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At least 1,513 records · Page 84
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Through-thickness fracture behavior of neutron-irradiated nuclear graphite NBG-17 Using X-ray micro-CT

Achieving precise control over crack propagation in nuclear graphite and conducting quantitative analysis remain challenging. In this study, the through-thickness fracture behavior of pristine and neutron-irradiated (700 °C, ∼7 dpa) NBG-17 nuclear graphite was investigated using split-disc testing coupled with micro-computed tomography (micro-CT). A notably lower number of micropores was observed in the neutron-irradiated specimen. The fracture toughness of neutron-irradiated NBG-17 was measured to be 1.45 MPa√m, compared to 1.17 ± 0.05 MPa√m for the pristine specimen. In both materials, cracks were found to initiate at the filler–binder interface, and often correlated with microstructural features such as pores and thermal cracks. Crack bridging and deflections emerged as the primary toughening mechanisms in both unirradiated and irradiated NBG-17. However, compared with the pristine specimen, the cracks in the neutron-irradiated specimen were more likely to grow trans granularly, resulting in less deflected crack paths. The reduced micro-porosity and strengthened filler–binder boundaries were considered to be the cause of the observed differences in crack morphologies. In conclusion, this study provides a qualitative analysis of the fracture behavior of neutron-irradiated nuclear graphite in the absence of radiolytic oxidation.

36 - MATERIALS SCIENCE↗
DOE OSTI2026

Investigation of nonlinear mechanical behavior of two superfine-grained graphites with DIC assisted disc splitting test

Using standardized uniaxial tensile test specimens is not practical due to the limited volumes in irradiation capsules, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed to provide a convenient way for estimating tensile strength. Unlike the traditional uniaxial tensile test in ASTM C749 (International Standard Test Method for Tensile Stress–Strain of Carbon and Graphite), which uses dog-bone shaped specimens larger than 12.95 mm × 120.65 mm, the ASTM D8289 standard uses smaller discs with diameters of 6–12.7 mm. A digital image correlation (DIC) system, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 disc splitting test on IG-110 samples and compared with previous measurements from Mersen 2114 samples. Results confirmed that the DIC technique can measure the surface displacement/strain on these small (Ø6 mm × 3 mm) graphite specimens with good repeatability. However, Mersen 2114 and IG-110 samples exhibited strain discrepancies when DIC measurements were compared with analytical and finite element simulation values. The loading history and strain results also indicated different mechanical behaviors between Mersen 2114 and IG-110, particularly the nonlinear behavior of the IG-110 samples. Good agreement was observed by comparing the splitting tensile strengths of two superfine-grained grades with results from other work. The specimen size effect is discussed when comparing the splitting tensile strength with corresponding uniaxial tensile strength of these two graphite grades.

Lin, Lianshan [ORNL] (ORCID:0000000203399219)↗
DOE OSTI2021

The effect of aspect ratio on the mechanical behavior of Li metal in solid-state cells

The Li metal anode is necessary for solid-state batteries to dramatically exceed the energy density of state-of-the-art conventional Li-ion batteries. To enable the Li metal anode, the mechanical properties of Li metal under compression in a commercially relevant cell configuration must be determined. This work examines the compression creep behavior of Li metal coupled with a relevant model solid-state electrolyte (Li 6.5 La 3 Ta 0.5 Zr 1.5 O 12 ) and current collector (Ni) as a function of applied stress (1–10 MPa) and Li foil thickness (100–700 μm). At 1 MPa applied stress, the strain rate of all Li foil thicknesses under compression was almost four orders of magnitude lower than what is predicted from tensile creep tests. Steady-state creep behavior was observed for Li foil ≥350 μm at 5 MPa and ≥250 μm at 10 MPa. Conversely, sustained creep deformation was not observed for 100 and 150 μm Li foils at any applied stress. It is suggested that friction at the Li/LLZO and Li/Ni interfaces leads to the formation of hydrostatic stress that controls Li deformation at low aspect ratios. Finally, these results have implications for battery pack stack pressure requirements, particularly relating to void formation during stripping and Li metal filament penetration during plating.

