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Hosemann, Peter

Publications and source records attributed to Hosemann, Peter.

At least 37 records · Page 2

A free-standing lithium phosphorus oxynitride thin film electrolyte promotes uniformly dense lithium metal deposition with no external pressure

Lithium phosphorus oxynitride (LiPON) is an amorphous solid electrolyte that has been extensively studied over the last three decades. Despite the promise of pairing it with various electrode materials, LiPON’s rigidity and air sensitivity set limitations to understanding its intrinsic properties. We report a methodology to synthesize LiPON in a free-standing form that manifests remarkable flexibility and a Young’s modulus of ∼33 GPa. We use solid-state nuclear magnetic resonance and differential scanning calorimetry to quantitatively reveal the chemistry of the Li/LiPON interface and the presence of a well-defined LiPON glass-transition temperature of 207 °C. Combining interfacial stress and a gold seeding layer, our free-standing LiPON shows a uniformly dense deposition of lithium metal without the aid of external pressure. This free-standing LiPON film offers opportunities to study fundamental properties of LiPON for interface engineering for solid-state batteries.

25 ENERGY STORAGE↗

Multi–length scale characterization of point defects in thermally oxidized, proton irradiated iron oxides

A key for the success of safe nuclear power generation system is to consider structural materials that are economical, meet mechanical property needs, possess good corrosion resistance, and are radiation tolerant. Nevertheless, fundamental insights that elucidate the details of radiation damage on materials corrosion performance are lacking. This includes the behavior of surface oxides which often regulate corrosion. For example, it is unclear how non-equilibrium point defects, oxide structure, mass transport in oxides, and subsequent oxidation behavior are altered by the radiation. Here, in this work, some of the effects of proton irradiation on the attributes of point defects, iron oxide microstructures, and the physical nature of the oxidation product were correlated with corrosion behavior. Iron oxides, fabricated by thermal oxidation in air at 400°C and 800°C for 1 h, were subjected to 200 keV, 0.03 dpa (displacements per atom) of proton irradiation, and subjected to corrosion reactivity assessment using AC and DC electrochemical methods. Experimental methods that target materials information at different length scales, such as positron annihilation spectroscopy (atomistic), transmission electron microscopy (mesoscopic), and electrochemical methods (macroscopic), were coupled to shed light on the impact of radiation-induced defect modifications and structural changes in oxides on corrosion reactivity which ultimately affects durability in harsh environments.

36 MATERIALS SCIENCE↗

Overview of a Versatile Loading System for Anisotropic Material Property Characterization

Additive manufacturing, cold rolling, and other thermomechanical treatments on metals, especially HCP, can cause texture and oriented grain structures resulting in anisotropic mechanical properties. This can lead to macroscopic response that significantly deviates from isotropic assumptions which motivates studying mechanical properties in multiple directions. In addition, multiaxial loading and complex stress states overlapping the above mentioned material anisotropy can lead to unexpected outcomes. Idaho National Laboratory developed an advanced mechanical testing system to study a range of uniaxial to multiaxial stress states while measuring the anisotropic response bringing insight into the overlap between material properties and stress states. High-temperature capability and stress- or strain-controlled loading is available to enable a variety of experiment types and conditions to measure elastic, plastic, and viscoplastic properties. This poster presents the design and capabilities of this system with preliminary results highlighting the benefits of multiaxial loading and anisotropic analysis in an integrated system.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of tellurium concentration on the corrosion and mechanical properties of 304 stainless steel in molten FLiNaK salt

In this study, the effect of Te concentration in molten FLiNaK salt on the corrosion and mechanical properties of 304 stainless steel was investigated. The corrosion depth of samples after the immersion tests for 48 h at 600 °C decreased with increasing Te concentration. Likewise, the sample after the immersion test containing 1.0 wt% of Te (1.0 wt% Te sample) showed less reduction in mechanical properties than the 0.1 wt% Te sample. We hypothesize that the condition for a Cr-oxide layer that has the protective property is fulfilled underneath the Ni-Fe rich layer which is formed by the selective leaching of Cr.

36 MATERIALS SCIENCE↗

Bridging the length scales on mechanical property evaluation (Final Report)

