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Tapes, cast by blade deposition of a lithium aluminosilicate glass slurry, were sintered using a YAG-fiber laser, with the aim of finding suitable parameters for an additive manufacturing process based on layer-wise slurry deposition and selective laser densification. The influence of the laser parameters (output power and scan velocity) on the sintering was evaluated, by scanning electron microscopy and by X-ray diffraction, on the basis of the quality of the processed layer. Well densified samples could be obtained only in a small window of values for the output power and the scan velocity. The measurement of the width of a set of single scanned lines allowed also to estimate the minimum resolution of the system along the layer plane.
Ceramic parts possessing an ordered porosity were produced for the first time by powder-based three-dimensional printing of a preceramic polymer followed by pyrolysis in an inert atmosphere. The main parameters involved in the process were investigated, and the precision of the printed and ceramized parts was assessed by means of scanning electron microscopy and micro computed tomography. The influence of two different printing solvents was investigated and the use of a mixture of 1-hexanol and hexylacetate in particular allowed the production of parts with a relative density of 80% both in the polymeric and in the ceramic state. The mixing of a cross-linking catalyst directly with the printing liquid greatly simplified the process, minimizing the necessity of preprocessing the starting powder. Three-dimensional printing of a preceramic polymer not containing any inert or active fillers was proved to be a feasible, convenient and precise process for the production of porous ceramic possessing a complex, ordered structure, such as stretch-dominated lattices.
Wollastonite (CaSiO 3 ) – diopside (CaMgSi 2 O 6 ) glass-ceramic scaffolds have been successfully fabricated using two different additive manufacturing techniques: powder-based 3D printing (3DP) and digital light processing (DLP), coupled with the sinter-crystallization of glass powders with two different compositions. The adopted manufacturing process depended on the balance between viscous flow sintering and crystallization of the glass particles, in turn in fluenced by the powder size and the sensitivity of CaO – MgO – SiO 2 glasses to surface nucleation. 3DP used coarser glass powders and was more appropriate for low temperature firing (800 – 900 °C), leading to samples with limited crystallization. On the contrary, DLP used finer glass powders, leading to highly crystallized glass-ceramic samples. Despite the differences in manufacturing technology and crystallization, all samples featured very good strength-to-density ratios, which bene fit theiruse for bone tissue engineering applications. The bioactivity of 3D-printed glass-ceramics after immersion in simulated body fluid and the similarities, in terms of ionic releases and hydroxyapatite formation with already validated bioactive glass-ceramics, were preliminarily assessed.
Highly porous (>60% open porosity) glass–ceramic scaffolds with remarkable mechanical properties (compression strength of ~15 MPa) were produced by indirect 3D printing. Precursor glass powders were printed into 3D ordered structures and then heat treated to sinter and develop crystalline phases. The final glass–ceramic contained a β-spodumene solid solution together with a secondary phase of lithium disilicate.
The precision of the printed geometry and the density of the struts in the scaffold depended on several processing parameters (e.g. powder size and flowability, layer thickness) and were improved by increasing the binder saturation and drying time. Two types of powders with different particle size distribution (PSD) and flowability were used. Powders with a larger PSD, could be processed within a wider range of printing parameters due to their good flowability; however, the printing precision and the struts density were lower compared to the scaffolds printed using the powder in a smaller average PSD.
Capsule summary
THE MATERIALS
Manufacturers can use preceramic polymers to produce ceramic components in a range of compositions using a variety of additive manufacturing technologies. Preceramic polymers even can overcome some of the problems that are intrinsic to additive manufacturing in general.
THE APPLICATION
Modifying the composition, molecular architecture, and molecular weight of preceramic polymers allows adaptation of these materials to specific processing requirements of individual additive manufacturing technologies.
THE OPPORTUNITY
Further development of new additive manufacturing technologies, in addition to improvement of existing technologies, will enable manufacturing of advanced ceramic components with enhanced mechanical characteristics and new functional properties.
2014AbstractWollastonite/apatite glass-ceramics have been successfully prepared by a novel approach, consisting of the heat treatment of a silicone resinembedding micro-sized CaCO3particles, that act as reactive fillers, and bioactive glass powder in the SiO2–CaO–P2O5–K2O–Na2O–MgO–CaF2system. Zn-containing silicates, such as hardystonite (Ca2ZnSi2O7) and willemite (Zn2SiO4), were also developed either by directly mixing ZnOpowders with the glass, or by embedding them in the preceramic polymer, as additional fillers.