25 ENERGY STORAGE↗
DOE OSTI2022

Deformation and Fracture Behaviors of Cylindrical Battery Shell During Thermal Runaway

Thermal runaway is one of the catastrophic failure modes of lithium-ion cells. During thermal runaway in cylindrical cells, sidewall shell rupture has been identified as a contributing factor for thermal runaway propagation in battery packs. Herein, the deformation and fracture behaviors of the battery shell during thermal runaway are investigated based on in-situ and ex-situ characterization as well as physics-based modeling. The deformation and fracture modes of the battery shell with/without Carbon Fiber Reinforced Polymer (CFRP) sleeves are identified. In the simulation, the strain introduced by thermal expansion of the system is considered, as well as the thermal and strain rate effects on the plastic stage. The final cell shell modeling is validated by cell thermal runaway tests. Results reveal the quantitative relation between shell deformation behaviors and the pressure and temperature distribution. Both the experiment and model demonstrate the effectiveness of adding a tight-fitting CFRP sleeve around the cell in limiting the side-wall rupture of the shell. The use of CFRP tubes introduces a novel phenomenon in the context of uneven temperature distribution. Results shed light on the mechanistic analysis of a cell side-wall rupture during thermal runaway and provide essential guidance for the next-generation safe battery design.

battery casing↗
DOE OSTI2014

Effect of p-type multi-walled carbon nanotubes for improving hydrogen storage behaviors

In this study, the hydrogen storage behaviors of p-type multi-walled carbon nanotubes (MWNTs) were investigated through the surface modification of MWNTs by immersing them in sulfuric acid (H{sub 2}SO{sub 4}) and hydrogen peroxide (H{sub 2}O{sub 2}) at various ratios. The presence of acceptor-functional groups on the p-type MWNT surfaces was confirmed by X-ray photoelectron spectroscopy. Measurement of the zeta-potential determined the surface charge transfer and dispersion of the p-type MWMTs, and the hydrogen storage capacity was evaluated at 77 K and 1 bar. From the results obtained, it was found that acceptor-functional groups were introduced onto the MWNT surfaces, and the dispersion of MWNTs could be improved depending on the acid-mixed treatment conditions. The hydrogen storage was increased by acid-mixed treatments of up to 0.36 wt% in the p-type MWNTs, compared with 0.18 wt% in the As-received MWNTs. Consequently, the hydrogen storage capacities were greatly influenced by the acceptor-functional groups of p-type MWNT surfaces, resulting in increased electron acceptor–donor interaction at the interfaces. - Graphical abstract: Hydrogen storage behaviors of the p-type MWNTs with the acid-mixed treatments are described. Display Omitted Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Anisotropic magnetic behaviors of monoclinic Li{sub 3}Fe{sub 2}(PO{sub 4}){sub 3}

Large sized α-Li{sub 3}Fe{sub 2}(PO{sub 4}){sub 3} single crystals with high quality are successfully grown by a flux method. Magnetic behaviors of the grown crystals are investigated by means of magnetic susceptibility, magnetization, and heat capacity measurements along different directions. The results confirm that α-Li{sub 3}Fe{sub 2}(PO{sub 4}){sub 3} exhibits weak ferrimagnetic behaviors at low temperature, which are in good agreement with those reported previously. However magnetic anisotropy is confirmed for the first time, suggesting that the c-axis is the likely magnetic easy axis and the a-axis is the magnetic hard one. Two anomalies are clearly observed in magnetic susceptibility along the a-axis and heat capacity data at zero field, suggesting the appearance of two successive magnetic transitions at ∼26 and ∼22 K in the system. - Graphical abstract: Magnetic anisotropy is confirmed for the first time using a single crystal sample of α-Li{sub 3}Fe{sub 2}(PO{sub 4}){sub 3} obtained by the flux method. - Highlights: • Large-sized single crystals of α-Li{sub 3}Fe{sub 2}(PO{sub 4}){sub 3} are grown by the flux method. • Magnetic anisotropy is confirmed for the first time in the system. • Two successive magnetic transitions are observed along the a-axis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

