Structural Electromagnetic Absorber Based on MoS2 /PyC-Al2 O3 Ceramic Metamaterials.

Limited by the types of suitable absorbents as well as the challenges in engineering the nanostructures (e.g., defects, dipoles, and hetero-interface) using state-of-the-art additive manufacturing (AM) techniques, the electromagnetic (EM) wave absorption performance of the current ceramic-based materials is still not satisfying. Moreover, because of the high residual porosity and the possible formation of cracks during sintering or pyrolysis, AM-formed ceramic components may in many cases exhibit low mechanical strength. In this work, semiconductive MoS2 and conductive PyC modified Al2 O3 (MoS2 /PyC-Al2 O3 ) ceramic-based structural EM metamaterials are developed by innovatively harnessing AM, precursor infiltration and pyrolysis (PIP), and hydrothermal methods. Three different meta-structures are successfully created, and the ceramic-based nanocomposite benefit from its optimization of EM parameters. Ultra-broad effective absorption bandwidth (EAB) of 35 GHz is achieved by establishment of multi-loss mechanism via nanostructure engineering and fabrication of meta-structures via AM. Due to the strengthening by the PyC phase, the bending strength of the resulting ceramics can reach ≈327 MPa, which is the highest value measured on 3D-printed ceramics of this type that has been reported so far. For the first time, the positive effect deriving from the engineering of the microscopic nano/microstructure and of the macroscopic meta-structure of the absorber on the permittivity and EM absorption performance is proposed. Integration of outstanding mechanical strength and ultra-broad EAB is innovatively realized through a multi-scale design route. This work provides new insights for the design of advanced ceramic-based metamaterials with outstanding performance under extreme environment.

Reorientation of Suspended Ceramic Particles in Robocasted Green Filaments during Drying.

This work considers the fabrication of ceramic parts with the help of an additive manufacturing process, robocasting, in which a paste with suspended particles is robotically extruded. Within the final part, the material properties depend on the orientation of the particles. A prediction of the particle orientation is challenging as the part usually undergoes multiple processing steps with varying contributions to the orientation. As the main contribution to the final particle orientation arises from the extrusion process, many corresponding prediction models have been suggested. Robocasting involves, however, further processing steps that are less studied as they have a smaller influence on the orientation. One of the processing steps is drying by natural convection, which follows directly after the extrusion process. A quantification of the reorientation that occurs during drying is mostly unknown and usually neglected in the models. Therefore, we studied the amount of reorientation of suspended particles in robocasted green filaments during drying in detail. For our study, we applied the discrete element method, as it meets various requirements: The exact particle geometry can be resolved precisely; particle-particle interactions can be described; the paste composition is reproduced exactly; the initial particle orientation can be set in accordance with the prediction from the analytical models for the extrusion part; macroscopic force laws exist to represent capillary forces due to the remaining fluid phase that remains during drying. From our study, we concluded that the magnitude of particle reorientation during drying is small compared to the orientation occurring during the extrusion process itself. Consequently, reorientation during drying might further be neglected within analytical orientation prediction models.

Microstructure and Hydrogen Permeability of Nb-Ni-Ti-Zr-Co High Entropy Alloys.

Hydrogen separation membranes are one of the most promising technologies for hydrogen purification. The development of high-entropy alloys (HEAs) for hydrogen separation membranes is driven by a "cocktail effect" of elements with different hydrogen affinities to prevent hydride formation and retain high permeability due to the single-phase BCC structure. In this paper, equimolar and non-equimolar Nb-Ni-Ti-Zr-Co high entropy alloys were fabricated by arc melting. The microstructure and phase composition of the alloys were analyzed by scanning electron microscopy and X-ray diffraction, respectively. The hydrogen permeation experiments were performed at 300-500 °C and a hydrogen pressure of 4 bar. In order to estimate the effect of composition and lattice structure on hydrogen location and diffusivity in Nb-Ni-Ti-Zr-Co alloy, ab initio calculations of hydrogen binding energy were performed using virtual crystal approximation. It was found that Nb-enriched and near equimolar BCC phases were formed in Nb20Ni20Ti20Zr20Co20 HEA while Nb-enriched BCC and B2-Ni(Ti, Zr) were formed in Nb40Ni25Ti18Zr12Co5 alloy. Hydrogen permeability tests showed that Nb20Ni20Ti20Zr20Co20 HEA shows lower activation energy and higher permeability at lower temperatures as well as higher resistance to hydrogen embrittlement compared to Nb40Ni25Ti18Zr12Co5 alloy. The effect of composition, microstructure and hydrogen binding energies on permeability of the fabricated alloys was discussed.

