Dan Thoma

Solidification cracking and liquation cracking have been reported frequently in additive manufacturing (AM) as well as welding. In the vast majority of weldability tests, a single-pass, single-layer weld is tested though multiple-pass, multiple-layer welding is common in welding practice. In AM, evaluating the cracking susceptibility based on the total number or length of cracks per unit volume requires repeated cutting and polishing of a built object, and the cracks are often too small to open easily for fracture-surface examination. The present study identified an existing weldability test and modified it to serve as a cracking susceptibility test for AM. A single-pass, single-layer deposit of metal powder was made along a slender specimen that was pulled like in tensile testing but with acceleration. Cracks were visible on the deposit surface and opened easily for examination. The critical pulling speed, i.e., the minimum pulling speed required to cause cracking, was determined as an index for the cracking susceptibility. The lower the critical pulling speed is, the higher the cracking susceptibility. 6061 Al and 7075 Al alloys were selected for testing in view of their high susceptibility to solidification cracking and liquation cracking in welding, respectively.

With the advent of additive manufacturing, manipulation of typical microstructural elements such as grain size, texture, and defect densities is now possible at a faster time scale. While the processing–structure–property relationship in additive manufactured metals has been well studied over the past decade, little work has been done in understanding how this process affects the dynamic behavior of materials. We postulate that additive manufacturing can be used to alter the material microstructure and used to enhance its dynamic strength. In this work, 316L stainless steel (SS) was manufactured via selected laser melting and its microstructure was altered through changing build parameters like laser power, speed, and hatch spacing systematically. These samples were then subjected to spall recovery experiments to measure the spall strength and quantify the amount of damage as a function of build parameters. By mapping the spall strength as a function of build parameters, this work demonstrated that indeed additive manufacturing can be used to tailor the spall strength of 316L SS. This work also determined the optimum build parameters (laser power=195W; scanning speed=1083mm/s; hatch spacing=0.09mm; layer thickness=0.02mm) to obtain the highest spall strength and the least amount of total damage in 316L SS. Microstructural characterization of the pre- and post-mortem samples revealed that increased grain average misorientation and textural index were the main driving force behind this higher spall strength. This work aims to enhance microstructural engineering techniques to design materials with greater resistance to dynamic shock loading.

Generating reduced-order, synthetic grain structure datasets that accurately represent the measured grain structure of a material is important for reducing the cost and increasing the accuracy of computational crystal plasticity efforts. This study introduces a machine-learning-based approach, termed texture adaptive clustering and sampling (TACS), for generating representative Euler angle datasets that accurately mimic the crystallographic texture. The TACS approach employs K-means clustering and density-based sampling in a closed-loop iteration to create representative Euler angle datasets. Proof-of-principle experiments were performed on rolled and recrystallized low-carbon steel. Validation of the TACS approach was extended to twenty-two datasets, varying lattice structures, and complex crystallographic textures, thereby encompassing a broad range of materials and crystal structures. Kolmogorov-Smirnov (K-S) test comparisons underscore the performance of the TACS approach over traditional electron backscatter diffraction EBSD dataset reduction techniques, with average K-S test scores nearing 0.9, indicating a high-fidelity representation of the original datasets. In contrast, conventional methods display scores below 0.3, indicating less reliability of the structure representation. The independence of the TACS approach from material texture and its capability to autonomously generate datasets with predetermined data points demonstrates its unbiased potential in streamlining dataset preparation for crystallographic analysis.

Bulk metallic glasses can exhibit novel material properties for engineering scale components, but the experimental discovery of new alloy compositions is time intensive and thwarts the rate of discovery. This study presents an experimental, high-throughput methodology to increase the speed of discovery for potential bulk metallic glass alloys. A well-documented system, Mg-Cu-Y, was used as a model system. A laser additive manufacturing technique, directed energy deposition, was used for the in situ alloying of elemental powders to synthesize discrete compositions in the ternary system. The laser processing technique can supply the necessary cooling rates of 103–104 Ks−1 for bulk metallic glass formation. The in situ alloying enables the rapid synthesis of compositional libraries with larger sample sizes and discrete compositions than are provided by combinatorial thin films. Approximately 1000 discrete compositions can be synthesized in a day. Surface smoothness, as discerned by optical reflectivity, can suggest glass-forming alloys. X-ray diffraction coupled with energy dispersive X-ray spectroscopy can further refine amorphous alloy signatures and compositions. Transmission electron microscopy confirms amorphous samples. The tiered rate of amorphous alloy synthesis and characterization can survey a large compositional space and permits a glass-forming range to be identified within one week, making the process at least three orders of magnitude faster than other discrete composition techniques such as arc-melting or melt-spinning.