High-temperature behavior of dicesium molybdate Cs{sub 2}MoO{sub 4}: Implications for fast neutron reactors

Dicesium molybdate (Cs{sub 2}MoO{sub 4})'s thermal expansion and crystal structure have been investigated herein by high temperature X ray diffraction in conjunction with Raman spectroscopy. This first crystal-chemical insight at high temperature is aimed at predicting the thermostructural and thermomechanical behavior of this oxide formed by the accumulation of Cs and Mo fission products at the periphery of nuclear fuel rods in sodium-cooled fast reactors. Within the temperature range of the fuel's rim, Cs{sub 2}MoO{sub 4} becomes hexagonal P6{sub 3}/mmc, with disordered MoO{sub 4} tetrahedra and 2D distribution of Cs–O bonds that makes thermal axial expansion both large (50≤α{sub l}≤70 10{sup −6} °C{sup −1}, 500–800 °C) and highly anisotropic (α{sub c}−α{sub a}=67×10{sup −6} °C{sup −1}, hexagonal form). The difference with the fuel's expansion coefficient is of potential concern with respect to the cohesion of the Cs{sub 2}MoO{sub 4} surface film and the possible release of cesium radionuclides in accidental situations. - Graphical abstract: The weakness of the Cs–O bonds and the disordering of the MoO{sub 4} tetrahedra array in the high-temperature form are responsible for the huge thermal expansion of Cs{sub 2}MoO{sub 4} along the c-axis. - Highlights: • Thermomechanical behavior of Cs{sub 2}MoO{sub 4} fission products compound is studied. • High-temperature form of Cs{sub 2}MoO{sub 4} is characterized by XRD and Raman. • Thermal expansion appears very high and anisotropic. • Cohesion between Cs{sub 2}MoO{sub 4} and nuclear fuel seems questionable, and Cs release is expected.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Ag{sub 1.75}InSb{sub 5.75}Se{sub 11}: A new noncentrosymmetric compound with congruent-melting behavior

A new type of quaternary selenide Ag{sub 1.75}InSb{sub 5.75}Se{sub 11} has been synthesized. It crystallizes in the non-centrosymmetric space group Cm of monoclinic system, with a=13.419 (1) Å, b=4.084 (1) Å, and c=19.165 (2) Å, Z=2. The compound has a new three-dimensional layer structure which consists of infinite {sup 2}{sub ∞}[AgSb{sub 2}Se{sub 4}] layers and {sup 2}{sub ∞}[Ag1(Sb6)Ag3InSb{sub 3}Se{sub 8}] layers. The band gap of Ag{sub 1.75}InSb{sub 5.75}Se{sub 11} is 0.94(2) eV, which agrees with its dark gray color. Moreover, the compound exhibits congruent-melting behavior. - Graphical abstract: Ag{sub 1.75}InSb{sub 5.75}Se{sub 11} has a new three-dimensional layer structure which consists of infinite {sup 2}{sub ∞}[AgSb{sub 2}Se{sub 4}] layers and {sup 2}{sub ∞}[Ag1(Sb6)Ag3InSb{sub 3}Se{sub 8}] layers. - Highlights: • The new quaternary selenide Ag{sub 1.75}InSb{sub 5.75}Se{sub 11} has been synthesized. • It crystallizes in non-centrosymmetric space group Cm and has a new layer structure. • The structure consists of {sup 2}{sub ∞}[AgSb{sub 2}Se{sub 4}] layers and {sup 2}{sub ∞}[Ag1(Sb6)Ag3InSb{sub 3}Se{sub 8}] layers. • The band gap of Ag{sub 1.75}InSb{sub 5.75}Se{sub 11} is 0.94(2) eV. • The compound exhibits congruent-melting behavior.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Redox-active porous coordination polymer based on trinuclear pivalate: Temperature-dependent crystal rearrangement and redox-behavior

