Wm⁻¹K⁻¹. Based on µCT-measurements, the representative volume-of-interest (VOI) of the samples digital twin was determined for further analysis. The interconnectivity, tortuosity, permeability, the local and global stress distribution as well as strut and cell size distribution were evaluated on the digital twin’s VOI. Based on the experimental and simulation results, the samples pore network can be tailored by changing the fiber to sphere ratio and the overall sacrificial template volume. The presence pore formers significantly influenced the mechanical and thermal properties, resulting in higher strengths for samples containing fibrous templates and lower heat conductivities for samples containing spherical templates. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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12 pages, 6603 KiB

Open AccessArticle

Refractory Metal Coated Alumina Foams as Support Material for Stem Cell and Fibroblasts Cultivation

by Georg Hasemann, Ulf Betke, Manja Krüger, Heike Walles and Michael Scheffler

Materials 2021, 14(11), 2813; https://doi.org/10.3390/ma14112813 - 25 May 2021

Cited by 1 | Viewed by 1757

Abstract

Ceramics are widely used as implant materials; however, they are brittle and may emit particles when used in these applications. To overcome this disadvantage, alumina foams, which represent a 3D cellular structure comparable to that of human trabecular bone structures, were sputter coated [...] Read more.

Ceramics are widely used as implant materials; however, they are brittle and may emit particles when used in these applications. To overcome this disadvantage, alumina foams, which represent a 3D cellular structure comparable to that of human trabecular bone structures, were sputter coated with platinum, tantalum or titanium and modified with fibronectin or collagen type I, components of the extracellular matrix (ECM). To proof the cell material interaction, the unmodified and modified materials were cultured with (a) mesenchymal stem cells being a perfect indicator for biocompatibility and releasing important cytokines of the stem cell niche and (b) with fibroblasts characterized as mediators of inflammation and therefore an important cellular component of the foreign body reaction and inflammation after implantation. To optimize and compare the influence of metal surfaces on cellular behavior, planar glass substrates have been used. Identified biocompatible metal surface of platinum, titanium and tantalum were sputtered on ceramic foams modified with the above-mentioned ECM components to investigate cellular behavior in a 3D environment. The cellular alumina support was characterized with respect to its cellular/porous structure and niche accessibility and coating thickness of the refractory metals; the average cell size was 2.3 mm, the average size of the cell windows was 1.8 mm, and the total foam porosity was 91.4%. The Pt, Ti and Ta coatings were completely dense covering the entire alumina foam surface. The metals titanium and tantalum were colonized very well by the stem cells without a coating of ECM components, whereas the fibroblasts preferred components of the ECM on the alumina foam surface. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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14 pages, 6821 KiB

Open AccessArticle

Open-Cellular Alumina Foams with Hierarchical Strut Porosity by Ice Templating: A Thickening Agent Study

by Kathleen Dammler, Katja Schelm, Ulf Betke, Tobias Fey and Michael Scheffler

Materials 2021, 14(5), 1060; https://doi.org/10.3390/ma14051060 - 24 Feb 2021

Cited by 7 | Viewed by 1900

Abstract

Alumina replica foams were manufactured by the Schwartzwalder sponge replication technique and were provided with an additional strut porosity by a freeze-drying/ice-templating step prior to thermal processing. A variety of thickeners in combination with different alumina solid loads in the dispersion used for [...] Read more.

Alumina replica foams were manufactured by the Schwartzwalder sponge replication technique and were provided with an additional strut porosity by a freeze-drying/ice-templating step prior to thermal processing. A variety of thickeners in combination with different alumina solid loads in the dispersion used for polyurethane foam template coating were studied. An additional strut porosity as generated by freeze-drying was found to be in the order of ~20%, and the spacings between the strut pores generated by ice-templating were in the range between 20 µm and 32 µm. In spite of the lamellar strut pore structure and a total porosity exceeding 90%, the compressive strength was found to be up to 1.3 MPa. Combining the replica process with freeze-drying proves to be a suitable method to enhance foams with respect to their surface area accessible for active coatings while preserving the advantageous flow properties of the cellular structure. A two-to-threefold object surface-to-object volume ratio of 55 to 77 mm⁻¹ was achieved for samples with 30 vol% solid load compared to 26 mm⁻¹ for non-freeze-dried samples. The freeze-drying technique allows the control of the proportion and properties of the introduced pores in an uncomplicated and predictable way by adjusting the process parameters. Nevertheless, the present article demonstrates that a suitable thickener in the dispersion used for the Schwartzwalder process is inevitable to obtain ceramic foams with sufficient mechanical strength due to the necessarily increased water content of the ceramic dispersion used for foam manufacturing. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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17 pages, 5189 KiB

