Search

Two new refractory amorphous high-entropy alloys (RAHEAs) within the W--Ta--Cr--V and W--Ta--Cr--V--Hf systems were herein synthesized using magnetron-sputtering and tested under high-temperature annealing and displacing irradiation using \textit{in situ} Transmission Electron Microscopy. While the WTaCrV RAHEA was found to be unstable under such tests, additions of Hf in this system composing a new quinary WTaCrVHf RAHEA was found to be a route to achieve stability both under annealing and irradiation. A new effect of nanoprecipitate reassembling observed to take place within the WTaCrVHf RAHEA under irradiation indicates that a duplex microstructure composed of an amorphous matrix with crystalline nanometer-sized precipitates enhances the radiation response of the system. It is demonstrated that tunable chemical complexity arises as a new alloy design strategy to foster the use of novel RAHEAs within extreme environments. New perspectives for the alloy design and application of chemically-complex amorphous metallic alloys in extreme environments are presented with focus on their thermodynamic phase stability when subjected to high-temperature annealing and displacing irradiation.

Nickel-based alloys are extensively used in a wide range of extreme environments because of their exceptional mechanical properties. The excellent strength of these alloys is derived from the addition of long-range ordered precipitates, introduced by thermal aging. The interactions between the dislocations and LRO precipitates dictate the deformation modes and plastic response in these alloys. While the majority of studies have focused on L12-structured precipitate-strengthened Ni-based alloys, less work has considered the Ni-based alloys containing Pt2Mo-structured, Ni2(Cr,Mo)-typed precipitates. In these alloys, Pt2Mo-structured precipitates enable room-temperature deformation twinning in addition to slip, which increases strain hardenability measured from bulk mechanical testing. Although previous geometric-based model suggested that deformation twinning is favored over slip, the factors that influence the activation between twinning versus slip have not been thoroughly explored in this class of Ni-based alloys. In this work, molecular dynamics examined the possible types of dislocation and Pt2Mo-structured precipitate interactions at low temperature. Combined with in situ micromechanical testing, the role of resolved shear stresses on dislocation partials were shown to directly influence the activation of slip versus twinning. Additionally, using an energy-based approach, molecular dynamics results demonstrated a novel twin formation process, caused by the dislocation interaction with the Pt2Mo-structured precipitates.

Microtensile testing of structural materials offers several advantages over conventional mesoscale tests, including the ability to target specific areas of interest and directly correlate the mechanical response to the microstructure of the material. As this technique becomes more widely adopted, it has the potential to have a tremendous impact in the nuclear materials field. However, further work on establishing appropriate testing parameters, unifying testing procedures, and demonstrating the effectiveness of the methodology is required before microtensile tests can be used to replace mesotensile tests for the qualification of materials for use in reactor environments. As a first step towards bridging the experimental length-scale gap for tensile tests, we conducted micro- and mesotensile tests on polycrystalline 304 stainless steel and directly compared the test data to identify the size scaling behavior in such material. Comparison of the results obtained on these two length scales clearly illustrates the specimen size effect, with smaller being stronger. The paper discusses the limitations of microtensile testing, outlines the challenges involved in interpretation of its results, and lists the lessons learned through the process.

Femtosecond laser cutting has been used to fabricate micro- and mesoscale specimens for mechanical testing, but the impact on mechanical properties has not been fully evaluated. Micropillars of various sizes were fabricated in a single crystal Cu specimen and Cu irradiated to 1.4 peak displacements per atom using a femtosecond laser cutting system followed by focused ion beam milling to a final dimension of 7 μm × 7 μm × 12 μm. Microcompression testing showed that removing 5 μm of material from the laser cut surface in both specimens resulted in similar behavior to purely focused ion beam milled micropillars.

