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A limited understanding regarding the underlying dynamics and mechanisms of material removal during continuous wave laser drilling has presented significant challenges in achieving precision and process control. To address this, we employed high-fidelity, in situ synchrotron x-ray imaging to reveal previously unknown material behaviors during continuous wave laser drilling with power modulation. Our findings highlight that high-aspect ratio drill holes are achieved when the laser modulation frequency falls within the range of 8–12 kHz, provided that the laser average power and modulation amplitude levels meet the specified limits. Under these conditions, we identified a material removal mechanism driven by incremental accumulation of recoil pressure that gradually pushes material upward from deep within the substrate to the surface. This mechanism manifested as a low-frequency fluctuation in the vapor depression depth, resulting in periodic instances of material ejection. Furthermore, our study underscores that rapid expansion of the melt pool and the widening of the drill hole opening can impede effective material removal by redirecting energy from material ejection to increasing the melt pool size. This investigation contributes essential insights into the subsurface dynamics involved in the drilling of high-aspect ratio holes, furthering our fundamental understanding of this intricate process. [ABSTRACT FROM AUTHOR]

Various nondestructive diagnostic techniques have been proposed for in situ process monitoring of laser powder bed fusion (LPBF), including melt pool pyrometry, whole-layer optical imaging, acoustic emission, atomic emission spectroscopy, high speed melt pool imaging, and thermionic emission. Correlations between these in situ monitoring signals and defect formation have been demonstrated with acoustic signals having been shown to predict pore formation with especially high confidence in recent machine learning studies. In this work, time-resolved acoustic data are collected in both the conduction and keyhole welding regimes of LPBF-processed Ti-6Al-4V alloy. A non-dimensionalized Strouhal number analysis, used in whistle aeroacoustics, is applied to demonstrate that the acoustic signals recorded in the keyhole regimes can be directly associated with the vapor depression morphology. This mechanistic understanding developed from whistle aeroacoustics shows that acoustic monitoring during the LPBF process can provide a direct probe into the vapor depression dynamics and defect occurrence, especially in the keyhole regimes relevant to printing and defect formation. [ABSTRACT FROM AUTHOR]

Electrolytic manganese dioxide is one of the promising cathode candidates for electrochemical energy storage devices due to its high redox capacity and ease of synthesis. Yet, high‐loading MnO2 often suffers from sluggish reaction kinetics, especially in non‐aqueous electrolytes. The non‐uniform deposition of MnO2 on a porous current collectors also makes it difficult to fully utilize the active materials at high mass loading. Here, a 3D printed graded graphene aerogel (3D GA) that contains sparsely separated exterior ligaments is developed to create large open channels for mass transport as well as densely arranged interior ligaments providing large ion‐accessible active surface. The unique structural design homogenizes the thickness of electro deposited MnO2 even at an ultrahigh mass loading of ≈70 mg cm−2. The electrode achieves a remarkable volumetric capacity of 29.1 mA h cm−3 in the non‐aqueous electrolyte. A Li‐ion hybrid capacitor device assembled with a graded 3D GA/MnO2 cathode and graded 3D GA/VOx anode exhibits a wide voltage window of 0–4 V and a superior volumetric energy density of 20.2 W h L−1. The findings offer guidance on 3D printed electrode design for supporting ultrahigh loading of active materials and developments of high energy density energy storage devices. [ABSTRACT FROM AUTHOR]

Laser powder bed fusion (LPBF) is a highly dynamic multi-physics process used for the additive manufacturing (AM) of metal components. Improving process understanding and validating predictive computational models require high-fidelity diagnostics capable of capturing data in challenging environments. Synchrotron x-ray techniques play a vital role in the validation process as they are the only in situ diagnostic capable of imaging sub-surface melt pool dynamics and microstructure evolution during LPBF-AM. In this article, a laboratory scale system designed to mimic LPBF process conditions while operating at a synchrotron facility is described. The system is implemented with process accurate atmospheric conditions, including an air knife for active vapor plume removal. Significantly, the chamber also incorporates a diagnostic sensor suite that monitors emitted optical, acoustic, and electronic signals during laser processing with coincident x-ray imaging. The addition of the sensor suite enables validation of these industrially compatible single point sensors by detecting pore formation and spatter events and directly correlating the events with changes in the detected signal. Experiments in the Ti–6Al–4V alloy performed at the Stanford Synchrotron Radiation Lightsource using the system are detailed with sufficient sampling rates to probe melt pool dynamics. X-ray imaging captures melt pool dynamics at frame rates of 20 kHz with a 2 µm pixel resolution, and the coincident diagnostic sensor data are recorded at 470 kHz. This work shows that the current system enables the in situ detection of defects during the LPBF process and permits direct correlation of diagnostic signatures at the exact time of defect formation. [ABSTRACT FROM AUTHOR]

