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At least 109 records · Page 6

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residual strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. Furthe, we found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.

304L stainless steel↗

Micromechanical Behavior of Solid-Solution-Strengthened Mg-1wt.%Al Alloy Investigated by In-Situ Neutron Diffraction

In-situ neutron-diffraction experiments were employed to investigate the micromechanical behavior of solid-solution-strengthened Mg-1wt.%Al alloy. Two starting textures were used: 1) as-extruded then solutionized texture, T1, in which the basal poles of most grains are tilted around 70~85 from the extrusion axis, and 2) a reoriented texture, T2, in which the basal poles of most grains are tilted around 10~20 from the extrusion axis. Lattice strains and diffraction peak intensity variations were measured in situ during loading-unloading cycles in uniaxial tension. Twinning activities and stress states for various grain orientations were revealed. The results show that the soft grain orientations, favorably oriented for either extension twinning or basal slip, exhibit the stress relaxation, resulting in the compressive residual strain after unloading. On the other hand, the hard grain orientations, unfavorably oriented for both extension twinning and basal slip, carry more applied load, leading to much higher lattice strains during loading followed by tensile residual strains upon unloading.

Lee, Sooyeol↗

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗

Magnetic phase diagram of (Mo 2/3 RE 1/3 ) 2 AlC, RE = Tb and Dy, studied by magnetization, specific heat, and neutron diffraction analysis

We report the results of magnetization, heat capacity, and neutron diffraction measurements on (Mo 2/3 RE 1/3 ) 2 AlC with RE = Dy and Tb. Temperature and field-dependent magnetization as well as heat capacity were measured on a powder sample and on a single crystal allowing the construction of the magnetic field-temperature phase diagram. To study the magnetic structure of each magnetic phase, we applied neutron diffraction in a magnetic field up to 6 T. For (Mo 2/3 Dy 1/3 ) 2 AlC in zero field, a spin density wave is stabilized at 16 K, with antiferromagnetic ordering at 13 K. Furthermore, we identify the coexistence of ferromagnetic and antiferromagnetic phases induced by magnetic fields for both RE = Tb and Dy. The origin of the field induced phases is resulting from the competing ferromagnetic and antiferromagnetic interactions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Neutron diffraction studies on structural and magnetic properties of RE{sub 2}NiGe{sub 3} (RE=La, Ce)

We report the crystallographic properties of RE{sub 2}NiGe{sub 3} (RE=La, Ce) synthesized by arc melting. Rietveld refinement on the powder neutron diffraction (ND) data suggest both compounds are isostructural and crystallize in the non-centrosymmetric Er{sub 2}RhSi{sub 3} type structure having hexagonal space group P6{sup ¯}2c. In the crystal structure of RE{sub 2}NiGe{sub 3}, two dimensional arrangements of nickel and germanium atoms lead to the formation of hexagonal layers with rare earth atoms sandwiched between them. Magnetic susceptibility measurements performed in low fields exhibit antiferromagnetic ordering in cerium compound around (T{sub o}=) 3.2 K. Neutron diffraction measurements at 2.8 K (i.e., at T<T{sub o}) neither show any change in the intensities of the diffraction lines nor indicate the appearance of any new diffraction lines in the Q-range of 0.47–7.34 Å{sup −1}, thus ruling out any long-range magnetic order. - Graphical abstract: The compounds La{sub 2}NiGe{sub 3} and Ce{sub 2}NiGe{sub 3} crystallize in the Er{sub 2}RhSi{sub 3} type. Magnetic susceptibility show antiferromagnetic ordering for Ce{sub 2}NiGe{sub 3} at 3.2 K and neutron diffraction confirms the absence of long range ordering. - Highlights: RE{sub 2}NiGe{sub 3} (RE=La, Ce) crystallize in the ordered superstructure of the AlB{sub 2} type. Magnetic susceptibility measurements exhibit antiferromagnetic ordering in Ce{sub 2}NiGe{sub 3}. Structure and magnetism of RE{sub 2}NiGe{sub 3} (RE=La, Ce) are studied by neutron diffraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The ferroelectric phase of CdTiO{sub 3}: A powder neutron diffraction study