Linking of trinuclear pivalate Fe{sub 2}NiO(Piv){sub 6} (Piv=O{sub 2}CC(CH{sub 3}){sub 3}) by 2,6-bis(4-pyridyl)-4-(1-naphthyl)pyridine (L) resulted in formation of 1D-porous coordination polymer Fe{sub 2}NiO(Piv){sub 6}(L)·Solv, which was characterized in two forms: DMSO solvate Fe{sub 2}NiO(Piv){sub 6}(L)(DMSO)·2.5DMSO (1) or water solvate Fe{sub 2}NiO(Piv){sub 6}(L)(H{sub 2}O) (2). X-ray structure of 1 was determined. Crystal lattice of 1 at 160 K contained open channels, filled by captured solvent, while temperature growth to 296 K led to the crystal lattice rearrangement and formation of closed voids. Redox-behavior of 2 was studied by cyclic voltammetry for a solid compound, deposited on glassy-carbon electrode. Redox-activity of L preserved upon incorporation in the coordination polymer. The presence of pores in desolvated sample Fe{sub 2}NiO(Piv){sub 6}(L) was confirmed by the measurements of N{sub 2} and H{sub 2} adsorption at 77 K. Potential barriers of the different molecules diffusion through pores were estimated by the means of molecular mechanics. - Graphical abstract: Redox-behavior of 1D-porous coordination polymer Fe{sub 2}NiO(Piv){sub 6}(L)(H{sub 2}O) was studied by cyclic voltammetry in thin film, deposited on glassy-carbon electrode. Redox-activity of L preserved upon incorporation in the coordination polymer. Potential barriers of different molecules diffusion through pores were estimated by the means of molecular mechanics. - Highlights: • Porous 1D coordination polymer was synthesized. • Temperature growth led to pores closing due to crystal lattice rearrangement. • Redox-activity of ligand preserved upon incorporation into coordination polymer. • Redox-properties of solid coordination polymer were studied in thin film. • Diffusion barriers were evaluated by molecular mechanics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

High magnetic field induced spin flip/flop behavior and magnetic phase diagram of CuFe{sub 1−x}Ga{sub x}O{sub 2}

The structure and magnetic properties of non-magnetic Ga{sup 3+} ion doped CuFe{sub 1−x}Ga{sub x}O{sub 2} (x=0, 0.03, and 0.05) single crystal samples were investigated. X-ray diffraction patterns analysis confirms that the samples are single-phase crystallizing. Doping effect on the magnetic behavior of the ground state and the field-induced spin flip/flop transitions were detected. The transition temperatures and critical magnetic fields of the spin flip/flop, as well as the magnetic hysteresis directly depend on the Ga{sup 3+} doping level. Such doping effects may associate with the competition between dilution effect (partial release of spin frustration) and the induced local magnetic moment, which is the result of the changed magnetic coupling both inter- and intra-planes of Fe ions. Based on the experimental results, the effects of Ga{sup 3+} doping on the spin flip/flop behavior and a detailed high field magnetic diagram were assumed. - Graphical abstract: Temperature dependence of the critical fields for CuFe{sub 1−x}Ga{sub x}O{sub 2} (x=0, 0.03, 0.05). (a) and (b) The magnetic field's parallel and perpendicular cases respectively. In which, the square, circle and triangular represent x=0, 0.03 and 0.05 respectively. - Highlights: • Single crystal samples of CuFe{sub 1−x}Ga{sub x}O{sub 2} (x=0, 0.03 and 0.05) were grown. • Magnetic field dependence of magnetization was measured in pulsed high magnetic field up to 54 T with different temperatures. • The magnetic field induced multi-step-like transitions were observed in all the single crystal samples. • A detailed magnetic diagram was assumed based on the experimental results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Dissociation behavior of protons incorporated in yttrium doped barium zirconate