Open AccessArticle

Sodium Solid Electrolytes: Na_xAlO_y Bilayer-System Based on Macroporous Bulk Material and Dense Thin-Film

by Antonia Hoppe, Cornelius Dirksen, Karl Skadell, Michael Stelter, Matthias Schulz, Simon Carstens, Dirk Enke and Sharon Koppka

Materials 2021, 14(4), 854; https://doi.org/10.3390/ma14040854 - 10 Feb 2021

Cited by 2 | Viewed by 1880

Abstract

A new preparation concept of a partially porous solid-state bilayer electrolyte (BE) for high-temperature sodium-ion batteries has been developed. The porous layer provides mechanical strength and is infiltrated with liquid and highly conductive NaAlCl₄ salt, while the dense layer prevents short circuits. [...] Read more.

A new preparation concept of a partially porous solid-state bilayer electrolyte (BE) for high-temperature sodium-ion batteries has been developed. The porous layer provides mechanical strength and is infiltrated with liquid and highly conductive NaAlCl₄ salt, while the dense layer prevents short circuits. Both layers consist, at least partially, of Na-β-alumina. The BEs are synthesized by a three-step procedure, including a sol-gel synthesis, the preparation of porous, calcined bulk material, and spin coating to deposit a dense layer. A detailed study is carried out to investigate the effect of polyethylene oxide (PEO) concentration on pore size and crystallization of the bulk material. The microstructure and crystallographic composition are verified for all steps via mercury intrusion, X-ray diffraction, and scanning electron microscopy. The porous bulk material exhibits an unprecedented open porosity for a Na_xAlO_y bilayer-system of ≤57% with a pore size of ≈200–300 nm and pore volume of ≤0.3 cm³∙g⁻¹. It contains high shares of crystalline α-Al₂O₃ and Na-β-alumina. The BEs are characterized by impedance spectroscopy, which proved an increase of ionic conductivity with increasing porosity and increasing Na-β-alumina phase content in the bulk material. Ion conductivity of up to 0.10 S∙cm⁻¹ at 300 °C is achieved. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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14 pages, 5207 KiB

Open AccessArticle

Cellular Nickel-Yttria/Zirconia (Ni–YSZ) Cermet Foams: Manufacturing, Microstructure and Properties

by Ulf Betke, Katja Schelm, Andreas Rodak and Michael Scheffler

Materials 2020, 13(11), 2437; https://doi.org/10.3390/ma13112437 - 26 May 2020

Cited by 4 | Viewed by 2773

Abstract

Open-celled ceramic composite foams were prepared from NiO and yttria-stabilized zirconia (YSZ) powders by the polymer sponge replication (Schwartzwalder) technique using the respective aqueous dispersions. Mechanically stable NiO–YSZ foams with an average porosity of 93 vol.% were obtained. After chemical reduction of the [...] Read more.

Open-celled ceramic composite foams were prepared from NiO and yttria-stabilized zirconia (YSZ) powders by the polymer sponge replication (Schwartzwalder) technique using the respective aqueous dispersions. Mechanically stable NiO–YSZ foams with an average porosity of 93 vol.% were obtained. After chemical reduction of the NiO phase with hydrogen, cellular Ni–YSZ cermet structures were obtained. They are characterized by an electric conductivity up to 19∙10³ S∙m⁻¹ which can be adjusted by both, the Ni volume fraction, and the sintering/reduction procedure. The NiO–YSZ ceramic foams, as well as the cellular Ni–YSZ cermets prepared therefrom, were characterized with respect to their microstructure by scanning electron microscopy, confocal Raman microscopy and X-ray diffraction with Rietveld analysis. In addition, the compressive strength, the electric conductivity and the thermal conductivity were determined. The collected data were then correlated to the sample microstructure and porosity and were also applied for modelling of the mechanical and electric properties of the bulk Ni–YSZ strut material. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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16 pages, 5364 KiB

Open AccessArticle

Injection Molding of 3-3 Hydroxyapatite Composites

by Jonas Biggemann, Patrizia Hoffmann, Ivaylo Hristov, Swantje Simon, Philipp Müller and Tobias Fey

Materials 2020, 13(8), 1907; https://doi.org/10.3390/ma13081907 - 17 Apr 2020

Cited by 8 | Viewed by 3859

Abstract

The manufacturing of ideal implants requires fabrication processes enabling an adjustment of the shape, porosity and pore sizes to the patient-specific defect. To meet these criteria novel porous hydroxyapatite (HAp) implants were manufactured by combining ceramic injection molding (CIM) with sacrificial templating. Varied [...] Read more.

