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DOE OSTI2017

Relating microstructure, temperature, and chemistry to explosive ignition and shock sensitivity

An analysis is put forth that relates explosive properties including microstructure, temperature, and chemistry to explosive ignition and sensitivity. Unlike approaches that focus only on elucidating mesoscopic mechanisms important to ignition, the present analysis seeks a methodology directly applicable to continuum explosive burn models. Because the Scaled Uniform Reactive Front (SURF) burn model has a microstructural basis, it is chosen as the starting point of the present analysis. To build upon the SURF framework, a literal translation is performed of the high-level conceptual notions for which SURF is based, to concrete ignition–combustion parameters, a statistical description of the microstructure, and other thermo-chemical data acquired by non-shock experiments. The analysis requires a void volume fraction distribution acquired from ultra-small angle neutron scattering (USANS). The shock response of PBX 9502 is used to illustrate the theory. While the analysis requires calibration to a shock experiment (the pop plot, for example), the results are a self-consistent set of realistic physical quantities that contribute to the shock initiation process including, initial temperature, chemical kinetics, a statistical description of the microstructure, and the hot spot size, spacing, and temperature. The utility of having a mesoscale based theory is that once the critical hot spot temperature, as a function of shock pressure, is known for a given explosive and initial porosity distribution, the entire set of meso- and macro-scale results, including the pop plot can be calculated for any other porosity. Thus, one can understand changes in sensitivity at different densities (void size distributions), relying only on the assumption that the hot spot temperature curve would not differ significantly if the morphology of the hots spots were similar. Another important utility of the present analysis is to address the question of the role of initial temperature on the observed shock sensitivity of PBX 9502 and other explosives.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Boundary characterization using 3D mapping of geometrically necessary dislocations in AM Ta microstructure

Additive manufacturing (AM) of high strength metallic materials produces microstructures and defects that deviate substantially from those created through conventional manufacturing methods. It has recently been demonstrated that with application of extreme energy densities, a high-temperature refractory metal, tantalum (Ta), can be printed to a fully dense state with exceptionally low porosity. Here we employ a combination of three-dimensional electron backscattered diffraction (EBSD) TriBeam technology and crystallographic geometrically necessary dislocation (GND) theory to characterize the microstructure and defect boundaries of this unusual AM product. Two-dimensional (2D) EBSD and these three-dimensional (3D) measurements indicate that the microstructure of AM Ta is highly oriented <111> along the build direction, yet at the same time contains large crystallographic orientation gradients that span mm’s across the build. Crystallographic GND density analysis of the 3D microstructure reveals that highly misoriented subboundaries exist within this strongly textured microstructure that have large dislocation densities of 1×10 16 m –2 , just as large as those comprising the high-angle grain boundaries (HAGBs) in the same material. The 3D crystallographic GND density mapping reveals these subboundaries are part of a complex, finely spaced network that extends throughout the entire microstructure. Here, the orientation of these boundaries can be related to the scan strategy used during printing. TEM measurements corroborate an extremely high dislocation density at the microscale and indicate a cell-like dislocation network structure existing in the AM Ta at the sub-μm scale.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of Different Thermomechanical Processes on the Microstructure, Texture, and Mechanical Properties of API 5L X70 Steel

A commercial API 5L X70 steel plate was subjected to different thermomechanical processes to propose a novel thermomechanical rolling path to achieve improved mechanical properties. Scanning electron microscopy, electron backscatter diffraction, and x-ray texture analysis were employed for microstructural characterization. The results showed that strain-free recrystallized {001} ferrite grains that developed at higher rolling temperature could not meet the American Petroleum Institute (API) requirements. Also, refined and work-hardened grains that have formed in the intercritical region with high stored energy do not provide suitable tensile properties. However, fine martensite–austenite constituents dispersed in ferrite matrix with grains having predominantly {111} and {110} orientations parallel to the normal direction that developed under isothermal rolling at 850 °C provided an outstanding combination of tensile strength and ductility.