CrAlN and CrAlSiN hard coatings deposited by magnetron sputtering were analyzed for their high temperature mechanical and tribological properties. High temperature nanoindentation measurements on both coatings were performed from room temperature up to 700 °C in steps of 100 °C where a reduction in hardness H and elastic modulus E* from their initial values was noticed. In addition, high temperature tribological tests were conducted in inert atmosphere in the same temperature range to obtain information about the coefficient of friction and the wear coefficient. In order to link the tribological behavior to the obtained mechanical properties, the H/E* ratio was calculated and compared to the high temperature wear from the current and other studies with similar coatings. The evolution of the mechanical and tribological properties at high temperature is discussed based on the current knowledge available in literature.

In the study of single cell RNA-seq data, a key component of the analysis is to identify sub-populations of cells in the data. A variety of approaches to this have been considered, and although many machine learning based methods have been developed, these rarely give an estimate of uncertainty in the cluster assignment. To allow for this probabilistic models have been developed, but single cell RNA-seq data exhibit a phenomenon known as dropout, whereby a large proportion of the observed read counts are zero. This poses challenges in developing probabilistic models that appropriately model the data. We develop a novel Dirichlet process mixture model which employs both a mixture at the cell level to model multiple populations of cells, and a zero-inflated negative binomial mixture of counts at the transcript level. By taking a Bayesian approach we are able to model the expression of genes within clusters, and to quantify uncertainty in cluster assignments. It is shown that this approach out-performs previous approaches that applied multinomial distributions to model single cell RNA-seq counts and negative binomial models that do not take into account zero-inflation. Applied to a publicly available data set of single cell RNA-seq counts of multiple cell types from the mouse cortex and hippocampus, we demonstrate how our approach can be used to distinguish sub-populations of cells as clusters in the data, and to identify gene sets that are indicative of membership of a sub-population. The methodology is implemented as an open source Snakemake pipeline available fromhttps://github.com/tt104/scmixture.

Small-scale mechanical testing techniques are currently being explored and developed for engineering applications. In particular, micro-tensile testing can add tremendous value, since the entire stress-strain curve, including the strain to failure, can be measured directly. In this work, 304 stainless steel specimens irradiated with 2 MeV protons to 10 dpa (full-cascade setting in the Stopping and Range of Ions in Matter, SRIM, software) at 360 °C was evaluated using micro-tensile testing. It was found that even on the micron scale, the measured strain corresponds well with macroscopic expectations. In addition, a new approach to analyzing sudden slip events is presented.

Experimentally quantifying the mechanical effects of radiation damage in reactor materials is necessary for the development and qualification of new materials for improved performance and safety. This can be achieved in a high-throughput fashion through a combination of ion beam irradiation and small scale mechanical testing in contrast to the high cost and laborious nature of bulk testing of reactor irradiated samples. The current work focuses on using spherical nanoindentation stress-strain curves on unirradiated and proton irradiated (10 dpa at 360 °C) 304 stainless steel to quantify the mechanical effects of radiation damage. Spherical nanoindentation stress-strain measurements show a radiation-induced increase in indentation yield strength from 1.36 GPa to 2.72 GPa and a radiation-induced increase in indentation work hardening rate of 10 GPa–30 GPa. These measurements are critically compared against Berkovich nanohardness, micropillar compression, and micro-tension measurements on the same material and similar grain orientations. The ratio of irradiated to unirradiated yield strength increases by a similar factor of 2 when measured via spherical nanoindentation or Berkovich nanohardness testing. A comparison of spherical indentation stress-strain curves to uniaxial (micropillar and micro-tension) stress-strain curves was achieved using a simple scaling relationship which shows good agreement for the unirradiated condition and poor agreement in post-yield behavior for the irradiated condition. The disagreement between spherical nanoindentation and uniaxial stress-strain curves is likely due to the plastic instability that occurs during uniaxial tests but is absent during spherical nanoindentation tests.

