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DOE OSTI2017

Surface nanostructuring in the carbon–silicon(100) system upon microwave plasma treatment

The study is concerned with the physical and chemical processes and the mechanisms of the effect of plasma preparation of a surface on the systematic features of condensation and surface phase transformations during the formation of Si–C mask domains on p-Si(100) crystals by the deposition of submonolayer C coatings in the microwave plasma of low-pressure ethanol vapors. It is shown that, at short durations of the deposition of carbon onto silicon wafers with a natural-oxide coating at a temperature of 100°C, the formation of domains is observed. The lateral dimensions of the domains lie in the range from 10–15 to 200 nm, and the heights of ridges produced by the plasma chemical etching of silicon through the mask domain coatings vary in the range from 40 to 80 nm.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Room temperature creep behavior of Ti–Nb–Ta–Zr–O alloy

The room temperature creep behavior and deformation mechanisms of a Ti–Nb–Ta–Zr–O alloy, which is also called “gum metal”, were investigated with the nanoindentation creep and conventional creep tests. The microstructure was observed with electron backscattered diffraction analysis (EBSD) and transmission electron microscopy (TEM). The results show that the creep stress exponent of the alloy is sensitive to cold deformation history of the alloy. The alloy which was cold swaged by 85% shows high creep resistance and the stress exponent is approximately equal to 1. Microstructural observation shows that creep process of the alloy without cold deformation is controlled by dislocation mechanism. The stress-induced α' martensitic phase transformation also occurs. The EBSD results show that the grain orientation changes after the creep tests, and thus, the creep of the cold-worked alloy is dominated by the shear deformation of giant faults without direct assistance from dislocations. - Highlights: •Nanoindentation was used to investigate room temperature creep behavior of gum metal. •The creep stress exponent of gum metal is sensitive to the cold deformation history. •The creep stress exponent of cold worked gum metal is approximately equal to 1. •The creep of the cold-worked gum metal is governed by the shear deformation of giant faults.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Elevated Temperature Solid Particle Erosion Performance of Plasma-Sprayed Co-based Composite Coatings with Additions of Al{sub 2}O{sub 3} and CeO{sub 2}

In this paper, investigation into solid particle erosion behavior of atmospheric plasma-sprayed composite coating of CoCrAlY reinforced with Al{sub 2}O{sub 3} and CeO{sub 2} oxides on Superni 76 at elevated temperature of 600 °C is presented. Alumina particles are used as erodent at two impact angles of 30° and 90°. The microstructure, porosity, hardness, toughness and adhesion properties of the as-sprayed coatings are studied. The effects of temperature and phase transformation in the coatings during erosion process are analyzed using XRD and EDS techniques. Optical profilometer is used for accurate elucidation of erosion volume loss. CoCrAlY/CeO{sub 2} coating showed better erosion resistance with a volume loss of about 50% of what was observed in case of CoCrAlY/Al{sub 2}O{sub 3}/YSZ coating. Lower erosion loss is observed at 90° as compared to 30° impact angle. The erosion mechanism evaluated using SEM micrograph revealed that the coatings experienced ductile fracture exhibiting severe deformation with unusual oxide cracks. Reinforced metal oxides provide shielding effect for erodent impact, enabling better erosion resistance. The oxidation of the coating due to high-temperature exposure reforms erosion process into oxidation-modified erosion process.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Assessment of firing conditions in old fired-clay bricks: The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Shock and Detonation Physics at Los Alamos National Laboratory

WX-9 serves the Laboratory and the Nation by delivering quality technical results, serving customers that include the Nuclear Weapons Program (DOE/NNSA), the Department of Defense, the Department of Homeland Security and other government agencies. The scientific expertise of the group encompasses equations-of-state, shock compression science, phase transformations, detonation physics including explosives initiation, detonation propagation, and reaction rates, spectroscopic methods and velocimetry, and detonation and equation-of-state theory. We are also internationally-recognized in ultra-fast laser shock methods and associated diagnostics, and are active in the area of ultra-sensitive explosives detection. The facility capital enabling the group to fulfill its missions include a number of laser systems, both for laser-driven shocks, and spectroscopic analysis, high pressure gas-driven guns and powder guns for high velocity plate impact experiments, explosively-driven techniques, static high pressure devices including diamond anvil cells and dilatometers coupled with spectroscopic probes, and machine shops and target fabrication facilities.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructural evolution and hardness response in the laser beam welded joints of pure titanium during recrystallization and grain growth