Novel hybrid method to additively manufacture denser graphite structures using Binder Jetting.

This study introduces two hybrid processes integrating an additive manufacturing technique with post-processing treatments namely (i) Binder Jetting Printing (BJP) + Cold Isostatic Pressing (CIP) + cycle and (ii) BJP + cycle where cycle refers to a sequence of Impregnation-Drying-Pyrolysis. These two new processes yielded additively manufactured parts with higher density and reduced defects/porosities. As a testbed, we used these new processes to fabricate graphite structures. The samples produced by both methods were compared with each other and benchmarked to the samples produced by (a) BJP alone and (b) Traditional uniaxial pressing like compaction moulding. Various characterisation methods were used to investigate the microstructure and mechanical properties which showed that the porosity of hybrid manufactured samples reduces from 55% to a record 7%. This technological pathway is expected to create a new avalanche of industrial applications that are hitherto unexplored in the arena of hybrid additive manufacturing with BJP method.

Microstructural Analysis of Novel Preceramic Paper-Derived SiCf/SiC Composites.

This paper presents the results of microstructural analysis of novel preceramic paper-derived SiCf/SiC composites fabricated by spark plasma sintering. The sintering temperature and pressure were 2100/2200 °C and 60/100 MPa, respectively. The content of fibers in the composites was approx. 10 wt %. The SiCf/SiC composites were analyzed by positron annihilation methods, X-ray diffraction technology, scanning electron microscopy, and Raman spectroscopy. Longer sintering time causes the proportion of the 6H-SiC composition to increase to ~80%. The increase in sintering temperature from 2100 °C to 2200 °C leads to partial transition of 4H-SiC to 6H-SiC during the sintering process, and the long-life component of positrons indicates the formation of Si vacancies. The Raman characteristic peaks of turbostratic graphite appear in the Raman spectrum of SiC fibers, this is caused by the diffusion of carbon from the surface of the SiC fiber and the preceramic paper during the high-temperature sintering process.

Preceramic Paper-Derived SiCf/SiCp Composites Obtained by Spark Plasma Sintering: Processing, Microstructure and Mechanical Properties.

Ceramic matrix composites (CMCs) based on silicon carbide (SiC) are promising materials for applications as structural components used under high irradiation flux and high temperature conditions. The addition of SiC fibers (SiCf) may improve both the physical and mechanical properties of CMCs and lead to an increase in their tolerance to failure. This work describes the fabrication and characterization of novel preceramic paper-derived SiCf/SiCp composites fabricated by spark plasma sintering (SPS). The sintering temperature and pressure were 2100 °C and 20-60 MPa, respectively. The content of fibers in the composites was approx. 10 wt.%. The matrix densification and fiber distribution were examined by X-ray computed tomography and scanning electron microscopy. Short processing time avoided the destruction of SiC fibers during SPS. The flexural strength of the fabricated SiCf/SiCp composites at room temperature varies between 300 and 430 MPa depending on the processing parameters and microstructure of the fabricated composites. A quasi-ductile fracture behavior of the fabricated composites was observed.

Porous ceramic bone scaffolds for vascularized bone tissue regeneration.

Hydroxyapatite scaffolds with a multi modal porosity designed for use in tissue engineering of vascularized bone graft substitutes were prepared by three dimensional printing. Depending on the ratio of coarse (mean particle size 50 microm) to fine powder (mean particle size 4 microm) in the powder granulate and the sintering temperature total porosity was varied from 30% to 64%. While macroscopic pore channels with a diameter of 1 mm were created by CAD design, porosity structure in the sintered solid phase was governed by the granulate structure of the printing powder. Scaffolds sintered at 1,250 degrees C were characterized by a bimodal pore structure with intragranular pores of 0.3-0.4 microm and intergranular pores of 20 microm whereas scaffolds sintered at 1,400 degrees C exhibit a monomodal porosity with a maximum of pore size distribution at 10-20 microm. For in-vivo testing, matrices were implanted subcutaneously in four male Lewis rats. Scaffolds with 50% porosity and an average pore size of approximately 18 microm were successfully transferred to rats and vascularized within 4 weeks.