The manufacturing of ideal implants requires fabrication processes enabling an adjustment of the shape, porosity and pore sizes to the patient-specific defect. To meet these criteria novel porous hydroxyapatite (HAp) implants were manufactured by combining ceramic injection molding (CIM) with sacrificial templating. Varied amounts (Φ = 0–40 Vol%) of spherical pore formers with a size of 20 µm were added to a HAp-feedstock to generate well-defined porosities of 11.2–45.2 Vol% after thermal debinding and sintering. At pore former contents Φ ≥ 30 Vol% interconnected pore networks were formed. The investigated Young’s modulus and flexural strength decreased with increasing pore former content from 97.3 to 29.1 GPa and 69.0 to 13.0 MPa, agreeing well with a fitted power-law approach. Additionally, interpenetrating HAp/polymer composites were manufactured by infiltrating and afterwards curing of an urethane dimethacrylate-based (UDMA) monomer solution into the porous HAp ceramic preforms. The obtained stiffness (32–46 GPa) and Vickers hardness (1.2–2.1 GPa) of the HAp/UDMA composites were comparable to natural dentin, enamel and other polymer infiltrated ceramic network (PICN) materials. The combination of CIM and sacrificial templating facilitates a near-net shape manufacturing of complex shaped bone and dental implants, whose properties can be directly tailored by the amount, shape and size of the pore formers. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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14 pages, 3728 KiB

Open AccessArticle

Phase Evolution, Filler-Matrix Interactions, and Piezoelectric Properties in Lead Zirconate Titanate (PZT)-Filled Polymer-Derived Ceramics (PDCs)

by Franziska Eichhorn, Simone Kellermann, Ulf Betke and Tobias Fey

Materials 2020, 13(7), 1520; https://doi.org/10.3390/ma13071520 - 26 Mar 2020

Cited by 5 | Viewed by 2292

Abstract

PZT-silsesquioxane-based 0-3 hybrid materials are prepared by mixing lead zirconate titanate (Pb(Zr,Ti)O₃; PZT) powder with a [R-SiO_3/2]_n (R = H, CH₃, CH=CH₂, C₆H₅) silsequioxane preceramic polymer. A PZT load up [...] Read more.

PZT-silsesquioxane-based 0-3 hybrid materials are prepared by mixing lead zirconate titanate (Pb(Zr,Ti)O₃; PZT) powder with a [R-SiO_3/2]_n (R = H, CH₃, CH=CH₂, C₆H₅) silsequioxane preceramic polymer. A PZT load up to 55 vol.% can be reached in the final composite. The piezoelectric and mechanical properties are investigated as a function of the filler content and are compared with theoretical models and reference samples made of the pure preceramic polymer or PZT filler. The piezoelectric response of the composites, as expressed by the relative permittivity and the piezoelectric coefficients d₃₃ and g₃₃, increases with an increasing PZT content. The bending strength of the composites ranges between 15 MPa and 31 MPa without a clear correlation to the filler content. The thermal conductivity increases significantly from 0.14 W∙m⁻¹∙K⁻¹ for the pure polymer-derived ceramic (PDC) matrix to 0.30 W∙m⁻¹∙K⁻¹ for a sample containing 55 vol.% PZT filler. From X-ray diffraction experiments (XRD), specific interactions between the filler and matrix are observed; the crystallization of the PDC matrix in the presence of the PZT filler is inhibited; conversely, the PDC matrix results in a pronounced decomposition of the filler compared to the pure PZT material. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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16 pages, 6048 KiB

Open AccessArticle

Mechanical and Surface-Chemical Properties of Polymer Derived Ceramic Replica Foams

by Katja Schelm, Elena Abreu Morales and Michael Scheffler

Materials 2019, 12(11), 1870; https://doi.org/10.3390/ma12111870 - 10 Jun 2019

Cited by 16 | Viewed by 3622

Abstract

Polymer derived ceramic foams were prepared with the replica method using filler free and filler loaded polysiloxane containing slurries for the impregnation of open celled polyurethane foams. A significant change in mechanical strength, porosity and surface energy, i.e., wettability after thermal treatment between [...] Read more.

Polymer derived ceramic foams were prepared with the replica method using filler free and filler loaded polysiloxane containing slurries for the impregnation of open celled polyurethane foams. A significant change in mechanical strength, porosity and surface energy, i.e., wettability after thermal treatment between 130 °C (crosslinking) and 1000 °C (pyrolysis) in argon atmosphere was observed. While low-temperature pyrolyzed foams are elastic and hydrophobic, foams pyrolyzed at high temperatures are brittle and hydrophilic, and they possess higher compression strength. Changes of these properties were correlated with the polymer-to-ceramic transformation. Full article

(This article belongs to the Special Issue Advances in Functional Cellular Structures and Composites)

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