In this work we aim to study the effect of temperature on the mechanical properties of a solid. For this, we have introduced a new first-principles based methodology to obtain the thermal variation of the elastic constants of NiTiSn, a multifunctional Heusler compound. In parallel using X-ray diffraction, we have measured the isothermal bulk modulus at 300~K. The agreement between the calculations and the experiments is within the experimental error bars showing the accuracy of the calculations. Using two other numerical methods, which give all coherent results, we have shown that NiTiSn conserves its very good mechanical properties up to 1500~K. In particular at 700~K (the best working temperature for thermoelectric applications), NiTiSn remains a ductile and robust material making it a compound of choice for applications in which large temperature fluctuations are present.
We coupled first principles calculations and the quasiharmonic approximation combined with experiments (X-Ray diffraction and dilatometry measurements) to determine the thermal properties of NiTiSn (half-Heusler) and Ni2TiSn (Heusler) compounds. These properties are important especially if they are to be used in thermoelectric applications. First, the calculation of their mode Gruneisen parameter shows that it is positive throughout the first Brillouin zone. This suggests that these compounds undergo a regular thermal expansion. Then, the calculation of the Ni2TiSn thermal expansion shows an e…
First principles calculations of the vibrational, thermodynamic and mechanical properties of the Ni-Ti-Sn Heusler and half-Heusler compounds have been performed. First, we have calculated the Raman and infrared spectra of NiTiSn, providing benchmark theoretical data directly useful for the assignments of its experimental spectra and clarifying the debate reported in the literature on the assignment of its modes. Then, we have discussed the significant vibrational density-of-states of Ni2TiSn at low-frequencies. These states are at the origin of (i) its smaller free energy, (ii) its higher entr…
Coherent x-ray micro-diffraction and local mechanical loading can be combined to investigate the mechanical deformation in crystalline nanostructures. Here we present measurements of plastic deformation in a copper crystal of sub-micron size obtained by loading the sample with an Atomic Force Microscopy tip. The appearance of sharp features in the diffraction pattern, while conserving its global shape, is attributed to crystal defects induced by the tip.
This work integrates in-situ neutron diffraction and crystal plasticity finite element modeling to study the kinematic stability of retained austenite in high carbon bearing steels. The presence of a kinematically metastable retained austenite in bearing steels can significantly affect the macro-mechanical and micro-mechanical material response. Mechanical characterization of metastable austenite is a critical component in accurately capturing the micro-mechanical behavior under typical application loads. Traditional mechanical characterization techniques are unable to discretely quantify the …
High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c $δ$-hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the $α$-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 \si{\degreeCelsius}. The f.c.c $δ$ was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in…
The ultrafast thermal and mechanical dynamics of a two-dimensional lattice of metallic nano-disks has been studied by near infrared pump-probe diffraction measurements, over a temporal range spanning from 100 fs to several nanoseconds. The experiments demonstrate that, in these systems, a two-dimensional surface acoustic wave (2DSAW), with a wavevector given by the reciprocal periodicity of the array, can be excited by ~120 fs Ti:sapphire laser pulses. In order to clarify the interaction between the nanodisks and the substrate, numerical calculations of the elastic eigenmodes and simulations o…
The high-pressure behaviour of PbS was investigated by angular dispersive X-ray powder diffraction up to pressures of 6.8 GPa. Experiments were accompanied by first principles calculations at the density functional theory level. By combining both methods reliable data for the elastic properties of rock-salt type alpha- and high-pressure beta-PbS could be obtained. beta-PbS could be determined to crystallise in the CrB-type (B33), with space group Cmcm. The reversible ferro-elastic alpha/beta transition is of first order. It is accompanied by a large volume discontinuity of about 5% and a coexi…
Understanding mechanical properties of materials requires not only complete determination of the three-dimensional response at a local scale, but also knowledge of the mode or the mechanism by which deformation takes place. Probing mechanical response at such a depth can be only achieved through a diffraction based method. In spite of this, diffraction based methods still are not commonly employed for strain measurements because they are perceived as very time intensive and non-intuitive. Herein we introduce the concept of a diffraction strain ellipsoid, and show how its shape, thickness, and …
This work describes a methodology for producing high quality metallic surfaces from uranium primarily for characterisation and investigations involving electron backscatter diffraction. Electrochemical measurements have been conducted to inform ideal polishing conditions to produce surfaces free from strain, induced by mechanical polishing. A commonly used solution for the electropolishing of uranium, consisting in part of phosphoric acid, was used to conduct the electrochemical experiments and polishing. X-ray diffraction techniques focusing on the surface show low stresses and strains are ex…