The availability of additive manufacturing enables the fabrication of cellular bone tissue engineering scaffolds with a wide range of structural and architectural possibilities. The purpose of bone tissue engineering scaffolds is to repair critical size bone defects due to extreme traumas, tumors, or infections. This research study presented the experimental validation and evaluation of the bending properties of optimized bone scaffolds with an elastic modulus that is equivalent to the young’s modulus of the cortical bone. The specimens were manufactured using laser powder bed fusion technology. The morphological properties of the manufactured specimens were evaluated using both dry weighing and Archimedes techniques, and minor variations in the relative densities were observed in comparison with the computer-aided design files. The bending modulus of the cubic and diagonal scaffolds were experimentally investigated using a three-point bending test, and the results were found to agree with the numerical findings. A higher bending modulus was observed in the diagonal scaffold design. The diagonal scaffold was substantially tougher, with considerably higher energy absorption before fracture. The shear modulus of the diagonal scaffold was observed to be significantly higher than the cubic scaffold. Due to bending, the pores at the top side of the diagonal scaffold were heavily compressed compared to the cubic scaffold due to the extensive plastic deformation occurring in diagonal scaffolds and the rapid fracture of struts in the tension side of the cubic scaffold. The failure in struts in tension showed signs of ductility as necking was observed in fractured struts. Moreover, the fractured surface was observed to be rough and dull as opposed to being smooth and bright like in brittle fractures. Dimple fracture was observed using scanning electron microscopy as a result of microvoids emerging in places of high localized plastic deformation. Finally, a comparison of the mechanical properties of the studied BTE scaffolds with the cortical bone properties under longitudinal and transverse loading was investigated. In conclusion, we showed the capabilities of finite element analysis and additive manufacturing in designing and manufacturing promising scaffold designs that can replace bone segments in the human body.

Bone-related defects that cannot heal without significant surgical intervention represent a significant challenge in the orthopedic field. The use of implants for these critical-sized bone defects is being explored to address the limitations of autograft and allograft options. Three-dimensional cellular structures, or bone scaffolds, provide mechanical support and promote bone tissue formation by acting as a template for bone growth. Stress shielding in bones is the reduction in bone density caused by the difference in stiffness between the scaffold and the surrounding bone tissue. This study aimed to reduce the stress shielding and introduce a cellular metal structure to replace defected bone by designing and producing a numerically optimized bone scaffold with an elastic modulus of 15 GPa, which matches the human’s cortical bone modulus. Cubic cell and diagonal cell designs were explored. Strut and cell dimensions were numerically optimized to achieve the desired structural modulus. The resulting scaffold designs were produced from stainless steel using laser powder bed fusion (LPBF). Finite element analysis (FEA) models were validated through compression testing of the printed scaffold designs. The structural configuration of the scaffolds was characterized with scanning electron microscopy (SEM). Cellular struts were found to have minimal internal porosity and rough surfaces. Strut dimensions of the printed scaffolds were found to have variations with the optimized computer-aided design (CAD) models. The experimental results, as expected, were slightly less than FEA results due to structural relative density variations in the scaffolds. Failure of the structures was stretch-dominated for the cubic scaffold and bending-dominated for the diagonal scaffold. The torsional and bending stiffnesses were numerically evaluated and showed higher bending and torsional moduli for the diagonal scaffold. The study successfully contributed to minimizing stress shielding in bone tissue engineering. The study also produced an innovative metal cellular structure that can replace large bone segments anywhere in the human body.

Acoustic topological systems explore topological behaviors of phononic crystals. Currently, most of the experimentally demonstrated acoustic topological systems are for airborne acoustic waves and work at or below the kHz frequency range. Here, we report an underwater acoustic topological waveguide that works at the MHz frequency range. The 2D topological waveguide was formed at the interface of two hexagonal lattices with different pillar radii that were fabricated with metal additive manufacturing. We demonstrated the existence of edge stages both numerically and in underwater experiments. Our work has potential applications in underwater/biomedical sensing, energy transport, and acoustofluidics.

Insufficient availability of molten salt corrosion‐resistant alloys severely limits the fruition of a variety of promising molten salt technologies that could otherwise have significant societal impacts. To accelerate alloy development for molten salt applications and develop fundamental understanding of corrosion in these environments, here an integrated approach is presented using a set of high‐throughput (HTP) alloy synthesis, corrosion testing, and modeling coupled with automated characterization and machine learning. By using this approach, a broad range of CrFeMnNi alloys are evaluated for their corrosion resistances in molten salt simultaneously demonstrating that corrosion‐resistant alloy development can be accelerated by 2 to 3 orders of magnitude. Based on the obtained results, a sacrificial protection mechanism is unveiled in the corrosion of CrFeMnNi alloys in molten salts which can be applied to protect the less unstable elements in the alloy from being depleted, and provided new insights on the design of high‐temperature molten salt corrosion‐resistant alloys.