36 MATERIALS SCIENCE↗

NASA NTRS2017

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Ceramics↗

DOE OSTI2015

3D RoboMET Characterization

The goal of this project is to generate 3D microstructural data by destructive and non-destructive means and provide accompanying characterization and quantitative analysis of such data. This work is a continuing part of a larger effort to relate material performance variability to microstructural variability. That larger effort is called “Predicting Performance Margins” or PPM. In conjunction with that overarching initiative, the RoboMET.3D™ is a specific asset of Center 1800 and is an automated serialsectioning system for destructive analysis of microstructure, which is called upon to provide direct customer support to 1800 and non-1800 customers. To that end, data collection, 3d reconstruction and analysis of typical and atypical microstructures have been pursued for the purposes of qualitative and quantitative characterization with a goal toward linking microstructural defects and/or microstructural features with mechanical response. Material systems examined in FY15 include precipitation hardened 17-4 steel, laser-welds of 304L stainless steel, thermal spray coatings of 304L and geological samples of sandstone.

Madison, Jonathan D.↗

DOE OSTI2021

X-ray computed tomography-based porosity analysis: Algorithms and application for porous woody biomass

The properties of lignocellulosic biomass, such as bulk physical, thermal, and mechanical properties, as well as the mobility of enzymes or catalysts, are largely affected by porosity, pore structures, and pore size distribution. While X-ray computed tomography (CT) has been introduced to effectively produce 3D volumetric images of material microstructure, a quantitative porosity analysis from the 3D images has never been done. This work introduces a first-of-its-kind X-ray CT-based quantitative porosity analysis method and applies the developed toolkit to characterize the internal porosity distribution of loblolly pine. A sample loblolly pine chip was scanned by a nano-resolution X-ray CT system and digitally reconstructed after a sequence of image processing operations. Here, a comprehensive porosity analysis was then performed to quantify the envelope porosity, the spatial distribution of local porosity, and the directional porosity. Solutions to the various challenges in image processing, porosity calculation, and large data handling are provided.

42 ENGINEERING↗

DOE OSTI2022

Investigation of deformation mechanisms in an advanced FeCrAl alloy using in-situ SEM-EBSD testing

The deformation mechanisms associated with uniaxial tensile testing are observed by conducting tensile experiments of an FeCrAl alloy using scanning electron microscopy (SEM) coupled with electron backscattered diffraction (EBSD). Prior to the deformation, investigated alloy was consisting grain and precipitate size of ~63.0 μm and ~6.7 μm, respectively. The recorded SEM micrographs and EBSD data at increasing levels of strains revealed the complex phenomena of slip bands’ formation in the presence of surface grain morphology evolution and their (001), (110) and (111) crystallographic planes distortions. The grains with orientation (110)||tensile direction (TD) shows higher shape change; however, (001)||TD and (111)||TD oriented grains show higher lattice gradient formation. Extracted information from the EBSD indicates that the crystallographic rotations drive towards specific, fiber-like texture in relation to the loading direction. Postmortem analysis of the recorded microstructure during the tensile deformation explains the phenomena of crack formation in the hard-intermetallic particles before the ultimate tensile strength (UTS). However, after the UTS, pores were identified in the neck that resulted from extensive plastic deformation. In-depth analysis was carried out to identify the cause of cracks and pores formation phenomena during the tensile test.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Carbon Support Microstructure Impact on High Current Density Transport Resistances in PEMFC Cathode

Cell voltages at high current densities (HCD) of an operating proton-exchange membrane fuel cell (PEMFC) cathode suffer from losses due to the local-O 2 and bulk-H + transport resistances in the catalyst layer. Particularly, the microstructure of high surface area carbon (HSC) support upon which both the platinum catalyst and ionomer are dispersed play a pivotal role in controlling the reactant transport to the active site in the catalyst layer. In this study, we perform a systematic analysis of the underlying microstructure of platinum-cobalt catalyst dispersed on various HSC supports in terms of their surface area and pore-size distribution. The carbon microstructure was found to strongly influence the PtCo nanoparticle dispersion, catalyst layer ionomer distribution and transport losses governing the performance at HCD. Catalyst layer electrochemical diagnostics carried out to quantify local-O 2 transport resistance and bulk-H + transport resistance in the cathode were found to be directly correlated to the micropore (<2 nm) and macropore (>8 nm) surface areas of the carbon support, respectively. Finally, a 1D-performance model has been developed to assimilate our understanding of the catalyst layer microstructure and transport resistances at HCD.

25 ENERGY STORAGE↗

DOE OSTI2026

Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials

Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.