Recent developments in micromechanical testing have allowed for the efficient evaluation of radiation effects in micron-scale volumes of ion-irradiated materials. In this study, both nanoindentation and in situ SEM microcompression testing are carried out on 10 dpa proton beam irradiated 304 stainless steel to assess radiation hardening and radiation-induced deformation mechanisms in the material. Using a focused ion beam (FIB), arrays of 2 μm × 2 μm cross-section microcompression pillars are fabricated in multiple dose regimes within the same grain, providing dose-dependent behavior in a single crystal orientation. Analysis of the microcompression load-displacement data and real-time SEM imaging during testing indicates significant hardening, as well as increased localization of deformation in the irradiated material. Although nanoindentation results suggest that irradiation hardening saturates at low doses, microcompression results indicate that the pillar yield stress continues to rise with dose above 10 dpa in the tested orientation.

Ni-based alloy 600 has been used as steam generator tubes in many pressurized water reactors (PWR). In these materials, oxidized grain boundaries are found, which may lead to (initiate) stress corrosion cracking in service. This work evaluates the cracking of oxidized grain boundaries on alloy 600. Novel testing procedure was developed, delivering not just yield strength, ultimate tensile strength and elongation data, but also direct observation of the failure. The information obtained will help to understand the stress corrosion cracking susceptibility of this alloy. It was found that the orientations of the two grains adjacent to a grain boundary play an important role in determining its propensity to crack; it also determines whether blocked volume ratio is an important consideration. Furthermore, it is found that the grain boundary shear stress needs to be considered in addition to the grain boundary normal stress.

Understanding the influence of radiation damage on the mechanical properties of HT-9 and other tempered martensitic alloys is part of the mission in developing radiation-tolerant materials for the next generation of nuclear reactors. Although there has been extensive data on the macroscopic mechanical properties of the irradiated HT-9 alloys and microstructural changes, it is not well-understood how radiation damage and the resulting microstructural changes influence the local mechanical properties. In this study, we utilized in situ SEM microtensile testing to investigate the deformation behavior of specific martensitic boundaries in 1 dpa proton-irradiated HT-9 and answered the question of what is the weakest link. We provided the direct observation of the failure modes of microtensiles containing high angle and low angle martensitic boundaries. In the unirradiated condition, the deformation is ductile and no martensitic boundary failure is observed. In the irradiated condition, the high angle martensitic boundaries are more susceptible to radiation-induced boundary failure as compared to the low angle martensitic boundaries.

Hardness and toughness are among of the most important physical properties of hard coatings and it is important to analyze them at temperatures present during coating applications. CrAlN and CrAlSiN are hard coating materials frequently used in high temperature applications. While both possess high oxidation resistance and thermal stability, they differ in their microstructure. In this work, the fracture toughness of magnetron-sputtered single-layer CrAlN and CrAlSiN hard coatings was determined up to 700 °C by in-situ scanning electron microscopy micro-cantilever deflection tests. The results show a decreasing trend of the fracture toughness with increasing temperature. While both coatings' fracture toughness trends are similar up to 400 °C, they diverge at higher temperatures. In general, the evolution of the fracture toughness with increasing temperature shows similarities to the observed changes in hardness in the same temperature range.

A team of students from the University of California, Berkeley, participated in a blade-smithing competition hosted by the Minerals, Metals, and Materials Society at the TMS 2015 144th annual meeting and exhibition. Motivated by ancient forging methods, the UC Berkeley team chose to fabricate our blade from historical smithing techniques utilizing naturally-occurring deposits of iron ore. This approach resulted in receiving the “Best Example of a Traditional Blade Process/Ore Smelting Technique” award for our blade named “Berkelium.” First, iron-enriched sand was collected from local beaches. Magnetite (Fe3O4) was then extracted from the sand and smelted into individual high- and low-carbon steel ingots. Layers of high- and low-carbon steels were forge-welded together, predominantly by hand, to form a composite material. Optical microscopy, energy dispersive spectroscopy, and Vickers hardness mechanical testing were conducted at different stages throughout the blade-making process to evaluate the microstructure and hardness evolution during formation. It was found that the pre-heat-treated blade microstructure was composed of ferrite and pearlite, and contained many nonmetallic inclusions. A final heat treatment was performed, which caused the average hardness of the blade edge to increase by more than a factor of two, indicating a martensitic transformation.

