Characterization of ceramic components fabricated using binder jetting additive manufacturing technology

Binder jetting additive manufacturing is an emerging technology with capability of processing a wide range of commercial materials, including metals and ceramics (316 SS, 420 SS, Inconel 625, Iron, Silica). In this project, aluminum oxide (Al₂O₃) powder was used for part fabrication. Various build parameters (e.g. layer thickness, saturation, particle size) were modified and different sintering profiles were investigated to achieve nearly full-density parts (~96%). The material's microstructure and physical properties were characterized. Full XRD, compression testing, and dielectric testing were conducted on all parts. Sintered alumina parts were achieved with an average compressive strength of 131.86 MPa (16 h sintering profile) and a dielectric constant of 9.47–5.65 for a frequency range of 20 Hz to 1 MHz. The complexity offered by additive processing aluminum oxide can be extended to the manufacturing of high value energy and environmental components for environmental systems (e.g. filters and membranes) or biomedical implants with integrated reticulated structures for improved osseointegration.     

Concurrent reaction-bonded joining and densification of additively manufactured silicon carbide by liquid silicon infiltration

In this study, additive-manufactured silicon carbide preforms were joined and densified by reaction bonding via liquid silicon infiltration. The silicon carbide preforms were first printed by binder jetting additive manufacturing. To demonstrate concurrent joining and densification, two preforms with carbon or parchment papers at the interface were concurrently joined and infiltrated by liquid silicon. Results showed a robust interface with thicknesses ranging from 150 to 500 µm, depending on the paper type and the number of paper layers. High-energy synchrotron X-ray revealed that β-phase silicon carbide was formed inside the interface. Finally, two additively manufactured samples with complicated channel geometry were successfully joined. Energy dispersive spectroscopy of the interface of the channeled samples showed a consistent and robust joining. This concurrent approach of joining and densification enables efficiency improvement of fabricating silicon carbide parts with complicated geometries and widens geometry freedom for additive manufacturing of silicon carbide.     

Additive manufacturing of zirconia ceramics by material jetting

The possibility of additive manufacturing of ceramics has been reported widely in scientific literature. This study investigates the potential of direct inkjet printing or material jetting of 3Y-TZP ceramics by assessing the microstructure and mechanical properties of the sintered printed parts. The technique allows to print in layers of 10.5 μm, with an as-printed green density of 58 % and nearly fully sintered density of 6.03 ± 0.1 g/cm³ (99.7 % TD). The dimensions of the green and sintered parts were highly accurate but showed an anisotropic roughness in function of the building direction, mainly due to the support structures. The biaxial bending and 4-point bending strength of the sintered material was found to be substantially higher in the XY direction than in the building (Z) direction. SEM and X-Ray computed tomography revealed the presence of delamination cracks, agglomerates and spherical pores, which were identified as fracture origins on fractured surfaces.     

3D printing of porcelain by layerwise slurry deposition

The Layerwise Slurry Deposition is a technology for the deposition of highly packed powder layers. A powder bed is achieved by depositing and drying layers of a ceramic suspension by means of a doctor blade. This deposition technique was combined with the binder jetting technology to develop a novel Additive Manufacturing technology, named LSD-print. The LSD-print was applied to a porcelain ceramic. It is shown that it was possible to produce parts with high definition, good surface finish and at the same time having physical and mechanical properties close to those of traditionally processed porcelain, e.g. by slip casting.This technology shows high future potential for being integrated alongside traditional production of porcelain, as it is easily scalable to large areas while maintaining a good definition. Both the Layerwise Slurry Deposition method and the binder jetting technologies are readily scalable to areas as large as >1?m².     

3D printing of fine alumina powders by binder jetting

Additive manufacturing of ceramics is still at an early-development stage; however, the huge interest in custom production of these materials has led to the development of different techniques that could provide highly performing devices. In this work, alumina (α-Al₂O₃) components were produced by binder jetting 3D printing (BJ), a powder-based technique that enables the ex-situ thermal treatment of the printed parts. The employment of fine particles has led to high green relative density values (>60 %), as predicted by Lubachevsky-Stillinger algorithm and DEM modelling. Then, extended sintering has been observed on samples treated at 1750 °C that have reached a final density of 75.4 %. Finally, the mechanical properties of the sintered material have been assessed through bending test for flexural resistance and micro-indentation for Vickers hardness evaluation.     