The development of small-scale mechanical testing in combination with microstructural investigation is of great interest to the nuclear materials community for both materials development and monitoring applications. Dramatically reducing the sample sizes to reduce radioactivity and obtaining mechanical properties of irradiated samples is truly intriguing. Moreover, such studies promise a range of benefits including cost reduction, fundamental insight in structure-property relationships, increased statistics on less sample material, and reinvestigation of prior irradiated and tested reactor samples while simultaneously enabling the generation of mechanical test data on ion beam irradiated materials with limited penetration depths. Small scale materials testing on sub-sized samples has been studied for several decades, though it has only been after the development of micro-testing based on Focused Ion Beam (FIB) sample manufacturing in that orders of magnitude smaller samples could really be investigated in a quantitative manner. In recent years, small scale mechanical testing techniques at a number of length scales has been developed for both unirradiated and irradiated (ion and neutron) materials. Technological advances made in this field have enabled ex-situ and in-situ transmission electron microscopy (TEM) and scanning electron microscopy (SEM) examination, thus leading to more accurate measurements as well as additional mechanistic information. A recent review of the benefits of these techniques show that these techniques are at a stage to tackle multi-scale ranges of materials investigations and can be utilized to obtain fundamental science-based understanding of nuclear materials. Considering the tremendous advances made, one can see how small-scale mechanical testing techniques combined with modeling can enable true small scale to bulk scale mechanical property correlations. However, for the engineering community to adapt this approach fully, one needs to demonstrate that a) that these techniques can produce results with high fidelity and reproducibility, b) generate engineering stress-strain data that one can utilize to understand bulk behavior, and c) generate new insight into relevant phenomena fostering the true understanding of radiation damage and microstructure in materials for nuclear applications. It is the objective of this proposal to bridge the length scale between macro- and micro- scale mechanical testing of unirradiated and irradiated materials. This involves the development and demonstration of procedures for multi-scale mechanical testing that enable high fidelity reproducibility of data and the generation bulk property data from small-scale mechanical tests. Through this, the proposal aims to enhance the confidence in the obtained data at the smaller length scales and enhance the insight provided from these techniques for bulk scale applications on both unirradiated and irradiated materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Detecting Thermally-Induced Spinodal Decomposition with Picosecond Ultrasonics in Cast Austenitic Stainless Steels

Destructive techniques to monitor nuclear reactor component health may not always be available during service, as they are time-consuming and often require pre-installed inspection coupons. Non-destructive evaluation (NDE) techniques can bridge this gap by rapidly identifying the state of mission-critical reactor components, via inference between NDE-measurable material properties and those of ultimate interest, such as ductility and toughness. Here, we demonstrate one such inference about the health of thermally aged cast austenitic stainless steels. Observations of surface acoustic wave peak (SAW) splitting correlate with spinodal decomposition-induced embrittlement as destructively measured by Charpy impact energy. Elastodynamic calculations and molecular dynamics simulations of the effects of spinodal decomposition on elastic moduli support that the new acoustic modes present are due to stiffening in the δ-ferrite domains. Finally, this discovery enables one to probe structure-property relationships in materials in a greatly accelerated manner, suggesting that similar inference methods can be used to determine material fitness-for-service, or to quickly uncover new structure-property relationships.

304-type stainless steel↗

Effect of thermal oxidation on helium implanted 316L stainless steel

The effect of thermal oxide layer on He implanted 316L stainless steel was studied to evaluate experimentally how thermal oxidation affects the diffusion and distribution of He in the material. In the case of thermal oxidation of a He implanted sample, with an increase in oxidation time, the max swelling height increases logarithmically as a function of time and finally saturates for all samples except for the lowest dose of implanted He. Concerning TEM results, two void regions are identified. Similar to the calculation, the total irradiated depth was around 250 nm and the large void region was formed around 100–150 nm depth. On the other hand, the small void region was observed immediately under oxide layer from the thermal oxidation. In contrast, there were no voids in the altered zone near the metal/oxide interface in the non-thermal oxidized/He implanted sample. This description of the phenomena was justified using the Kirkendall effect and the Point Defect Model.

36 MATERIALS SCIENCE↗

Detection of voids in hydrogen embrittled iron using transmission X-ray microscopy

Hydrogen embrittlement remains a barrier to widespread adoption of hydrogen as a carbon-neutral energy source. Here, hydrogen embrittlement mechanisms are investigated across length scales in iron using transmission X-ray microscopy (TXM), digital image correlation (DIC), and notched tensile testing during in-situ electrochemical hydrogen charging. TXM reveals void size and spatial distribution ahead of a propagating crack. We find hydrogen charging leads to voids within ~10 μm of the crack tip and suppression of voids beyond this distance. Near the crack tip, voids are elongated in the direction of the crack and are smaller than voids in an uncharged sample. In the presence of hydrogen, these voids lead to quasi-cleavage fracture and a sharper crack tip. DIC shows localization and reduction of plastic strain with hydrogen charging, and tensile testing reveals a reduction in fracture energy and elongation at failure. Finally, these results are discussed in the context of hydrogen embrittlement mechanisms.

08 HYDROGEN↗

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The effects of high energy deuteron ion beam irradiation on the tensile behavior of HT-9

Ion beam implantations are widely performed to understand the effects of irradiation-induced displacement damage on nuclear structural materials. However, the volume of material that can be investigated is often limited by the maximum energies of accelerator facilitates, leading to a limitation in the thickness of samples whose mechanical properties can be evaluated. The Lawrence Berkeley National Laboratory’s 88-Inch Cyclotron offers a wide range of ions and energies, allowing for material ion implantations at larger scales than typical. Four HT-9 SS-J-geometry tensile specimens were polished and then irradiated with deuterons at the 88-Inch Cyclotron to doses of approximately 0.2 dpa prior to small scale tensile testing. Here, the results from this study show irradiation hardening characterized by the tensile test results and black dot irradiation defects. Additionally, a comprehensive look at low temperature irradiations of high-Cr F/M steels is presented and our results show agreement with the available data.