The dissociation behavior of protons incorporated in yttrium-doped barium zirconate (BZY20) was investigated via combination of in-situ diffuse reflectance Fourier transform infrared spectroscopy (FT-IR) and evolved gas analysis. The vicinities of dopant or host ions were considered as sites of proton dissolution. The temperature dependence of the dissociation of protons from each site was evaluated. Protons which were considered to have dissolved in the vicinity of dopant ions were easily removed and dissociated as water. On the other hand, those which dissolved in the vicinity of host ions were dissociated as hydrogen at high temperatures. Such dissociation behavior was also detected after using D{sub 2}O saturated gas for pre-treatment. These results suggest that some protons which dissolved in the perovskite oxide could dissociate as hydrogen without forming oxygen vacancies. (131words) - Graphical abstract: Different dissociation reactions of protons from yttria doped barium zirconate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Insights into the phase stability window, phase transformation behavior, and anisotropic thermal expansion of rhombohedral bismuth oxide

Rhombohedral bismuth oxide has emerged as a promising SOFC electrolyte material, particularly at low-to-intermediate temperatures. The stability window of this phase was explored using a co-doped system, using yttrium and lanthanum or aluminum, over 7.5–25 % total dopant content and 0.907–1.154 Å weighted average dopant cationic radius. The phase transformation behavior of rhombohedral-rich phase mixtures was also investigated in situ from 360 to 656 °C to assess the effects of minor impurity phases and thermal evolution pathways. Our results reveal that low-dopant, rhombohedral-rich compositions exhibit poor structural stability upon heating. Anisotropic thermal expansion behavior was observed over 450–656 °C, serving as a sensitive indicator of sequential phase changes, including the rhombohedral β2-to-β1 transition (∼450 °C), monoclinic phase formation, and delayed or incomplete formation of the cubic phase (∼ 550 °C). These multiple unfavorable phase transitions compromise the mechanical robustness required for SOFC operation. This study underscores the need for compositional tuning to balance ionic conductivity with thermal phase stability in rhombohedral Bi 2 O 3 -based systems.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Plastic deformation behaviors of Ni- and Zr-based bulk metallic glasses subjected to nanoindentation

Plastic deformation behaviors of Ni{sub 42}Ti{sub 20}Zr{sub 21.5}Al{sub 8}Cu{sub 5}Si{sub 3.5} and Zr{sub 51}Ti{sub 5}Ni{sub 10}Cu{sub 25}Al{sub 9} bulk metallic glasses at room temperature were studied by nanoindentation testing and atomic force microscopy under equivalent indentation experimental conditions. The different chemical composition of these two bulk metallic glasses produced variant tendencies for displacement serrated flow to occur during the loading process. The nanoindentation strain rate was calculated as a function of indentation displacement in order to verify the occurrence of displacement serrated flow at different loading rates. Atomic force microscopy revealed decreasing numbers of discrete shear bands around the indentation sites as loading rates increased from 0.025 to 2.5 mNs{sup −1}. Variations in plastic deformation behaviors between Ni and Zr-based glasses materials can be explained by the different metastable microstructures and thermal stabilities of the two materials. The mechanism governing plastic deformation of these metallic glasses was analyzed in terms of an established model of the shear transformation zone. - Highlights: • Plastic deformation of Ni- and Zr-based BMG is studied under identical conditions • Zr-based BMG undergoes a greater extent of plastic deformation than Ni-based BMG • Nanoindentation strain rate is studied to clarify variation in plastic deformation • Metastable microstructure, thermal stability affect BMG plastic deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Dynamic recrystallization behavior of an as-cast TiAl alloy during hot compression