TEM sample preparation↗

DOE OSTI2025

Hydrogen influences thermal activation parameters for dislocation glide during low cycle fatigue of 316L stainless steel

Measurements of activation areas are used to investigate the effect of hydrogen on the kinetics of dislocation glide during cyclic deformation in cold-worked 316L stainless steel. Non-charged and hydrogen-precharged (H-precharged) specimens were tested in low cycle fatigue (LCF) under plastic strain control. A series of plastic strain rate changes was performed periodically at the peak true plastic strain from the first cycle to half-life, and at various plastic strain values around stable hysteresis loops near half-life to determine the operational activation area, Δ a ∗. Both material conditions demonstrate a rapid increase in Δ a ∗ during the initial rapid softening followed by a region of approximately constant values coinciding with a reduced rate of softening. Near half-life, hydrogen reduces Δ a ∗ at a given true stress due to its effect on the activation distance and obstacle spacing. The magnitudes of Δ a ∗ reveal that bypassing solutes, cutting forest dislocations, and initiating cross slip are important mechanisms of thermally activated dislocation glide at all amplitudes, except hydrogen suppresses cross slip at the lowest plastic strain amplitudes. These results are supported by electron microscopy characterization of deformed microstructures. A Haasen plot analysis indicates that forest dislocations control the kinetics of deformation in both material conditions. It also reveals the presence of athermal obstacles in both non-charged and H-precharged conditions, likely dense dislocation tangles and cell walls. Additionally, the effect of hydrogen on microstructure evolution (by reducing the propensity for cross slip) leads to a dependence of athermal stress on plastic strain amplitude.

Activation area↗

DOE OSTI2014

Fabrication of a Mo based high temperature TZM alloy by non-consumable arc melting technique

High temperature structural materials are in great demand for power, chemical and nuclear industries which can perform beyond 1000 °C as super alloys usually fail. In this regard, Mo based TZM alloy is capable of retaining strength up to 1500 °C with excellent corrosion compatibility against molten alkali metals. Hence, currently this alloy is considered an important candidate material for high temperature compact nuclear and fusion reactors. Due to reactive nature of Mo and having high melting point, manufacturing this alloy by conventional process is unsuitable. Powder metallurgy technique has limited success due to restriction in quantity and purity. This paper deals with fabrication of TZM alloy by nonconsumable tungsten arc melting technique. Initially a ternary master alloy of Mo-Ti-Zr was prepared which subsequently by dilution method, was converted into TZM alloy gradually by external addition of Mo and C in various proportions. A number of melting trials were conducted to optimize the process parameters like current, voltage and time to achieve desired alloy composition. The alloy was characterized with respect to composition, elemental distribution profile, microstructure, hardness profile and phase analysis. Well consolidated alloy button was obtained having desired composition, negligible material loss and having microstructure as comparable to standard TZM alloy. (author)

36 MATERIALS SCIENCE↗

DOE OSTI2016

3D analysis of macrosegregation in twin-roll cast AA3003 alloy

Twin-roll cast aluminium alloys have a high potential for industrial applications. However, one of the drawbacks of such materials is an inhomogeneous structure generated by macrosegregation, which appears under certain conditions in the center of sheets during solidification. Segregations in AA3003 alloy form as manganese, iron and silicon rich channels spread in the rolling direction. Their spatial distribution was successfully detected by X-ray computed tomography. Scanning electron microscopy was used for a detailed observation of microstructure, morphology and chemical analysis of the segregation. - Highlights: •Macrosegregations in twin-roll cast sheets stretch along the rolling direction. •X-ray computed tomography is an effective tool for visualization of the segregation. •The segregations copy the shape of grain boundaries.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Creep and microstructural processes in a low-alloy 2.25%Cr1.6%W steel (ASTM Grade 23)