Highlights: • The LABs and high local misorientations indicate the existence of plastic strains in the as-welded HAZ and FZ. • During heat treatment the recrystallization occurs in the HAZs, decreasing plastic strains, but it doesn't appear in the FZs. • The coarse and unstrained grains gradually replace the fine and strained ones in the HAZs during recrystallization. • The decrease of plastic strains in the HAZs during recrystallization causes the descent of average hardness values based on the strain strengthening. - Abstract: Microstructural evolution and hardness response in the laser beam welded joints of pure titanium during recrystallization and grain growth were investigated by means of electron backscatter diffraction and hardness measurement. The low-angle boundaries (LABs) and high local misorientations, in the as-welded heat affected zone (HAZ) and fusion zone (FZ), indicate the existence of plastic strains caused by the plastic strains due to the thermal stress and the non-equilibrium phase transformations. The recrystallization occurs in the HAZs during heat treatment, but the grain growth after recrystallization does not appear under the heat treatment conditions. Moreover as a result of the slightly high impurity contents in the as-welded FZ, no distinct recrystallization is found in the FZs in this work. During recrystallization in the HAZs, the coarse and unstrained grains with equiaxed shape and smooth boundary gradually consume the fine and strained ones with irregular shape and serrate boundary. Meanwhile, the LABs disappear and the low local misorientations replace the high ones in the modified grains. The recrystallization during heat treatment causes the decrease of plastic strains in the HAZs, which reflects on the descent of average hardness values based on the strain strengthening.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Dynamics of the gold–silicon eutectic reaction studied at limited length scales using in situ $\mathrm{TEM}$ and $\mathrm{STEM}$

We report the dynamics of the gold–silicon eutectic reaction in limited dimensions were studied using in situ transmission electron microscopy and scanning transmission electron microscopy heating experiments. The phase transformation, viewed in both plan-view and cross-section of the film, occurs through a complex combination of dislocation and grain boundary motion and diffusion of silicon along gold grain boundaries, which results in a dramatic change in the microstructure of the film. The conversion observed in cross-section shows that the eutectic mixture forms at the Au–Si interface and proceeds into the Au film at a discontinuous growth rate. This complex process can lead to a variety of microstructures depending on sample geometry, heating temperature, and the ratio of gold to silicon which was found to have the largest impact on the eutectic microstructure. The eutectic morphology varied from dendrites to hollow rectangular structures to Au–Si eutectic agglomerates with increasing silicon to gold ratio.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Tribological Performance of Austempered and Tempered Ductile Iron

Austempered ductile iron with its unique ausferritic structure is produced by an isothermal heat treatment process. Austempered ductile iron is a potential material to substitute for traditional steel castings and forgings in current industry due to its excellent mechanical properties. The tempering process is frequently used to enhance the ductility and toughness of a material and reduce residual stress. In this research, the phase transformation of austempered ductile iron was studied by applying various tempering temperatures with constant holding duration. It was found that the ausferritic structure was decomposed into dispersive cementite particles after receiving a tempering temperature of 538 °C or higher. The specific amount of retained austenite was analyzed by X-ray diffraction. The wear resistance of tempered austempered ductile iron was investigated by using a ball-on-disk sliding test configuration. The results were compared with conventional quenched and tempered ductile iron under equivalent hardness. Both austempered ductile iron and tempered austempered ductile iron samples had better wear resistance than quenched and tempered ductile iron. The results presented in this research can be utilized as a reference in the tempering treatment of austempered ductile iron material for future applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Unveiling Swift Heavy Ion Track Morphology in Sr-Based High-Entropy Perovskites