36 MATERIALS SCIENCE↗

Corrosion behavior of a series of combinatorial physical vapor deposition coatings on SiC in a simulated boiling water reactor environment

Here, the simulated boiling water condition corrosion properties of multilayer and combinatorial physical vapor deposition metal coatings (Zr, Cr, and/or Ti) deposited on a SiC f -SiC composite were investigated. Various compositions within the ternary system were corroded to the most suitable composition preventing underlying SiC f -SiC from further attack. Mass measurements and visual observations were conducted to identify which coatings formed protective oxides and which coatings spalled. Transmission electron microscopy was conducted to observe the microstructure of the physical vapor deposition metal layer before and after corrosion as well as identify the oxide which were forming.

36 MATERIALS SCIENCE↗

Progress Report on Mockup Irradiation Capsule Fuel Measurements at LANSCE

Irradiation tests are a key component of nuclear fuel development and identifying typical and atypical regions in the irradiated fuel volume relies on very few characterization techniques. The goal of the effort reported here is to provide complementary measurements adding to the available parameter space for post irradiation examination as well as to inform subsequent hot cell PIE examinations by identifying typical and atypical regions with respect to microstructure, tomographic data, or isotope densities. Pulsed neutrons, enabling diffraction as well as energy-resolved neutron imaging and neutron absorption resonance spectroscopy, offer unique capabilities for this purpose. Time-of-flight neutron diffraction has the potential to offer efficient, non-destructive and non-contact microstructural characterization of irradiated fuel specimen with spatial resolution of 1 mm 3 to 1 cm 3 while for energy-resolved neutron imaging (and by extension tomography) a resolution of 100 μm 3 was demonstrated. The potential results include crystallinity vs. amorphous volumes and microstructural information such as phase compositions, lattice strains (indicative of residual stresses or chemistry variations) and textures from the diffraction data as well as distances (e.g. pellet to cladding), cracks, and isotope densities of minor actinides, fission products as well as fission gas partial pressures e.g. in the plenum from energy resolved neutron imaging.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Tempering kinetics during multilayer laser additive manufacturing of a ferritic steel

Grade 91 steel forms martensite during additive manufacturing and the extent of tempering of martensite significantly affects the mechanical properties of parts. Currently, there is a lack of quantitative understanding of the tempering kinetics for Grade 91 steel, and as a result, the effects of repeated thermal cycles on properties for different processing conditions cannot be determined. Here we evaluate the tempering kinetics by determining the constant terms in the Johnson Mehl Avrami kinetic equation from the tempering data available in the literature and the thermal cycles computed using a rigorously-tested heat and fluid flow model of multi-layer additive manufacturing. The raw tempering data are cleaned using a neural network to enhance accuracy. The lower layers experience repeating cycles of heating and cooling when the upper layers are added. As a result, the hardness is reduced owing to the tempering of martensite. In contrast, martensite formed in the upper layers is not tempered to the same extent and the hardness remains high. Therefore, the hardness of the part increases with the distance from the substrate. Variations in the heat input at different laser powers and scanning speeds significantly affect the extent of tempering. Finally, since the method used here can provide a quantitative understanding of the tempering of martensite and the spatial variation in hardness, it can be used to tailor the microstructure and hardness of heat treatable printed metallic parts.

36 MATERIALS SCIENCE↗

Mechanical Property Evaluation of CuNb Composites Manufactured with High-Pressure Torsion

Copper is under consideration as the optimum material for both high heat flux applications and high pulsed magnets. One challenge is that copper has low strength which is problematic to deployment in these applications. One solution is to alloy copper with BCC elements to improve its mechanical properties. However, the limited solubility of the BCC elements in copper requires high deformation processes to be used in order to manufacture these 3D composites. Here, high energy ball milling combined with high pressure torsion was used to manufacture 3D Cu-Nb composites. After the consolidation the mechanical properties of the composites were measured using micro- and nanohardness testing at room and elevated temperature. The results indicated that after 10 turns during the high-pressure torsion consolidation, the mechanical properties of the composites were completely saturated displaying uniform properties across the manufactured disk. Performing the high pressure torsion at temperature further improved consolidation of the disk. The high temperature nanoindentation also indicated a change in the deformation mechanism between 200 and 500 ºC.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A multimodal approach to revisiting oxidation defects in Cr 2 O 3

The oxidation of chromium in air at 700 °C was investigated with a focus on point defect behavior and transport during oxide layer growth. A comprehensive set of characterization techniques targeted characteristics of chromium oxide microstructure and chemical composition analysis. TEM showed that the oxide was thicker with longer oxidation times and that, for the thicker oxides, voids formed at the metal/oxide interface. PAS revealed that the longer the oxidation time, there was an overall reduction in vacancy-type defects, though chromium monovacancies were not found in either case. EIS found that the longer oxidized material was more electrochemically stable and that, while all oxides displayed p-type character, the thicker oxide had an overall lower charge carrier density. Together, the results suggest anion oxygen interstitials and chromium vacancy cluster complexes drive transport in an oxidizing environment at this temperature, providing invaluable insight into the mechanisms that regulate corrosion.

36 MATERIALS SCIENCE↗