High temperature compressive deformation behaviors of as-cast Ti–43Al–4Nb–1.4W–0.6B alloy were investigated at temperatures ranging from 1050 °C to 1200 °C, and strain rates from 0.001 s{sup −1} to 1 s{sup −1}. Electron back scattered diffraction technique, scanning electron microscopy and transmission electron microscopy were employed to investigate the microstructural evolutions and nucleation mechanisms of the dynamic recrystallization. The results indicated that the true stress–true strain curves show a dynamic flow softening behavior. The dependence of the peak stress on the deformation temperature and the strain rate can well be expressed by a hyperbolic-sine type equation. The activation energy decreases with increasing the strain. The size of the dynamically recrystallized β grains decreases with increasing the value of the Zener–Hollomon parameter (Z). When the flow stress reaches a steady state, the size of β grains almost remains constant with increasing the deformation strain. The continuous dynamic recrystallization plays a dominant role in the deformation. In order to characterize the evolution of dynamic recrystallization volume fraction, the dynamic recrystallization kinetics was studied by Avrami-type equation. Besides, the role of β phase and the softening mechanism during the hot deformation was also discussed in details. - Highlights: • The size of DRXed β grains decreases with increasing the value of the Z. • The CDRX plays a dominant role in the deformation. • The broken TiB{sub 2} particles can promote the nucleation of DRX.

36 MATERIALS SCIENCE↗
DOE OSTI2014

High-temperature low cycle fatigue behavior of a gray cast iron

The strain controlled low cycle fatigue properties of the studied gray cast iron for engine cylinder blocks were investigated. At the same total strain amplitude, the low cycle fatigue life of the studied material at 523 K was higher than that at 423 K. The fatigue behavior of the studied material was characterized as cyclic softening at any given total strain amplitude (0.12%–0.24%), which was attributed to fatigue crack initiation and propagation. Moreover, this material exhibited asymmetric hysteresis loops due to the presence of the graphite lamellas. Transmission electron microscopy analysis suggested that cyclic softening was also caused by the interactions of dislocations at 423 K, such as cell structure in ferrite, whereas cyclic softening was related to subgrain boundaries and dislocation climbing at 523 K. Micro-analysis of specimen fracture appearance was conducted in order to obtain the fracture characteristics and crack paths for different strain amplitudes. It showed that the higher the temperature, the rougher the crack face of the examined gray cast iron at the same total strain amplitude. Additionally, the microcracks were readily blunted during growth inside the pearlite matrix at 423 K, whereas the microcracks could easily pass through pearlite matrix along with deflection at 523 K. The results of fatigue experiments consistently showed that fatigue damage for the studied material at 423 K was lower than that at 523 K under any given total strain amplitude. - Highlights: • The low cycle fatigue behavior of the HT250 for engine cylinder blocks was investigated. • TEM investigations were conducted to explain the cyclic deformation response. • The low cycle fatigue cracks of HT250 GCI were studied by SEM. • The fatigue life of the examined material at 523 K is higher than that at 423 K.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructural evolution and the variation of tensile behavior after aging heat treatment of precipitation hardened martensitic steel

The effects of aging temperature on the microstructural evolution and the tensile behavior of precipitation hardened martensitic steel were investigated. Microscopic analysis using transmission electron microscope (TEM) was combined with the microstructural analysis using the synchrotron X-ray diffraction (XRD) to characterize the microstructural evolution with aging temperature. Peak hardness was obtained by precipitation of the Ni{sub 3}Al ordered phase. After aging at temperature range from 420 to 590 °C, spherical Ni{sub 3}Al precipitates and ellipsoidal M{sub 23}C{sub 6} carbides were observed within laths and at lath boundaries, respectively. Strain hardening behavior was analyzed with Ludwik equation. It is observed that the plastic strain regimes can be divided into two different stages by a rapid increase in strain hardening followed by a comparatively lower increase. At the first strain hardening stage, the aged specimen exhibited higher strain hardening exponent than the as-quenched specimen, and the exponent in the aged specimen was not changed considerably with increasing aging temperature. It is revealed that the strain hardening exponents at the first and the second stages were associated with the Ni{sub 3}Al precipitates and the domain size representing the coherent scattering area, respectively. - Highlights: • All of aged specimen exhibited higher strain hardening exponent than the as-quenched specimen at the first stage. • The value of strain hardening exponent in the aged specimen was nearly constant with aging temperature. • Ni{sub 3}Al precipitation dominantly influenced to the increase of strain hardening exponent at the first strain hardening stage. • Domain size was associated with strain hardening exponent at the second strain hardening stage.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Comparative study of structure formation and mechanical behavior of age-hardened Ti–Nb–Zr and Ti–Nb–Ta shape memory alloys

