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The infrared-optical properties and particularly the emissivity of sintered ceramics depend on the material's bulk properties and structural properties such as porosity, pore size distribution and pore diameter. The infrared-optical properties can be varied across a wide range by specifically selecting the material's bulk and structural properties. A major concern of the present study is the development of a ceramic coating material with a total emissivity below 0.2 at a temperature of 800 °C. For this purpose, various samples of a TiO2-Y2O3 (TY) ceramic composite were produced with different properties. On variation in the Y2O3 content from 5 to 60 wt%, the porosity of the ceramic composites varies from 3 % to 47 % with the mean pore diameter lying in a range from 0.3 µm to 1.7 µm. The addition of graphitic pore builders increases the porosity up to 60 % and the mean pore diameter to a maximum of 15 µm. By optimizing the total porosity and the pore size of the TY ceramics, a total emissivity as low as 0.17 at 800 °C could be achieved.
Transparent microspheres with the eutectic composition 65 Al2O3-16 Y2O3-19 ZrO2 (mol%) have been produced by laser fusing with a CO2 laser. The influence of the starting material – not pre-calcined and pre-calcined – as well as the laser power on the resulting microspheres – was investigated. After fabrication, the microspheres were analyzed by means of XRD to quantify the amorphous content of the spheres as well as to identify the residual crystalline phases, with a laser granulometer to measure the particle sizes of the starting material and the resulting microspheres, with DSC to characterize the glass transition temperature and crystallization behavior, and with SEM to investigate the microstructure of the microspheres. The laser-treated materials consist of transparent and opaque beads as well as sintered particles. The amorphous amount in the samples was detected to be ~ 85 %. Based on these results transparent beads were collected and annealed over a range of temperatures to analyze the crystallization behavior.
Advancements in the fields of biocompatible materials, manufacturing processes, computational methods and medicine have led to the emergence of a new field: micro-scale scaffolds for bone replacement and regeneration. Yet most such scaffolds produced today are characterized by very basic geometry, and their microstructure differs greatly from that of the actual tissue they are intended to replace. In this paper, we propose a novel approach for generating micro-scale scaffolds based on processing actual micro-CT images and then reconstructing a highly accurate geometrical model. This model is manufactured by means of a state-of-the-art 3D additive manufacturing process from biocompatible materials. At the micro-scale level, these scaffolds are very similar to the original tissue, thus interfacing better with the surrounding tissue and facilitating more efficient rehabilitation for the patient. Moreover, the approach facilitates the design and manufacture of patient-specific scaffolds which can copy patients exact structural and mechanical characteristics, taking into account their physical condition and medical history. By means of multi-resolution volumetric modeling methods, scaffold porosity can also be adapted according to specific mechanical requirements. The process of designing and manufacturing micro-scale scaffolds involves five major stages: (a) building a volumetric multi-resolution model from micro-CT images; (b) generation of surface geometric model in STL format; (c) additive manufacturing of the scaffold; (d) scaffold shape verification relative to the geometric design; and (e) verification of mechanical properties through finite element analysis. In this research, all the proposed stages of the approach were tested. The input included micro-CT scans of porous ceramic structure, which is quite similar to commercial porous scaffolds. The results show that the proposed method is feasible for design and manufacture of micro-scale scaffolds.
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.
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.
Porous Si3N4 ceramics were prepared via partial nitridation and self-propagating high temperature synthesis (SHS) process. Raw Si and additive Y2O3 were mixed and molded under 10 MPa into a compact, the compact was partial nitridation at 1300 °C to form a porous Si/Si3N4, and then it was buried in a Si/Si3N4 bed for SHS to obtain porous Si3N4 with rod-like β-Si3N4 morphology. The processing combined the advantages of the nitridation of Si and SHS with low cost, low shrinkage and time saving. Porous Si3N4 with a porosity of 47%, a strength of 143 MPa were obtained by this method.
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.
The production of agglomerate-free SiO2 particles exhibiting a monomodal distribution of particle sizes of around 300 nm by means of direct laser fuming of micrometric SiO2 powders has been successfully demonstrated. With a 12 kW cw CO2 laser system, a production rate of up to 1 kilogram powder per hour was achieved. Almost ideal spherical amorphous SiO2 particles in a broad particle size distribution between 10 nm and several 100 nm (d50 ≈ 300 nm) were synthesized. Several observations suggest weak agglomeration forces between the particles. A temperature reduction of 200 °C for sintering powder compacts was observed.
The most successful additive manufacturing (AM) technologies are based on the layer-by-layer deposition of a flowable powder. Although considered as the third industrial revolution, one factor still limiting these processes to become completely autonomous is the often necessary build-up of support structures. Besides the prevention of lateral shifts of the part during the deposition of layers, the support assures quality and stability to the built process. The loose powder itself surrounding the built object, or so-called powder-bed, does not provide this sustenance in most existent technology available. Here we present a simple but effective and economical method for stabilizing the powder-bed, preventing distortions in the geometry with no need for support structures. This effect, achieved by applying an air flow through the powder-bed, is enabling an entirely autonomous generation of parts and is a major contribution to all powder-based additive manufacturing technologies. Moreover, it makes powder-based AM independent of gravitational forces, which will facilitate crafting items in space from a variety of powdery materials.