The incorporation of multiple cations on a single lattice site in the high-entropy oxides is considered the key driving factor for modifying the known atomic-level response to energetic ion irradiation due to the presence of structural disorder; however, these effects are not well-understood yet. In this work, we present atomic-level insight into irradiation-induced nanoscale phase transformations in a perovskite-structured high-entropy oxide, Sr(Zr 0.2 Sn 0.2 Ti 0.2 Hf 0.2 Nb 0.2 )O 3 (Sr(HE)O 3 ), subjected to 774 MeV swift Xe heavy ions, where damage is dominated by inelastic ion−lattice interactions. While these ions generally are known to create nanoscale disordered channels, “ion tracks”, along the penetration direction in the material, this study shows the formation of discontinuous and partially recrystallized ion tracks in Sr(HE)O 3 . Compared to SrTiO 3 irradiated under identical energy loss conditions, the ion tracks in Sr(HE)O 3 exhibit significantly reduced diameters and a markedly different interfacial structure. Notably, the crystalline−amorphous interface in Sr(HE)O 3 shows minimal lattice distortion, confined to approximately 2−3 monolayers, in contrast to the extended disordered shell commonly observed in SrTiO 3 . Using in situ atomic-resolution electron microscopy, we further demonstrate that the amorphous/disordered regions within Sr(HE)O 3 ion tracks remain highly stable under electron irradiation, whereas tracks in SrTiO 3 readily recrystallize. This enhanced stability is attributed to the dominance of structural and chemical complexity arising from multiple B-site cations, which suppress defect migration and templated recrystallization driven by electronic excitations and local heating. Overall, this study highlights how high-entropy oxide chemistry fundamentally reshapes irradiation damage evolution, offering insights into defect formation and phase stability under extreme conditions.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructure and Mechanical Properties of Friction Stir Welded Q235 Low-Carbon Steel

Three-millimeter-thick Q235 steel plates were friction stir welded using a tool made of tungsten-rhenium alloy in the present study. The microstructure and mechanical properties of welded joints at various traverse speeds from 50 to 150 mm/min were analyzed. It was demonstrated that traverse speed had great impacts on microstructure and mechanical properties of the joints. Phase transformation accompanied with recrystallization occurred during FSW process which resulted in different microstructures in the WNZ, and the grain size in other zones was significantly affected by traverse speed. The highest hardness was located in the nugget zone, while the lowest hardness was found in the heat-affected zone. The transverse tensile test suggested that all the joints showed slightly lower tensile strength than that of the base material, and the tensile strength increased with increasing traverse speed. All the joints fractured in the heat-affected zone with ductile fracture mode. The impact test showed that the impact toughness decreased with the increasing traverse speed and the impact fracture surface could be divided into shear lip zone and fibrous zone which showed a typical ductile fracture.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Reactive Ballistic Deposition of Nanostructured Model Materials for Electrochemical Energy Conversion and Storage

Finely structured, supported thin films offer a host of opportunities for fundamental and applied research. Nanostructured materials often exhibit physical properties which differ from their bulk counterparts due to the increased importance of the surface in determining the thermodynamics and behavior of the system. Thus, control of the characteristic size, porosity, morphology, and surface area presents opportunities to tailor new materials which are useful platforms for elucidating the fundamental processes related to energy conversion and storage. The ability to produce high purity materials with direct control of relevant film parameters such as porosity, film thickness, and film morphology is of immediate interest in the fields of electrochemistry, photocatalysis, and thermal catalysis. Studies of various photoactive materials have introduced questions concerning the effects of film architecture and surface structure on the performance of the materials, while recent work has demonstrated that nanostructured, mesoporous, or disordered materials often deform plastically, making them robust in applications where volumetric expansion and phase transformations occur, such as in materials for lithium-ion batteries. Moreover, renewed emphasis has been placed on the formation of semi-conductive electrodes with controlled pore-size and large surface areas for the study and application of pseudo-capacitance and cation insertion processes for electrical energy storage. Understanding how the performance of such materials depends on morphology, porosity, and surface structure and area requires a synthesis technique which provides for incremental variations in structure and facilitates assessment of the performance with the appropriate analytical tools, preferably those that provide both structural information and kinetic insight into photoelectrochemical processes.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2017

Heat-Treated TiO{sub 2} Plasma Spray Deposition for Bioactivity Improvement in Ti-6Al-4V Alloy