This work sets out to study the peculiar effects of aging treatment on the structure and mechanical behavior of cold-rolled and annealed biomedical Ti–21.8Nb–6.0Zr (TNZ) and Ti–19.7Nb–5.8Ta (TNT) (at.%) shape memory alloys by means of transmission electron microscopy, X-ray diffractometry, functional fatigue and thermomechanical testing techniques. Dissimilar effects of aging treatment on the mechanical behavior of Zr- and Ta-doped alloys are explained by the differences in the ω-phase formation rate, precipitate size, fraction and distribution, and by their effect on the alloys' critical stresses and transformation temperatures. Even short-time aging of the TNZ alloy leads to its drastic embrittlement caused by “overaging”. On the contrary, during aging of the TNT alloy, formation of finely dispersed ω-phase precipitates is gradual and controllable, which makes it possible to finely adjust the TNT alloy functional properties using precipitation hardening mechanisms. To create in this alloy nanosubgrained dislocation substructure containing highly-dispersed coherent nanosized ω-phase precipitates, the following optimum thermomechanical treatment is recommended: cold rolling (true strain 0.37), followed by post-deformation annealing (600 °C, 15–30 min) and age-hardening (300 °C, 30 min) thermal treatments. It is shown that in TNT alloy, pre-transition diffraction effects (diffuse reflections) can “mask” the β-phase substructure and morphology of secondary phases. - Highlights: • TNZ alloy is characterized by much higher ω-phase precipitation rate than TNT alloy. • Difference in precipitation rates is linked to the difference in Zr and Ta diffusion mobility. • Aging of nanosubgrained TNZ alloy worsens its properties irrespective of the aging time. • Aging time of nanosubgrained TNT alloy can be optimized to improve its properties.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of grain orientation on the incipient oxidation behavior of Haynes 230 at 900 °C

Ni-based superalloy Haynes 230 is used in many applications such as very high temperature reactor (VHTR) or solid oxide fuel cells (SOFCs) where it is exposed to high temperature service environment. In order to improve the resistance for high temperature oxidation, the effect of crystallographic orientation on the early stage oxidation was investigated. It was demonstrated that different oxide thicknesses are formed on grains having different orientations. Comparison of electron backscatter diffraction (EBSD) orientation maps before and after oxidation at 900 °C indicates that grains near (111) orientation, especially with the deviation angle from <111> that is smaller than 20°, are more oxidation resistant than grains of other orientations. Correlation between the results of electron backscatter diffraction (EBSD) and atomic force microscopy (AFM) was used to compare the oxidation rate of grains having different crystallographic orientation. The oxidation rate was found to change with the crystallographic orientation as follows (111) < (110) < (100), also it was demonstrated that the oxidation rate changes are a nearly linear function of the angle of deviation from <111> direction. The morphology of surface oxide also depends on the orientation of grains. - Highlights: • Comparison of EBSD maps before and after oxidation allows to investigate the effect of orientation on oxidation in a more direct way; • Effect of crystallographic orientation on oxidation behavior of alloy 230 is studied by combination of EBSD and AFM; • Different thickness of oxide is formed on grain with different orientation and dependence of anisotropic oxidation behavior is discussed; • The morphology of grains is also orientation dependence.

36 MATERIALS SCIENCE↗