The present study demonstrates the development of a dimensionless number to predict the build height in the additive manufacturing technique of directed energy deposition (DED). The build height can also be used to estimate the dendrite arm spacing and, thus, the cooling rate in the fabrication of samples. A baseline sample, 316L stainless steel, was used to fit the build height to the dimensionless number. A range of process parameters, including laser power, laser feed rate, powder flow rate, layer thickness, and hatch spacing, were varied. Based upon dendrite arm spacing, the estimated cooling rate varied between 102 and 104 K/s. Using the fitted relationship for the stainless steel, high-throughput (HT) processing of multi-principal element alloys (MPEAs) was performed. For this study, HT is the ability to fabricate a batch of 25 bulk samples (∼1 cm3) with different compositions within a 5-h period with ±10 at. % accuracy. A range of compositions using in situ alloying of elemental powders in the Fe–Ni–Cr–Mo system were made. The MPEAs' build height followed the same relationship to the dimensionless number as the 316L alloy. The dimensionless number predicts both macro and meso-scale features in HT processing, thus offering a design tool for choosing process parameters in DED additive manufacturing. Also, the ability to control or increase cooling rates can enhance the ability to promote metastability as well as control meso-scale chemical distributions of alloy samples.

Cerebral aneurysm clips are biomedical implants applied by neurosurgeons to re-approximate arterial vessel walls and prevent catastrophic aneurysmal hemorrhages in patients. Current methods of aneurysm clip production are labor intensive and time-consuming, leading to high costs per implant and limited variability in clip morphology. Metal additive manufacturing is investigated as an alternative to traditional manufacturing methods that may enable production of patient-specific aneurysm clips to account for variations in individual vascular anatomy and possibly reduce surgical complication risks. Relevant challenges to metal additive manufacturing are investigated for biomedical implants, including material choice, design limitations, postprocessing, printed material properties, and combined production methods. Initial experiments with additive manufacturing of 316 L stainless steel aneurysm clips are carried out on a selective laser melting (SLM) system. The dimensions of the printed clips were found to be within 0.5% of the dimensions of the designed clips. Hardness and density of the printed clips (213 ± 7 HV1 and 7.9 g/cc, respectively) were very close to reported values for 316 L stainless steel, as expected. No ferrite and minimal porosity is observed in a cross section of a printed clip, with some anisotropy in the grain orientation. A clamping force of approximately 1 N is measured with a clip separation of 1.5 mm. Metal additive manufacturing shows promise for use in the creation of custom aneurysm clips, but some of the challenges discussed will need to be addressed before clinical use is possible.

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012.

Extended abstract of a paper presented at Microscopy and Microanalysis 2008 in Albuquerque, New Mexico, USA, August 3 – August 7, 2008

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2006

A thermodynamically complete equation of state for the compression and heating of near-equiatomic Ni–Ti alloy in the CsCl (B2) structure was predicted, based on quantum-mechanical calculations of the electron ground states and a Grüneisen lattice-thermal model. The quantum-mechanical calculations used ab initio pseudopotentials and the local-density approximation; the accuracy of the calculations was investigated for elemental Ni and Ti. These calculations demonstrated that simple averaging techniques do not provide an accurate prediction of the properties of metal alloys, and rigorous treatment of the electron wave functions is needed. Predictions were also made of the behavior of NiTi under uniaxial loading. The pressure-density relation obtained from isotropic compression did not match the mean pressure calculated from uniaxial compression, demonstrating that it is not generally accurate to split the stress response of a material into a scalar equation of state and a stress deviator according to the usual prescription. Polycrystalline NiTi samples were prepared with a range of compositions, in the form of disks from 100 to 400μm thick and 5mm in diameter. Flyer impact experiments were performed using a long-pulse laser drive at the TRIDENT facility to obtain shock wave data on the response of NiTi to around 15GPa; the new data were consistent with the published results from gas gun experiments. The theoretical equation of state was consistent with the shock wave data.

Using resonant-ultrasound spectroscopy, we measured beryllium’s elastic constants for both a monocrystal and a polycrystal. Thus, we consider the monocrystal–polycrystal elastic-constant relationship for hexagonal symmetry. Beside the Cij, we report the Debye characteristic temperature Θ and the Grüneisen parameter γ. We comment on beryllium’s chemical bonding and its remarkably low Poisson ratio.