Carbon aerogels (CAs) combine unique properties including ultra-high surface area, high electrical conductivity, corrosion resistance, and robust mechanical properties making them ideal materials for electrochemical applications. Traditional CA synthesis results in isotropic, random nanoporous networks that work well for applications relying on diffusional mass transport. However, many applications would benefit from integration of engineered macroporous network structures that enable directed pressure-gradient-driven mass transport. Here, we report on using 3D-printed sacrificial polymeric templates to generate templated CAs (t-CAs) with integrated engineered nonrandom macroporous network structures. Specifically, we used projection micro-stereo-lithography (PμSL) and two-photon polymerization direct laser writing (2PP-DLW) to fabricate millimeter-to-centimeter-sized 3D sacrificial polymeric templates with features ranging from tens of microns (PμSL) to 100s of nanometers (2PP-DLW). T-CAs were fabricated by infiltrating the templates with resorcinol-formaldehyde (RF) precursor solution, followed by carbonization at 1050 °C to simultaneously convert the RF gel to a CA and decompose the 3D-printed template, leaving an embedded templated macroporous network structure behind. X-ray computer tomography confirms integration of the macroporous architecture defined by the template. The templated macroporous architecture improves mass transport in t-CAs compared to traditional bulk CA as demonstrated by more uniform activation and their response in electrochemical cyclic voltammetry and galvanostatic charge-discharge tests. [Display omitted] • Fabrication of carbon aerogels with engineered nonrandom macropore networks. • Using 3D printed sacrificial polymeric templates as molds for carbon aerogels. • Integrated macroporosity improves energy storage performance of carbon aerogels. • Integrated macropores enable more uniform activation of carbon aerogels. • Integration of macroporosity designed for pressure driven mass transport. [ABSTRACT FROM AUTHOR]

X‐ray propagation‐based imaging techniques are well established at synchrotron radiation and laboratory sources. However, most reconstruction algorithms for such image modalities, also known as phase‐retrieval algorithms, have been developed specifically for one instrument by and for experts, making the development and diffusion of such techniques difficult. Here, PyPhase, a free and open‐source package for propagation‐based near‐field phase reconstructions, which is distributed under the CeCILL license, is presented. PyPhase implements some of the most popular phase‐retrieval algorithms in a highly modular framework supporting its deployment on large‐scale computing facilities. This makes the integration, the development of new phase‐retrieval algorithms, and the deployment on different computing infrastructures straightforward. Its capabilities and simplicity are presented by application to data acquired at the synchrotron source MAX IV (Lund, Sweden). [ABSTRACT FROM AUTHOR]

Bone-like materials comprise carbonated-hydroxyapatite nanocrystals (c-Ap) embedding a fibrillar collagen matrix. The mineral particles stiffen the nanocomposite by tight attachment to the protein fibrils creating a high strength and toughness material. The nanometer dimensions of c-Ap crystals make it very challenging to measure their mechanical properties. Mineral in bony tissues such as dentine contains 2~6 wt.% carbonate with possibly different elastic properties as compared with crystalline hydroxyapatite. Here we determine strain in biogenic apatite nanocrystals by directly measuring atomic deformation in pig dentine before and after removing carbonate. Transmission electron microscopy revealed the platy 3D morphology while atom probe tomography revealed carbon inside the calcium rich domains. High-energy X-ray diffraction in combination with in situ hydrostatic pressurization quantified reversible c-Ap deformations. Crystal strains differed between annealed and ashed (decarbonated) samples, following 1 or 10 h heating at 250 °C or 550 °C respectively. Measured bulk moduli (K) and a- / c- lattice deformation ratios (η) were used to generate synthetic K syn and η syn identifying the most likely elastic constants C 33 and C 13 for c-Ap. These were then used to calculate the nanoparticle elastic moduli. For ashed samples, we find an average E 11 =107 GPa and E 33 =128 GPa corresponding to ~5% and ~17% stiffening of the a-/c- axes of the nanocrystals as compared with the biogenic nanocrystals in annealed samples. Ashed samples exhibit ~10% lower Poisson's ratios as compared with the 0.25~0.36 range of carbonated apatite. Carbonate in c-Ap may therefore serve for tuning local deformability within bony tissues. Carbonated apatite nanoparticles, typical for bony tissues, stiffen the network of collagen fibrils. However, it is not known if the biogenic apatite mechanical (elastic) properties differ from those of geologic mineral counterparts. Indeed the tiny dimensions and variable carbonate composition may have strong effects on deformation resistance. The present study provides experimental measurements of the elastic constants which we use to estimate Young's moduli and Poisson's ratio values. Comparison between ashed and annealed dentine samples quantifies the properties of both carbonated and decarbonated apatite nanocrystals. The results reveal fundamental attributes of bony mineral and showcase the additive advantages of combining X-ray diffraction with in situ hydrostatic compression, backed by atom probe and transmission electron microscopy tomography. Image, graphical abstract [ABSTRACT FROM AUTHOR]