The synthesis of bulk samples of polycrystalline CdTiO{sub 3} in both the rhombohedral ilmenite and orthorhombic perovskite forms is described and the structures of these have been refined using powder neutron diffraction data. This involved the preparation of samples enriched in {sup 114}Cd. Cooling perovskite-type CdTiO{sub 3} to 4 K induces a ferroelectric phase transition, with the neutron data suggesting the low temperature structure is in Pna2{sub 1}. Mode analysis shows the polar mode to be dominant at low temperatures. The ilmenite-structure of CdTiO{sub 3} is compared with that of ZnTiO{sub 3}. The refined scattering length of the {sup 114}Cd is estimated to be 5.56 fm. Attempts to dope CdTiO{sub 3} with Ca and Sr are described. - Graphical abstract: The structure of three phases of CdTiO{sub 3} have been refined using high resolution powder neutron diffraction data. This involved the preparation of samples enriched in {sup 114}Cd. Cooling perovskite-type CdTiO{sub 3} to 4 K results in a ferroelectric phase in Pna2{sub 1}. Highlights: > Both the ilmenite and perovskite forms of CdTiO{sub 3} have been prepared using {sup 114}Cd. > Cooling the perovskite form results in a ferroelectric phase. > The structures of these are refined from powder neutron diffraction data. > Attempts to dope CdTiO{sub 3} are described.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Effect of microstructure anisotropy on the deformation of MAX polycrystals studied by in-situ compression combined with neutron diffraction

In situ compression tests combined with neutron diffraction were performed on Ti{sub 2}AlN MAX polycrystals with lamellar anisotropic microstructure: the diffraction peak evolution (position and profile) with applied stress reveals that lamellar grains parallel to compression axis remain elastic while lamellar grains perpendicular to compression plastify, both families being subjected to strong variations of heterogeneous strains (types II and III). We demonstrate that this behavior originates from the complex response of the very anisotropic lamellar microstructure and explains the observation of reversible hysteretic loops when cycling MAX polycrystals even in the elastic regime.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Ambient and High-Temperature Bulk Characterization of Additively Manufactured Ti-6Al-4V Using Neutron Diffraction

Characterization of the bulk microstructure using neutron diffraction has been applied to investigate the phase fractions and textures of α- and β-phases in Ti-6Al-4V fabricated by additive manufacturing. The microstructure of a specimen cut from a fan structure, built by either electron beam melting (EBM) or selective laser melting, indicated that predominantly the build direction and not the fan angle determines the microstructure. In situ heating experiments of specimens from a rod built using EBM provided insight into the lattice strain, phase fraction, and texture evolution, providing a rich picture of the microstructure changes during heat treatment of additively manufactured Ti-6Al-4V. Finally, a remarkably low weight fraction of β-phase at lower temperatures, deviations from thermal expansion behavior attributed to vanadium repartitioning, as well as texture strengthening were observed.

36 MATERIALS SCIENCE↗

Investigating the Difference in Mechanical Stability of Retained Austenite in Bainitic and Martensitic High-Carbon Bearing Steels using in situ Neutron Diffraction and Crystal Plasticity Modeling

In situ neutron diffraction of the uniaxial tension test was used to study the effect of the surrounding matrix microstructure on the mechanical stability of retained austenite in high-carbon bearing steels. Comparing the samples with bainitic microstructures to those with martensitic ones, it was found that the retained austenite in a bainitic matrix starts transforming into martensite at a lower strain compared to that within a martensitic matrix. On the other hand, the rate of transformation of the austenite was found to be higher within a martensitic microstructure. Crystal plasticity modeling was used to analyze the transformation phenomenon in these two microstructures and determine the effect of the surrounding microstructure on elastic, plastic, and transformation components of the strain. The results showed that the predominant difference in the deformation accumulated was from the transformation strain and the critical transformation driving force within the two microstructures. The retained austenite was more stable for identical loading conditions in case of martensitic matrix compared to the bainitic one. It was also observed that the initial volume fraction of retained austenite within the bainitic matrix would alter the onset of transformation to martensite, but not the rate of transformation.

bainite↗

Martensitic transformation in a B2-containing CuZr-based BMG composite revealed by in situ neutron diffraction