New nanocrystalline, multicomponent extremely soft magnetic materials with superior high temperature magnetic properties hold great promise in power applications. Fabricated in ribbon form by rapid solidification methods, the initial material is amorphous. By controlled annealing procedures, the amorphous material was transformed into a nanocrystalline form with the degree of crystallinity determined by the annealing temperature and time. The magnetic structures of ribbons, as-fabricated and annealed at temperatures from 550 to 750 °C were examined by magnetic force microscopy to determine the impact of residual stress and nanocrystallinity on the observed structure. A correlation was seen between the magnetic structures and surface microstructure. The wheel side of the as-processed ribbon was rougher than the top side of the ribbon and a complicated magnetic domain structure was present in the amorphous material. After annealing, nanocrystals formed, increasing in size with increasing temperature. The lowest temperature annealed sample had a bimodal grain size distribution and a combination of stripe and localized domains. After annealing little difference was seen between the two sides of the ribbons. Stripe domains were absent in the ribbons annealed at the highest temperatures.

Laves-phase intermetallics are of potential use as high-temperature structural materials. NbCr2-based C15-structured alloys are of particular interest for such applications. The effect of Ti alloying on the microstucture and mechanical properties of such alloys has been investigated and it has been shown that Ti can improve the fracture toughness of the monolithic CI 5 Laves phase8 and dual-phase (bcc and CI 5) alloys. In the Nb-Cr-Ti system, there is a complete solid solution between NbCr2 and TiCr2, with a significant range of solubility of the C15 phase and a large two phase, bcc and C15, region. The initial characterization of the defect structure of an alloy of overall composition Nb10Cr75Ti15 is discussed here.

Nb10Cr75Ti15 was prepared by arc-melting the high-purity elemental metals followed by annealing at 1400°C for 120 h and then cooling at l°C/min. Specimens were prepared for observation in the TEM by cutting 3 mm discs with a coring saw, followed by dimpling and ion milling.

The development of Fe73.5Si13.5B9Nb3Cu1 (FINEMET) by Yoshizawa et al. and Fe88Zr7B4Cu1 (NANOPERM) by Inoue et al. have shown that nanocrystalline microstructures can play an important role in the production of materials with outstanding soft magnetic properties. The FINEMET and NANOPERM materials rely on nanocrystalline α-Fe3Si and α-Fe, respectively, for their soft magnetic properties. The magnetic properties of a new class of nanocrystalline magnets are described herein. These alloys with a composition of (Fe,Co)–M–B–Cu (where M=Zr and Hf) are based on the α- and α′-FeCo phases, have been named HITPERM magnets, and offer large magnetic inductions to elevated temperatures. This report focuses on thermomagnetic properties, alternating current (ac) magnetic response, and unambiguous evidence of α′-FeCo as the nanocrystalline ferromagnetic phase, as supported by synchrotron x-ray diffraction. Synchrotron data have distinguished between the HITPERM alloy, with nanocrystallites having a B2 structure from the FINEMET alloys, with the D03 structure, and NANOPERM alloys, with the A2 structure. Thermomagnetic data shows high magnetization to persist to the α→γ phase transformation at 980 °C. The room temperature ac permeability has been found to maintain a high value of 1800 up to a frequency of ∼2 kHz. The room temperature core loss has also been shown to be competitive with that of commercial high temperature alloys with a value of 1 W/g at BS=10 kG and f=1 kHz.

Capsules with beryllium ablators have long been considered as alternatives to plastic for the National Ignition Facility laser [J. A. Paisner et al., Laser Focus World 30, 75 (1994)]; now the superior performance of beryllium is becoming well substantiated. Beryllium capsules have the advantages of high density, low opacity, high tensile strength, and high thermal conductivity. Three-dimensional (3-D) calculations with the HYDRA code [NTIS Document No. DE-96004569 (M. M. Marinak et al. in UCRL-LR-105821-95-3)] confirm two-dimensional (2-D) LASNEX [G. B. Zimmerman and W. L. Kruer, Comments Plasmas Phys. Controlled Thermonucl. Fusion 2, 51 (1975)] results that particular beryllium capsule designs are several times less sensitive than the CH point design to instability growth from deuterium-tritium (DT) ice roughness. These capsule designs contain more ablator mass and leave some beryllium unablated at ignition. By adjusting the level of copper dopant, the unablated mass can increase or decrease, with a corresponding decrease or increase in sensitivity to perturbations. A plastic capsule with the same ablator mass as the beryllium and leaving the same unablated mass also shows this reduced perturbation sensitivity. Beryllium’s low opacity permits the creation of 250 eV capsule designs. Its high tensile strength allows it to contain DT fuel at room temperature. Its high thermal conductivity simplifies cryogenic fielding.