In the present study, titanium di-oxide (TiO{sub 2}) coating has been developed on Ti-6Al-4V substrate by plasma spray deposition. Followed by plasma spraying, heat treatment of the sprayed sample has been carried out by isothermally holding it at 823 K (550 °C) for 2 h. Microstructural analysis shows the presence of porosity and unmelted particles on the as-sprayed surface, the area fraction of which reduces after heat treatment. X-ray diffraction analysis shows the phase transformation from anatase (in precursor powder) to rutile (in as-sprayed coating and the same after heat treatment). There is an improvement in nano-hardness, “Young’s modulus” and wear resistance in plasma-sprayed TiO{sub 2} coating (as-sprayed as well as post-heat-treated condition) as compared to as-received Ti-6Al-4V, though post-heat treatment offers a superior hardness, “young’s modulus” and wear resistance as compared to as-sprayed coating. The corrosion behavior in “hank’s solution” shows decrease in corrosion resistance after plasma spraying and post-heat treatment as compared to as-received substrate. A significant decrease in contact angle and improvement in bioactivity (in terms of apatite deposition) were observed in TiO{sub 2}-coated surface as compared to as-received Ti-6Al-4V.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Size-dependent radiation damage mechanisms in nanowires and nanoporous structures

Nanostructures with a high density of interfaces, such as in nanoporous materials and nanowires, resist radiation damage by promoting the annihilation and migration of defects. This study details the size effect and origins of the radiation damage mechanisms in nanowires and nanoporous structures in model face-centered (gold) and body-centered (niobium) cubic nanostructures using accelerated multi-cascade atomistic simulations and in-situ ion irradiation experiments. Our results reveal three different size-dependent mechanisms of damage accumulation in irradiated nanowires and nanoporous structures: sputtering for very small nanowires and ligaments, the formation and accumulation of point defects and dislocation loops in larger nanowires, and a face-centered-cubic to hexagonal-close-packed phase transformation for a narrow range of wire diameters in the case of gold nanowires. Smaller nanowires and ligaments have a net effect of lowering the radiation damage as compared to larger wires that can be traced back to the fact that smaller nanowires transition from a rapid accumulation of defects to a saturation and annihilation mechanism at a lower dose than larger nanowires. These irradiation damage mechanisms are accompanied with radiation-induced surface roughening resulting from defect-surface interactions. Comparisons between nanowires and nanoporous structures show that the various mechanisms seen in nanowires provide adequate bounds for the defect accumulation mechanisms in nanoporous structures with the difference attributed to the role of nodes connecting ligaments in nanoporous structures. Altogether, our results shed light on the compounded, size-dependent mechanisms leading to the radiation resistance of nanowires and nanoporous structures.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Raman Study of the Structural Distortion in the Ni 1–x Co x TiO 3 Solid Solution

In this paper, Raman spectra were collected on Ni 1–x Co x TiO 3 (0 ≤ x ≤ 1) ilmenite samples as a function of the temperature between 4 and 1200 K. An evident symmetry lowering from the prototype R$\bar{3}$symmetry is observed. The distortion was largest for the x = 0.40 and 0.50 samples and significantly diminished for small and large values of x. The distortion was preserved in the whole temperature range and, except for the x = 0.50 sample, did not show significant changes. Notably, between 25 and 69 K, distortion of the x = 0.40 sample is accompanied by ferromagnetic order. The direct cation–cation and O-mediated indirect interactions are discussed as mechanisms behind the distortion and magnetic order. A reversible order–disorder phase transformation, assigned to occur between the ilmenite and corundum phases, took place at 973 K in the x = 0.50 sample. Completion of the transformation took over 1 h. Finally, the role of the overlap of Co/Ni and Ti 3d orbitals through O octahedral faces for charge transfer is discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2013

Disparate effects of an O{sub 2} internal impurity on the elongation and quantum transport of gold and silver nanowires