Additive manufacturing of zirconia parts by indirect selective laser sintering

Thermally induced phase separation (TIPS) was used to produce spherical polypropylene–zirconia composite powder for selective laser sintering (SLS). The influence of the composition of the composite starting powder and the SLS parameters on the density and strength of the composite SLS parts was investigated, allowing realizing SLS parts with a relative density of 36%. Pressure infiltration (PI) and warm isostatic pressing (WIPing) were applied to increase the green density of the ZrO₂–PP SLSed parts. Infiltrating the SLS parts with an aqueous 30 vol.% ZrO₂ suspension allowed to increase the sintered density from 32 to 54%. WIPing (135 °C and 64 MPa) of the SLS and SLS/infiltrated complex shape green polymer–ceramic composite parts prior to debinding and sintering allowed raising the sintered density of the 3 mol Y₂O₃ stabilized ZrO₂ parts to 92 and 85%, respectively.     

Fabrication of powder components with internal channels by spark plasma sintering and additive manufacturing

A novel method of producing complex ceramic and metallic parts with designed internal channels is developed. The method utilizes a combination of the additive manufacturing technique of solvent jetting and spark plasma sintering (SPS.) The developed manufacturing approach brings benefits in producing complex shapes with internal channels. Along with geometric customization of the 3D printed mold, a major advantage of this method is the removal of the need for a long debinding process, usually necessary with other 3D printing methods, by using the SPS. High density ceramic and metallic complex parts with internal channels were successfully produced with close to theoretical densities. The conducted studies include the development of a model that can predict the evolution and/or distortions of the complex-shaped powder assembly during the sintering process. The model is based on the continuum theory of sintering formulations embedded in a finite element code.     

X-ray tomography of additive-manufactured zirconia: Processing defects – Strength relations

X-ray Computed Tomography (XCT) analysis was applied to identify and quantify typical defects in dense 3Y-TZP zirconia processed by the Lithography-based Ceramic Manufacturing (LCM) technique. XCT derived strengths were anticipated from the XCT data and compared to experimental measurement. A good agreement between XCT data, bending strength measurement and fractographic analysis demonstrates the suitability of X-ray tomography for both defects detection and predictive mechanical strength estimation. It allows also to rank the different defects related to LCM in terms of their criticality versus mechanical resistance.     

Characterization of zirconia specimens fabricated by ceramic on-demand extrusion

The Ceramic On-Demand Extrusion (CODE) process is a novel additive manufacturing method for fabricating dense (~99% of theoretical density) ceramic components from aqueous, high solids loading pastes (>50?vol%). In this study, 3?mol% Y₂O₃ stabilized zirconia (3YSZ) specimens were fabricated using the CODE process. The specimens were then dried in a humidity-controlled environmental chamber and afterwards sintered under atmospheric conditions. Mechanical properties of the sintered specimens were examined using ASTM standard test techniques, including density, Young’s modulus, flexural strength, Weibull modulus, fracture toughness, and Vickers hardness. The microstructure was analyzed and grain size measured using scanning electron microscopy. The results were compared with those from Direct Inkjet Printing, Selective Laser Sintering, Lithography-based Ceramic Manufacturing (LCM), and other extrusion-based processes, and indicated that zirconia specimens produced by CODE exhibit superior mechanical properties among the additive manufacturing processes. Several sample components were produced to demonstrate CODE’s capability for fabricating geometrically complex ceramic components. The surface roughness of these components was also examined.     

Osteoblast behaviour on zirconia fabricated by additive and subtractive technology

Zirconia is an attractive material for the manufacturing of oral implants and patient-individual barriers for guided bone regeneration. This study compared osteoblast behaviour on additive manufactured and milled 3-mol% yttria-stabilized tetragonal polycrystal zirconia (ZrO₂).Two groups of samples (Ø5 × 2 mm) were manufactured by stereolithography (LithaCon 230, Lithoz, Vienna, Austria) and subsequently heat-treated and sintered. One group remained superficially unmodified (AM-ZrO₂-unmod.), while the other was polished according to DIN EN ISO 6872 standard using automated grinding (AM-ZrO₂-pol.). For comparison, milled samples (e.max ZirCAD LT, Ivoclar Vivadent, Schaan, Liechtenstein) were sintered and polished similarly (Mil-ZrO₂-pol.). Surface roughness was characterized using tactile profilometry. Adhesion, proliferation and coverage of human fetal osteoblasts (hFOB 1.19) as well as expression of osteogenic marker genes ALPL and RUNX2 were determined (and statistically compared using Kruskal-Wallis-analyses and Dunn's Post-hoc-tests).The surface roughness of AM-ZrO₂-unmod. Was 45 times higher than that of the polished groups. No significant differences were detected between the three groups regarding cell adhesion and proliferation. With regard to cell coverage, AM-ZrO₂-pol. Significantly outperformed the two other groups (p < 0.05). ALPL- and RUNX2-mRNA expression was insignificantly superior for AM-ZrO₂-unmod. Compared to the two other groups. Therefor no detrimental effect on osteoblast behaviour caused by the investigated, acrylic binder-based 3D printing workflow was observed.