A low-alloy 2.25%Cr1%Mo steel (ASTM Grade 22) has been greatly improved by the substitution of almost all of the 1%Mo by 1.6%W. The improved material has been standardized as P/T23 steel (Fe–2.25Cr–1.6W–0.25V–0.05Nb–0.07C). The present investigation was conducted on T23 steel in an effort to obtain a more complete description and understanding of the role of the microstructural evolution and deformation processes in high-temperature creep. Constant load tensile creep tests were carried out in an argon atmosphere in the temperature range 500–650 °C at stresses ranging from 50 to 400 MPa. It was found that the diffusion in the matrix lattice is the creep-rate controlling process. The results of an extensive transmission electron microscopy (TEM) analysis programme to investigate microstructure evolution as a function of temperature are described and compared with the thermodynamic calculations using the software package Thermo-Calc. The significant creep-strength drop of T23 steel after long-term creep exposures can be explained by the decrease in dislocation hardening, precipitation hardening and solid solution hardening due to the instability of the microstructure at high temperature. - Highlights: • The constant load creep tests of T23 steel were carried out at 500–650 °C. • The stress exponents of the creep rate correspond to power law (dislocation) creep. • Diffusion in the matrix lattice is the creep-rate controlling process. • The microstructure instability is the main creep degradation process in T23 steel.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Processing eutectics in space

Experimental work is reported which was directed toward obtaining interface shape control while a numerical thermal analysis program was being made operational. An experimental system was developed in which the solid-liquid interface in a directionally solidified aluminum-nickel eutectic could be made either concave to the melt or convex to the melt. This experimental system provides control over the solid-liquid interface shape and can be used to study the effect of such control on the microstructure. The SINDA thermal analysis program, obtained from Marshall Space Flight Center, was used to evaluate experimental directional solidification systems for the aluminum-nickel and the aluminum-copper eutectics. This program was applied to a three-dimensional ingot, and was used to calculate the thermal profiles in axisymmetric heat flow. The results show that solid-liquid interface shape control can be attained with physically realizable thermal configurations and the magnitudes of the required thermal inputs were indicated.

Douglas, F. C.↗

NASA NTRS2000

BUNDLE: A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

Carrasquillo, Edgar J.↗

NASA NTRS2001

BUNDLE - A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

Carrasquillo, Edgar J.↗

DOE OSTI2016

Polycrystalline BiFeO{sub 3} thin film synthesized via sol-gel assisted spin coating technique for photosensitive application

We are reporting photosensitivity property of BiFeO{sub 3} thin film under optical illumination. The thin film used for photosensitivity work was fabricated via sol-gel assisted spin coating technique. I-V measurements on the Cu/BiFeO{sub 3}/Al structure under dark condition show a good rectifying property and show dramatic blue shit in threshold voltage under optical illumination. The microstructure, morphology and elemental analysis of the films were characterized by using XRD, UV-Vis, FTIR, SEM and EDS.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2012

Effect of La{sub 2}O{sub 3}, CoO, Cr{sub 2}O{sub 3} and MoO{sub 3} nucleating agents on crystallization behavior and magnetic properties of ferromagnetic glass-ceramic in the system Fe{sub 2}O{sub 3}{center_dot}CaO{center_dot}ZnO{center_dot}SiO{sub 2}

Highlights: Black-Right-Pointing-Pointer Crystallization of magnetic glass ceramic with different nucleating agents. Black-Right-Pointing-Pointer The effect of La{sub 2}O{sub 3}, CoO, Cr{sub 2}O{sub 3} and MoO{sub 3} as nucleating agents was studied. Black-Right-Pointing-Pointer XRD for as prepared samples revealed crystallization of pure magnetite. Black-Right-Pointing-Pointer Heat treatment revealed minor calcium silicate, hematite and cristobalite. Black-Right-Pointing-Pointer TEM revealed crystallization of crystallite size in the range 50-100 nm. -- Abstract: Preparation and characterization of ferromagnetic glass ceramic in the system Fe{sub 2}O{sub 3}{center_dot}CaO{center_dot}ZnO{center_dot}SiO{sub 2} with different nucleating agents was studied. The effect of La{sub 2}O{sub 3}, CoO, Cr{sub 2}O{sub 3} and MoO{sub 3} as nucleating agents was investigated. Differential thermal analysis; X-ray diffraction and transmission electron microscope were used to investigate thermal behavior, sequence of crystallization and microstructure of the samples. XRD analysis for as prepared samples revealed the crystallization of single magnetite phase. Heat treatment at 900 Degree-Sign C/2 h revealed the appearance of minor amounts of calcium silicate, hematite and cristobalite beside magnetite. TEM revealed crystallization of crystallite size in the range 50-100 nm. Lattice parameters, cell volume and crystallite size were stimulated from XRD data. Magnetic properties of quenched samples were measured under 20 kG.

36 MATERIALS SCIENCE↗