Zirconium alloys are used in the nuclear industry as structural materials, and can be subject to high strain rate loading conditions during forming and in the case of a reactor accident. In this context, the relationship between strain rate dependent mechanical properties, crystallographic texture and deformation modes, such as slip and deformation twinning, are explored in this work. Commercially pure zirconium is deformed to 10 % engineering strain under quasi-static and high strain rate loading, and post-mortem analysis of the samples is performed using electron backscatter diffraction (EBS…
We demonstrate that highly-ordered two-dimensional crystals of ligand-capped gold nanoparticles display a local photo-mechanical stiffness as high as that of solids such as graphite. In out-of equilibrium electron diffraction experiments, a strong temperature jump is induced in a thin film with a femtosecond laser pulse. The initial electronic excitation transfers energy to the underlying structural degrees of freedom, with a rate generally proportional to the stiffness of the material. With femtosecond small-angle electron diffraction, we observe the temporal evolution of the diffraction feat…
Microstructural features and mechanical properties of an Al-Mg-Si alloy processed by high-pressure torsion have been investigated using transmission electron microscopy, X-ray diffraction, three-dimensional atom probe, tensile tests and microhardness measurements. It is shown that HPT processing of the Al-Mg-Si alloy leads to a much stronger grain size refinement than of pure aluminium (down to 100 nm). Moreover, massive segregation of alloying elements along grain boundaries is observed. This nanostructure exhibits a yield stress even two times higher than that after a standard T6 heat treatm…
The purpose of the present article is to make a model using analytical equations, based on elasticity theory of continuous media for small deformations, with the aim of completely characterizing the material in their mechanical properties as well as the principal stresses-strains of thin films. The approach differs from the standard literature which usually brings crystal symmetries or is directly concerned with crystalline materials. It is entirely possible to define and to analyze anisotropy in elastic media from first principles in thin films. Therefore, the constitutive relation between st…
Atom probe tomography (APT), electron probe microanalysis (EPMA) and nanoindentation were used to characterise the oxygen-rich layer on an in-service jet engine compressor disc, manufactured from the titanium alloy TIMETAL 834. Oxygen ingress was quantified and related to changes in mechanical properties through nanoindentation studies. The relationship between oxygen concentration, microstructure, crystal orientation and hardness has been explored through correlative hardness mapping, EPMA and electron backscatter diffraction (EBSD). The role of microstructure on oxygen ingress has been studi…
An amorphous Se$_{0.80}$S$_{0.20}$ alloy produced by Mechanical Alloying was studied by Raman spectroscopy, x-ray diffraction, extended x-ray absorption fine structure (EXAFS) and optical absorption spectroscopy, and also through reverse Monte Carlo simulations of its total structure factor and EXAFS data. Its vibrational modes, optical gap and structural properties as average interatomic distances and average coordination numbers were determined and compared to those found for an amorphous Se$_{0.90}$S$_{0.10}$ alloy. The results indicate that coordination numbers, interatomic distances and a…
Numerous different crystal structures of Ta2O5 are reported in literature. Although experimentally and computationally obtained lattice parameters and mechanical properties are in excellent agreement there is a pronounced deviation when it comes to electronic structures of Ta2O5. Based on ab initio studies and nano-beam X-ray diffraction of sputtered Ta2O5 thin films, we introduce an orthorhombic basic structure with a = 0.6425, b = 0.3769, and c = 0.7706 nm, which is stabilized by flipping of an oxygen atom in neighboring c-planes. The calculated energy of formation is with -3.209 eV/atom alm…
The aging of a nanocrystalline equiatomic ZnSe alloy produced by mechanical alloying was investigated using X-ray diffraction (XRD) and differential scanning calorimetry (DSC) techniques. The measured XRD patterns showed that Se atoms located at interfacial component migrated with aging giving raise to a crystalline selenium (c-Se) phase. DSC spectra of heat-treated samples at temperatures above 221oC followed by quenching showed that the c-Se particles changed to the amorphous state. It was also observed that the as-milled and aged samples are highly hydrophilic. The lattice parameters and th…
Zircaloy-4 is used as a fuel cladding material for water reactors, as it has good mechanical properties, corrosion resistance, and a low thermal neutron absorption cross section. However, the mechanical performance of Zircaloy-4 can be reduced during service due to hydrogen uptake and hydride formation. These hydrides are brittle, and often reduce the strength and toughness of materials as well as increase susceptibility to delayed hydride cracking (DHC). In this work, large grain Zircaloy-4 with hydrides was prepared and then cross sectioned using cryo-ion beam polishing, using plasma focused…
Aluminum single crystals are tested using X-Ray Bragg diffraction, which may have applications in microscopy and electronics fabrication industry. Yet, their efficiency for x- ray beam diffraction depends on the accurate crystal orientation, the microstructure and imperfections. Moreover, the final sample that is formed from the as-grown crystal by cutting, grinding, polishing and chemical etching, introduces various surface defects that penetrate deep into the crystal affecting its natural structure. Defect penetration is attributed to the fact that ultra-pure aluminum single crystals are sof…