Silicate bioceramics possess an excellent bioactivity; however, shaping them into complex geometries is still challenging. Therefore, this paper aims to present a new strategy for the shaping of a bioglass-ceramic with controlled geometry and properties starting from a glass powder combined with a preceramic polymer, i.e. a silicon resin, and reactive fillers. The powder-based three-dimensional (3D)-printing of wollastonite (CaSiO3)-based silicate bioceramic parts was demonstrated in this work. The resin plays a dual role, as it not only acts as a non-sacrificial binder for the filler powders in the printing process but it also reacts with the fillers to generate the desired bioceramic phases. The mechanical and physical properties, i.e. ball-on-three-balls test, density, porosity and morphology, were evaluated in 3D-printed discs. These samples possessed a total porosity around 64 vol% and a biaxial flexural strength around 6 MPa. The raw materials used in this work also enabled the 3D-printing of scaffolds possessing a designed multi-scale porosity, suitable bioceramic phase assemblage and a compressive strength of 1 MPa (for cylindrical scaffolds with total porosity ~80 vol%). Solubility in TRIS/HCl and in vitro assays, i.e. viability, cytotoxicity and apoptosis assays, were also performed. In vitro tests indicated good cell viability and no cytotoxicity effect on the cells.
Additive manufacturing (AM) is a technology which has the potential not only to change the way of conventional industrial manufacturing processes, adding material instead of subtracting, but also to create entirely new production and business strategies. Since about three decades, AM technologies have been used to fabricate prototypes or models mostly from polymeric or metallic materials. Recently, products have been introduced into the market that cannot be produced in another way than additively. Ceramic materials are, however, not easy to process by AM technologies, as their processing requirements (in terms of feedstock and/or sintering) are very challenging. On the other hand, it can be expected that AM technologies, once successful, will have an extraordinary impact on the industrial production of ceramic components and, moreover, will open for ceramics new uses and new markets.
In this work, we demonstrated that the hardystonite (Ca2ZnSi2O7) bioceramics can be produced withhigh phase purity, starting from different preceramic polymers and suitable fillers (precursors for CaOand ZnO) after heating at 1200◦C in air. Open-celled hardystonite foams were easily prepared from a filler-containing silicone resin using hydrazine as foaming agent. The fabrication of cellular structures using a preceramic polymer and fillers was possible because the polymeric melt allowed for the entrapment of the gases generated by the decomposition of hydrazine, and the simultaneous cross-linking of the preceramic polymer enabled the retention of the foam structure. Samples with a well-developed hierarchical porous structure, with an open porosity ranging from ∼65 to ∼81 vol% and an average cell window size ranging from 150 to 500 µm were produced. The hardystonite components possessed a compressive strength ranging from ∼1.4 to ∼2.1 MPa.
The possibility of creating patient-specific individual implants makes Additive Manufacturing technologies of special interest for the medical sector. For substitution of bone defects, powder based Additive Manufacturing by Binder Jetting is a suitable method to produce complex scaffold-like structures made of bioceramics with easily adapted geometries and controlled porosity. The process inherent residual porosity in the printed part, even though desired as it supports bone ingrowth, also leads to limited mechanical strength. Currently, bioceramic scaffolds made by Binder Jetting feature suitable biocompatible and biodegradable properties, while a sufficient mechanical stability is rather challenging. The purpose of this work is to apply the gas flow assisted powder deposition introduced in 2014 by Zocca et al., to the powder bed during printing of bioceramic tablets and scaffolds using α-TCP powder as feedstock. This enables exploiting the advantages of an increased powder bed density, thereby improving the mechanical properties of the printed parts.
Advanced ceramics printed with photon-based additive manufacturing deals with anisotropic mechanical properties from the layer-by-layer manufacturing. Motivated by the success in using highly filled transparent slurries containing nanoparticles for powder-based two-photon-polymerization (2PP) for advanced ceramic printing, this works approach is the transfer to Xolography, a volumetric additive manufacturing technology based on linear two-photon excitation and without recoating steps. This paper reports the results of a preliminary investigation optimizing the photocurable slurry to the requirements of Xolography in terms of transparency, over a significantly larger mean free path, compared to 2PP. A feedstock filled with 70 % weight fraction of ceramic particles (∼30 vol%) exhibiting an exceptionally high degree of transparency in the relevant wavelength range of 400–800 nm was prepared from 5 nm zirconia nanoparticles. The high transparency of the photocurable slurry is attributed to the near-monomodal particle size distribution of the zirconia nanoparticles used.
Purpose – This paper aims to present an additive manufacturing-based approach in which a new strategy for a thermally activated local melting and material flow, which results in densification of printed structures, is introduced.
Design/methodology/approach – For enabling this self-organized relaxation of printed objects by the viscous flow of material, two interconnected structures are printed simultaneously in one printing process, namely, Structure A actually representing the three dimensional object to be built and Structure B acting as a material reservoir for infiltrating Structure A. In an additional process step, subsequent to the printing job, an increase in the objects’ temperature results in the melting of the material reservoir B and infiltration of structure A.
Findings – A thermally activated local melting of the polymethylsilsesquioxane results in densification of the printed structures and the local formation of structures with minimum surface area.
Originality/value – The present work introduces an approach for the local relaxation of printed three-dimensional structures by the viscous flow of the printed material, without the loss of structural integrity of the structure itself. This approach is not restricted only to the materials used, but also offers a more general strategy for printing dense structures with a surface finish far beyond the volumetric resolution of the 3D printing process.