Here, CuZr-based bulk-metallic-glass (BMG) composites reinforced by a B2-type CuZr crystalline-phase (CP) have been widely studied, and exhibit that the plastic deformation of the CP induces martensitic transformation from the B2 to B19', which plays a dominant role in the deformation behavior and mechanical properties. In the present study, 2.0% Co containing CuZr-based BMG composites were investigated using in-situ neutron-diffraction technique. The in-situ neutron-diffraction results reveal the continuous load transfer from the glass matrix to B2 CP and martensitic transformation from the B2 CP to B19' during the deformation of the composite. Moreover, it was found that the martensitic transformation is initiated at the applied stress higher than 1500 MPa, and is significantly suppressed during the deformation, as compared to other 0.5% Co-containing CuZr-based BMG composites. Based on these in-situ neutron-diffraction results, the martensitic transformation is strongly affected by the amount of the addition of Co, which determines the mechanical properties of CP-reinforced BMG composites, such as ductility and hardening capability.

36 MATERIALS SCIENCE↗

In-situ neutron diffraction characterization of temperature dependence deformation in α-uranium

In-situ strain neutron diffraction measurements were conducted at temperature on specimens coming from a clock-rolled α-uranium plate, and Elasto-Plastic Self-Consistent (EPSC) modeling was employed to interpret the findings. The modeling revealed that the active slip systems exhibit a thermally activated response, while deformation twinning remains athermal over the temperature ranges explored (25-150 °C). The modeling also allowed assessment of the effects of thermal residual stresses on the mechanical response during compression. These results are consistent with those from a prior study of room-temperature deformation, indicating that the thermal residual stresses strongly influence the internal strain evolution of grain families, as monitored with neutron diffraction, even though accounting for these residual stresses has little effect on the macroscopic flow curve, except in the elasto-plastic transition.

36 MATERIALS SCIENCE↗

Structure and Thermal Expansion of YSZ and La 2 Zr 2 O 7 Above 1500°C from Neutron Diffraction on Levitated Samples

High-temperature time-of-flight neutron diffraction experiments were performed in this paper on cubic yttria-stabilized zirconia (YSZ, 10 mol% YO 1.5 ) and lanthanum zirconate (LZ) prepared by laser melting. Three spheroids of each composition were aerodynamically levitated and rotated in argon flow and heated with a CO 2 laser. Unit cell, positional and atomic displacement parameters were obtained by Rietveld analysis. Below ~1650°C the mean thermal expansion coefficient (TEC) for YSZ is higher than for LZ (13 ± 1 vs. 10.3 ± 0.6) × 10 -6 /K. From ~1650°C to the onset of melting of LZ at ~2250°C, TEC for YSZ and LZ are similar and within (7 ± 2) × 10 -6 /K. LZ retains the pyrochlore structure up to the melting temperature with Zr coordination becoming closer to perfectly octahedral. Congruently melting LZ is La deficient. The occurrence of thermal disordering of oxygen sublattice (Bredig transition) in defect fluorite structure was deduced from the rise in YSZ TEC to ~25 × 10 -6 /K at 2350°C–2550°C with oxygen displacement parameters (U iso ) reaching 0.1 Å 2 , similar to behavior observed in UO 2 . Acquisition of powder-like high-temperature neutron diffraction data from solid-levitated samples is feasible and possible improvements are outlined. Finally, this methodology should be applicable to a wide range of materials for high-temperature applications.

36 MATERIALS SCIENCE↗

The incommensurately modulated structures of low-temperature labradorite feldspars: a single-crystal X-ray and neutron diffraction study

Labradorite feldspars of the plagioclase solid solution series have been known for their complicated subsolidus phase relations and enigmatic incommensurately modulated structures. Characterized by the irrationally indexed e -reflections in the diffraction pattern, e -labradorite shows the largest variation in the incommensurate ordering states among the e -plagioclase structures. The strongly ordered low-temperature e -labradorite is one of the last missing pieces of the e -plagioclase puzzle. Nine plutonic and metamorphic labradorite feldspar samples from Canada, Ukraine, Minnesota (USA), Tanzania and Greenland with compositions ranging from An 52.5 to An 68 were studied with single-crystal X-ray diffraction. Two crystals from Labrador, Canada, and Duluth, MN, USA, with wide enough twin lamellae were analyzed with single-crystal neutron diffraction. The incommensurately modulated structures of e -plagioclase are refined for the first time with neutron diffraction data, which confirmed that the T—O distance modulation in the low-temperature e -plagioclase results from the Al–Si ordering in the framework. Detailed configurations of the M site are also observed in the structures refined from neutron diffraction data, which were not possible to see with X-ray diffraction data. The relation between the q -vectors and the mole% An composition is revealed for the entire compositional range of e -plagioclase, from An 25 to An 75 . The previously proposed two-trend relation depending on the cooling rate and phase transition path is confirmed. A new classification of e -plagioclase ( e α , e β and e γ ) is proposed based on the q -vector of the structure, which makes it an independent character from the presence/absence of density modulation. New parameters are proposed to quantify the ordering states of these complicated aperiodic structures of e -plagioclases, such as the difference between $\langle$T 1 o—O$\rangle$ and $\langle$T 1 m—O$\rangle$ at phase t = 0.2 or the normalized intensity of the (071\bar 1) reflection.