Compared to tedious, multi-step treatments for electroless gold plating of traditional thermoplastics, this communication describes a simpler three-step procedure for 3D printed crosslinked polyacrylate substrates. This allows for the synthesis of ultralight gold foam microlattice materials with great potential for architecture-sensitive applications in future energy, catalysis, and sensing. [ABSTRACT FROM AUTHOR]

Monolithic porous bulk materials have many promising applications ranging from energy storage and catalysis to high energy density physics. High resolution additive manufacturing techniques, such as direct laser writing via two photon polymerization (DLW-TPP), now enable the fabrication of highly porous microlattices with deterministic morphology control. In this work, DLW-TPP is used to print millimeter-sized foam reservoirs (down to 0.06 g cm−3) with tailored density-gradient profiles, where density is varied by over an order of magnitude (for instance from 0.6 to 0.06 g cm−3) along a length of <100 µm. Taking full advantage of this technology, however, is a multiscale materials design problem that requires detailed understanding of how the different length scales, from the molecular level to the macroscopic dimensions, affect each other. The design of these 3D-printed foams is based on the brickwork arrangement of 100 × 100 × 16 µm3 log-pile blocks constructed from sub-micrometer scale features. A block-to-block interdigitated stitching strategy is introduced for obtaining high density uniformity at all length scales. Finally, these materials are used to shape plasma-piston drives during ramp-compression of targets under high energy density conditions created at the OMEGA Laser Facility. [ABSTRACT FROM AUTHOR]

Dentin in teeth is a bone-like nanocomposite built of carbonated hydroxyapatite (cHAP) mineral particles, protein, and water. It does not remodel nor heal and is excellently adapted for decades of mechanical function, due to the interplay between its constituents. Using samples of human origin, we combine heat treatments with synchrotron X-ray diffraction, second-harmonic generation microscopy, Raman spectroscopy, and phase contrast-enhanced nanotomography to study the water-assisted functional coupling of the biocomposite components. Across roots we find a gradual reduction in the c-lattice parameter of the cHAP nanocrystals, from 6.894 Å externally down to 6.885 Å on the inside. Thus, the tissue formed at later stages of tooth development around the pulp contains crystals with smaller unit cells. In all regions, a compressive strain of ∼0.3% is observed upon drying by mild heating (125 °C). Dehydration also results in a substantial increase in the averaged microstrain fluctuations in the mineral nanoparticles. The mineral crystallite platelet lengths fall off from ∼36 nm externally to ∼26 nm closer to the pulp. Our results suggest that both morphology and tight mineral-collagen coupling allow mineral nanoparticles in dentin to sustain rather large stresses of 300 MPa, far exceeding mastication loads. [ABSTRACT FROM AUTHOR]

Recent advances in additive manufacturing, specifically direct ink writing (DIW) and ink-jetting, have enabled the production of elastomeric silicone parts with deterministic control over the structure, shape, and mechanical properties. These new technologies offer rapid prototyping advantages and find applications in various fields, including biomedical devices, prosthetics, metamaterials, and soft robotics. Stereolithography (SLA) is a complementary approach with the ability to print with finer features and potentially higher throughput. However, all high-performance silicone elastomers are composites of polysiloxane networks reinforced with particulate filler, and consequently, silicone resins tend to have high viscosities (gel- or paste-like), which complicates or completely inhibits the layer-by-layer recoating process central to most SLA technologies. Herein, the design and build of a digital light projection SLA printer suitable for handling high-viscosity resins is demonstrated. Further, a series of UV-curable silicone resins with thiol-ene crosslinking and reinforced by a combination of fumed silica and MQ resins are also described. The resulting silicone elastomers are shown to have tunable mechanical properties, with 100–350% elongation and ultimate tensile strength from 1 to 2.5 MPa. Three-dimensional printed features of 0.4 mm were achieved, and complexity is demonstrated by octet-truss lattices that display negative stiffness. [ABSTRACT FROM AUTHOR]

James S. Oakdale, Juergen Biener, and co‐workers report 3D‐printing of low density foams with submicrometer features in article number 1702425. The foam is successfully applied in plasma drive shaping: A plasma shock wave travels through the foam before impinging upon and ramp compressing an aluminum sample to pressures of over 50 GPa. The 3D printed foam helps to smoothen and shape the plasma piston drive, thereby ensuring uniform compression. [ABSTRACT FROM AUTHOR]