Small scale mechanical testing (SSMT) allows for the quantification of the mechanical responses for microscale and nanoscale material volumes. It has significant potential in improving our fundamental understanding of plastic deformation and in providing an engineering solution for testing complex and/or critical materials. Importantly, previous studies have revealed that plastic intermittency, manifested as strain bursts, are characteristic of the plastic flow behavior at the small length scale. In this work, interfacial constraint has been utilized to suppress strain bursts in order to stabilize plasticity. A new parameter, blocked volume ratio (BVR), is introduced to quantify the degree of constraint for a microscale specimen due to an interface. We showed that the plastic flow behavior in FCC Ni-based metals is highly dependent on the BVR of the specimen.

Understanding the changes in mechanical properties and failure mechanisms as a function of radiation damage is important for long-term operation of structural components in nuclear reactors. Due to the expense, the activation of the sample, and the long duration of neutron irradiation, ion beam irradiations (proton-irradiation and, increasingly, heavy-ion irradiation) are used as surrogates for neutron irradiation. However, the shallow irradiation depths of ion-beam irradiation have restricted mechanical property measurements until the recent advent of small-scale mechanical testing. In previous studies, nano-hardness and yield strength of proton-irradiated 304SS were measured using nanoindentation and in situ microcompression respectively. This study develops an in situ microtensile testing method to provide direct stress-strain curves, including the strain to failure, which previous studies do not provide. In addition, a novel way of quantifying irradiation-induced susceptibility to slip band formation in microscale specimens was demonstrated. Lastly, the paper introduces a new technique for measuring grain boundary strength, demonstrated on an oxidized grain boundary of Alloy 600 exposed to primary water chemistry environment.

High dielectric constant (high-k) materials are needed for embedded passives in advanced packaging applications. This work presents a systematic theoretical investigation of the effective dielectric constant, dielectric loss of dielectric polymers filled with high-k coated conducting particles with the objective to aid the design of polymer/filler composite materials with high dielectric constant and low dielectric loss at high frequencies. Our results demonstrate that, contrary to prevailing views, the filler concentration and coating layer thickness dependences of the effective dielectric constant and loss are nonmonotonic. Implications for high-k materials design are also outlined.

The existing CAD formulae are complicated and inaccurate at high frequencies. In particular, no closed-form expression has been obtained for the effective dielectric constant of microstrip lines on multi-layed dielectric substrate by considering the line-substrate interphase effect, although attempts have been made to study the finite thickness effect of the conductor and dielectric substrate. The present work represents the first attempt to obtain a closed-form CAD formula for the effective dielectric constant of microstrip lines on dielectric substrates by considering the effect of conductor-substrate interphase, in addition to the skin effect losses, dielectric loss, dispersion and radiation losses based on the quasi-TEM assumption and the superposition of partial capacitance. The model is verified by experimental observations on the effective dielectric constant and its dependence on microstrip dimension and frequency.

The results of small-scale mechanical tests are convoluted by the so-called size effect, whereby materials appear stronger when the scale of the test is reduced to the order of microns or less. The dimensional range over which this occurs has been shown to be linked to a change in sample microstructure, such as the addition of defects induced by irradiation. To investigate this response, a CuCrZr alloy was subjected to proton irradiation and mechanically tested using micro compression of pillars with a range in size. It was found that irradiation defects dominate over the extrinsic size effect and the sensitivity to differences in precipitate microstructure was also somewhat reduced, suggesting that size-independent results could be obtained from much smaller test volumes in irradiated material compared to their non-irradiated counterparts. Finally, comparison was made between the increase in yield strength predicted by models and the experimentally measured values to establish the key parameters driving the strengthening behaviour.