36 MATERIALS SCIENCE↗

Neutron Diffraction Analysis of Residual Strain in High-Pressure Die Cast A383 Engine Blocks

The residual strains in three high-pressure die cast A383 engine blocks were measured using neutron diffraction. Residual strains and stresses can be generated during high-pressure die casting process due to high thermal gradients and may cause fatigue failure or dimensional distortion. Neutron diffraction can measure the residual strain distributions deep inside castings with complex geometries, because neutrons can penetrate substantially more material than x-rays. In this paper, the residual strains (in the axial and hoop directions) along the whole cylinder bridge of high-pressure die cast A383 engine blocks in as-cast and heat-treated conditions were measured by neutron diffraction methods. The effect of heat treatment on the distribution and magnitude of residual strains was also investigated. The results indicate that the residual strain in the cylinder bridge is tensile in both the axial and hoop components for both the as-cast and the heat-treated engine blocks. The residual strain in the hoop direction is bigger in magnitude than the residual strain in the axial direction. Heat treatment significantly relaxes the residual strain in the axial direction but only slightly relaxes the residual strain in the hoop direction.

36 MATERIALS SCIENCE↗

Neutron diffraction and electrical transport studies on the incommensurate magnetic phase transition in holmium at high pressures

Neutron diffraction and electrical transport measurements have been made on the heavy rare earth metal holmium at high pressures and low temperatures in order to elucidate its transition from a paramagnetic (PM) to a helical antiferromagnetic (AFM) ordered phase as a function of pressure. The electrical resistance measurements show a change in the resistance slope as the temperature is lowered through the antiferromagnetic Neel temperature. The temperature of this antiferromagnetic transition decreases from approximately 122 K at ambient pressure at a rate of -4.9 K GPa(-1) up to a pressure of 9 GPa, whereupon the PM-to-AFM transition vanishes for higher pressures. Neutron diffraction measurements as a function of pressure at 89 and 110 K confirm the incommensurate nature of the phase transition associated with the antiferromagnetic ordering of the magnetic moments in a helical arrangement and that the ordering occurs at similar pressures as determined from the resistance results for these temperatures.

High Pressure↗

Simulation driven adaptive sampling for neutron-diffraction based strain mapping of additively manufactured parts

Neutron diffraction based strain mapping is a useful technique for measuring residual strains in additively manufactured (AM) metal parts. The measurement is traditionally done by scanning the sample in a point-wise raster pattern to extract the strain at each position. Since the overall scan can span several hours, adaptive sampling approaches using Bayesian optimization based on Gaussian process (BO-GP) regression have been introduced—demonstrating that even with a fraction of the typically made measurements the dominant strain patterns in the sample can be reconstructed. However, the parameters of the BO-GP algorithm have to be carefully chosen for best performance, and the movement time between arbitrary points can offset the time savings from a reduced number of measurement locations. In this paper, we propose algorithms to refine the BO-GP based methods by using simulations of strain patterns in AM parts based on the materials and the process used to print them. We demonstrate that the simulated strain patterns can be used to help choose better parameters for the BO-GP based framework—leading to low reconstruction error for the final strain pattern. Furthermore, we show that the strain mapping experiment can be initialized with a sampling pattern learnt from the simulation data and ordered to reduce movement time, dramatically enabling reduction in the overall time required to run the baseline BO-GP method.

Gaussian process regression↗

A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell has also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured.

Vadlamani, Bhaskar S↗