In this work, we investigated the effects of an internal O{sub 2} impurity on the conductance of elongated gold and silver nanowires (NWs) using density functional theory calculations. We found that the O{sub 2} interacts with these metallic NWs very differently. In the case of gold NWs, the presence of an internal oxygen molecule locally strengthens the wire, therefore, forcing the phase transformations connected to the thinning process (3D to 2D and 2D to single atom chain) to occur far from the oxygen. As a consequence, towards the end of the elongation, the internal O{sub 2} is located far from the main conductance channel and therefore has little influence on the conductance of the NW. In contrast, in silver NWs, the presence of an internal oxygen molecule involves a larger charge transfer from the metallic atoms to the oxygen, therefore, weakening the Ag-Ag binding. During the initial stages of the elongation, several metallic bonds adjacent to the impurity break, so that in most simulations the NW thinning takes place near the O{sub 2}. This thinning mechanism places the O{sub 2} near the main conductance channel, therefore, significantly reducing the conductivity of the elongated silver NWs. For both metals, our findings agree well with the published experimental results.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2014

Pressure-induced amorphization in orthorhombic Ta{sub 2}O{sub 5}: An intrinsic character of crystal

The phase transition of orthorhombic Ta{sub 2}O{sub 5} was investigated by in situ synchrotron X-ray diffraction and Raman spectroscopy. The orthorhombic phase transforms into an amorphous form completely at 24.7 GPa. A bulk modulus B{sub 0} = 139 (9) GPa for the orthorhombic Ta{sub 2}O{sub 5} is derived from the P-V data. We suggest that the pressure-induced amorphization (PIA) in Ta{sub 2}O{sub 5} can be attributed to the unstability of the a axis under high pressure leads to the connections of polyhedral breaking down and even triggers disorder of the whole crystal frame. These results demonstrate that the PIA is an intrinsic character of Ta{sub 2}O{sub 5} which depends on its orthorhombic crystal structure rather than nanosize effects. This study provides a new kind of bulk material for investigating PIA in metal oxides.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Determining the refractive index of shocked [100] lithium fluoride to the limit of transmissibility

Lithium fluoride (LiF) is a common window material used in shock- and ramp-compression experiments because it displays a host of positive attributes in these applications. Most commonly, it is used to maintain stress at an interface and velocimetry techniques are used to record the particle velocity at that interface. In this application, LiF remains transparent to stresses up to 200 GPa. In this stress range, LiF has an elastic-plastic response with a very low (<0.5 GPa) elastic precursor and exhibits no known solid-solid phase transformations. However, because the density dependence of the refractive index of LiF does not follow the Gladstone-Dale relation, the measured particle velocity at this interface is not the true particle velocity and must be corrected. For that reason, the measured velocity is often referred to as the apparent velocity in these types of experiments. In this article, we describe a series of shock-compression experiments that have been performed to determine the refractive index of LiF at the two most commonly used wavelengths (532 nm and 1550 nm) between 35 and 200 GPa to high precision. A modified form of the Gladstone-Dale relation was found to work best to fit the determined values of refractive index. In addition, we provide a direct relationship between the apparent and true particle velocity to correct experimentally obtained wave profiles by others using these velocimetry techniques.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2011

Synchrotron X-ray Study of Filled Skutterudites CeFe4Sb12 and Ce0.8Fe3CoSb12

In situ synchrotron X-ray diffraction measurements are carried out on filled skutterudites CeFe{sub 4}Sb{sub 12} and Ce{sub 0.8}Fe{sub 3}CoSb{sub 12} up to 32 and 20 GPa, respectively, at room temperature. No phase transformation was observed for both samples in the pressure range. Fitting the pressure-volume data (up to 10 GPa) to the third-order Birch-Murnaghan equation of state, the bulk modulus B{sub 0} is determined to be 74(4) GPa, with the pressure derivative B'{sub 0} = 7(2) for CeFe{sub 4}Sb{sub 12}, and B{sub 0} = 71(2) GPa and B'{sub 0} = 8(2) for Ce{sub 0.8}Fe{sub 3}CoSb{sub 12}. The bulk moduli of filled skutterudites CeFe{sub 4}Sb{sub 12} and Ce{sub 0.8}Fe{sub 3}CoSb{sub 12} in our study are smaller than those from previous studies on unfilled skutterudite CoSb{sub 3}. The P-V curves of the unfilled skutterudite CoSb{sub 3} and filled skutterudites CeyFe{sub 4-x}Co{sub x}Sb{sub 12} showed good agreement, indicating that the Ce filling fraction and the replacement of Fe with Co have little effect on their compression behaviors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