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Understanding the mechanical properties of three-dimensional (3D)-printed ceramics while keeping the parts intact is crucial for advancing their application in high-performance and biocompatible fields, such as biomedical and aerospace engineering. This study uses non-destructive nanoindentation techniques to investigate the mechanical performance of 3D-printed zirconia across pre-conditioned and sintered states. Vat photopolymerization-based additive manufacturing (AM) was employed to fabricate zirconia samples. The structural and mechanical properties of the printed zirconia samples were explored, focusing on hardness and elastic modulus variations influenced by printing orientation and post-processing conditions. Nanoindentation data, analyzed using the Oliver and Pharr method, provided insights into the elastic and plastic responses of the material, showing the highest hardness and elastic modulus in the 0° print orientation. The microstructural analysis, conducted via scanning electron microscopy (SEM), illustrated notable changes in grain size and porosity, emphasizing the influencing of the printing orientation and thermal treatment on material properties. This research uniquely investigates zirconia’s mechanical evolution at the nanoscale across different processing stages—pre-conditioned and sintered—using nanoindentation. Unlike prior studies, which have focused on bulk mechanical properties post-sintering, this work elucidates how nano-mechanical behavior develops throughout additive manufacturing, bridging critical knowledge gaps in material performance optimization.
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Increased strength in carbon-poly(ether ether ketone) composites from material extrusion with rapid microwave post processing
One critical challenge for commercial products manufactured via material extrusion 3D printing is their inferior mechanical properties in comparison to injection molding; in particular, 3D printing leads to weaker properties perpendicular to the plane of the printed roads (z-direction). Here, rapid (≤20 s) post-processing of 3D printed carbon- poly(ether ether ketone) (PEEK) with microwaves is demonstrated to dramatically increase the modulus, such that the z-direction after microwave processing (2.7–3.8 GPa) exhibits a higher elastic modulus than the maximum in any direction for the as-printed part (2.3 GPa). Additionally, the stress at break in the z-orientation is increased by an order of magnitude by microwaves to slign with the stress for other print orientations in the as-printed state. The rapid heating and cooling by coupling of the microwave energy with the carbon filler in the PEEK does not increase the crystallinity of the PEEK, so the increased mechanical properties are attributed to improved interfaces between printed roads. This simple microwave post-processing enables large increases in the elastic modulus of the printed parts and can be tuned by the microwave power. As PEEK is generally difficult to print, these concepts can likely be applied to other commercial engineering plastic filaments that contain carbon or other fillers that are microwave active to rapidly post process 3D printed thermoplastics without requiring modification of the filament with selective placement of microwave absorbers. Additionally, these results demonstrate that the average crystallinity does not necessarily correlate with the strength of 3D printed semicrystalline plastics due to the importance of the details of the interface between adjacent printed roads.
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- PAR ID:
- 10641474
- Publisher / Repository:
- Elseiver
- Date Published:
- Journal Name:
- Additive manufacturing
- Volume:
- 60
- Issue:
- A
- ISSN:
- 2214-8604
- Page Range / eLocation ID:
- 103209
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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Print conditions for thermoplastics by filament-based material extrusion (MatEx) are commonly optimized to maximize the elastic modulus. However, these optimizations tend to ignore the impact of thermal history that depends on the specimen size and print path selection. Here, we investigate the effect of size print path (raster angle and build orientation) and print sequence on the mechanical properties of polycarbonate (PC) and polypropylene (PP). Examination of parallel and series printing of flat (XY) and stand-on (YZ) orientation of Type V specimens demonstrated that to observe statistical differences in the mechanical response that the interlayer time between printed roads should be approximately 5 s or less. The print time for a single layer in XY orientation is much longer than that for a single layer in YZ orientation, so print sequence only impacts the mechanical response in the YZ orientation. However, the specimen size and raster angle did influence the mechanical properties in XY orientation due to the differences in thermal history associated with intralayer time between adjacent roads. Moreover, all of these effects are significantly larger when printing PC than PP. These differences between PP and PC are mostly attributed to the mechanism of interface consolidation (crystallization vs. glass formation), which changes the requirements for a strong interface between roads (crystals vs. entanglements). These results illustrate how the print times dictated by the print path layout impact observed mechanical properties. This work also demonstrated that the options available in some standards developed for traditional manufacturing will change the quantitative results when applied to 3D printed parts.more » « less
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Polyether ether ketone (PEEK) is an organic polymer that has excellent mechanical, chemical properties and can be additively manufactured (3D-printed) with ease. The use of 3D-printed PEEK has been growing in many fields. This article systematically reviews the current status of 3D-printed PEEK that has been used in various areas, including medical, chemical, aerospace, and electronics. A search of the use of 3D-printed PEEK articles published until September 2021 in various fields was performed using various databases. After reviewing the articles, and those which matched the inclusion criteria set for this systematic review, we found that the printing of PEEK is mainly performed by fused filament fabrication (FFF) or fused deposition modeling (FDM) printers. Based on the results of this systematic review, it was concluded that PEEK is a versatile material, and 3D-printed PEEK is finding applications in numerous industries. However, most of the applications are still in the research phase. Still, given how the research on PEEK is progressing and its additive manufacturing, it will soon be commercialized for many applications in numerous industries.more » « less
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Poly(ether ether ketone) (PEEK) was found to form gels in the benign solvent 1,3-diphenylacetone (DPA). Gelation of PEEK in DPA was found to form an interconnected, strut-like morphology composed of polymer axialites. To our knowledge, this is the first report of a strut-like morphology for PEEK aerogels. PEEK/DPA gels were prepared by first dissolving PEEK in DPA at 320 °C. Upon cooling to 50 °C, PEEK crystallizes and forms a gel in DPA. The PEEK/DPA phase diagram indicated that phase separation occurs by solid–liquid phase separation, implying that DPA is a good solvent for PEEK. The Flory–Huggins interaction parameter, calculated as χ12 = 0.093 for the PEEK/DPA system, confirmed that DPA is a good solvent for PEEK. PEEK aerogels were prepared by solvent exchanging DPA to water then freeze-drying. PEEK aerogels were found to have densities between 0.09 and 0.25 g/cm3, porosities between 80 and 93%, and surface areas between 200 and 225 m2/g, depending on the initial gel concentration. Using nitrogen adsorption analyses, PEEK aerogels were found to be mesoporous adsorbents, with mesopore sizes of about 8 nm, which formed between stacks of platelike crystalline lamellae. Scanning electron microscopy and X-ray scattering were utilized to elucidate the hierarchical structure of the PEEK aerogels. Morphological analysis found that the PEEK/DPA gels were composed of a highly nucleated network of PEEK axialites (i.e., aggregates of stacked crystalline lamellae). The highly connected axialite network imparted robust mechanical properties on PEEK aerogels, which were found to densify less upon freeze-drying than globular PEEK aerogel counterparts gelled from dichloroacetic acid (DCA) or 4-chlorphenol (4CP). PEEK aerogels formed from DPA were also found to have a modulus–density scaling that was far more efficient in supporting loads than the poorly connected aerogels formed from PEEK/DCA or PEEK/4CP solutions. The strut-like morphology in these new PEEK aerogels also significantly improved the modulus to a degree that is comparable to high-performance crosslinked aerogels based on polyimide and polyurea of comparable densities.more » « less
- Free Publicly Accessible Full Text
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Accepted Manuscript1.0
- Journal Article:
- https://doi.org/10.1016/j.addma.2022.103209