We report on the growth of Y2Ti2O7 single crystals by optical floating zone technique. X-ray diffraction and Raman spectroscopy studies confirm the structural quality of the crystal. The UV-Vis optical studies reveal that the grown crystals have a high optical transparency with an optical band gap of 3.44 eV. The hardness of Y2Ti2O7 single crystal is measured for the first time using nanoindentation. The measured hardness, indentation and bulk modulus are found to be 16.4$\pm$0.4, 321.1$\pm$6.9 and 243.3$\pm$5.2 GPa respectively, which are higher than its polycrystalline counterpart and its co…
The mechanical properties of polycrystalline metals are governed by the interaction of defects that are generated by deformation within the 3D microstructure. In materials that deform by slip, the plasticity is usually highly heterogeneous within the microstructure. Many experimental tools can be used to observe the results of slip events at the free surface of a sample; however, there are only a few methods for imaging these events in the bulk. In this article, the imaging of bulk slip events within the 3D microstructure are enabled by the combined use of X-ray diffraction contrast tomography…
A filamentary composite elaborated by cold drawing was processed by High Pressure Torsion (HPT). The nanostructure resulting from this severe plastic deformation (SPD) was investigated thanks to scanning electron microscopy, transmission electron microscopy, X-ray diffraction and 3D atom probe. Although the mutual solubility of Cu and Fe is extremely low at room temperature in equilibrium conditions, it is shown that nanoscaled Fe clusters dissolve in the Cu matrix. The non-equilibrium copper supersaturated solid solutions contain up to 20at.% Fe. The driving force of the dissolution is attrib…
In this work we report a study of the magnetic behavior of ferrimagnetic oxide CoFe2O4 treated by mechanical milling with different grinding balls. The cobalt ferrite nanoparticles were prepared using a simple hydrothermal method and annealed at 500oC. The non-milled sample presented coercivity of about 1.9 kOe, saturation magnetization of 69.5 emu/g, and a remanence ratio of 0.42. After milling, two samples attained coercivity of 4.2 and 4.1 kOe, and saturation magnetization of 67.0 and 71.4 emu/g respectively. The remanence ratio MR/MS for these samples increase to 0.49 and 0.51, respectivel…
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
The Timken Company（铁姆肯公司）；Chemical and Engineering Materials Division, Spallation Neutron Source, Oak Ridge National Laboratory（橡树岭国家实验室散裂中子源化学与材料工程部）
Equiatomic TaNbHfZr and TaNbHfZrTi high-entropy alloys (HEAs) have been investigated for their phase stability, short-range clustering (SRC) type chemical ordering, other structural phenomena and and the effects on strengthening. Ab-initio calculations have been done to determine the thermodynamic stability parameters. The as-cast structures do not contain any local chemical order, but the high-resolution transmission electron microscopy (HRTEM) studies reveal their locally distorted lattice. The local lattice distortion of the average structure in their as-cast and annealed state is quantifie…
New ternary Mg-Ni-Mn intermetallics have been successfully synthesized by High Energy Ball Milling (HEBM) and have been studied as possible materials for efficient hydrogen storage applications. The microstructures of the as-cast and milled alloys were characterized by means of X-ray Powder Diffraction (XRD) and Scanning Electron Microscopy (SEM) both prior and after the hydrogenation process, while the hydrogen storage characteristics (P-c-T) and the kinetics were measured by using a commercial and automatically controlled Sievert-type apparatus. The hydrogenation and dehydrogenation measurem…
Martensitic transformations are strain driven displacive transitions governing the mechanical and physical properties in intermetallic materials. This is the case in Ni$_2$MnGa, where the martensite transition is at the heart of the striking magnetic shape memory and magneto-caloric properties. Interestingly, the martensitic transformation is preceded by a pre-martensite phase, and the role of this precursor and its influence on the martensitic transition and properties is still a matter of debate. In this work, we report on the influence of Co doping (Ni$_{50-x}$Co$_x$Mn$_{25}$Ga$_{25}$ with …
The local atomic order of an amorphous Ga$_{50}$Se$_{50}$ alloy produced by Mechanical Alloying (MA) was studied by the Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Diffraction (XRD) techniques and by Reverse Monte Carlo (RMC) simulations of its total x-ray structure factor. The coordination numbers and interatomic distances for the first neighbors were determined by means of EXAFS analysis and RMC simulations. The RMC simulations also furnished the partial pair distribution functions $G^{\text{RMC}}_{\text{Ga-Ga}}(r)$, $G^{\text{RMC}}_{\text{Ga-Se}}(r)$ and $G^{\text{RMC}}_{\tex…
The crystalline structures of superionic high temperature copper selenides Cu$_{2-x}$Se ($0 \le x \le 0.25$) produced by Mechanical Alloying were investigated using X-ray diffraction (XRD) technique. The measured XRD patterns showed the presence of the peaks corresponding to the crystalline superionic high temperature $α$-Cu$_2$Se phase in the as-milled sample, and its structural data were determined by means of a Rietveld refinement procedure. After a heat treatment in argon at 200$^\circ$C for 90 h, this phase transforms to the superionic high temperature $α$-Cu$_{1.8}$Se phase, whose struct…
Twenty-one distinct AlxCoCrFeNi alloys were rapidly prepared by laser alloying an equiatomic CoCrFeNi substrate with Al powder to create an alloy library ranging x=0.15-1.32. Variations in crystal structure, microstructure and mechanical properties were investigated using X-ray diffraction, scanning electron microscopy, scanning transmission electron microscopy and nanoindentation. With increasing Al content, the crystal structure transitioned from a disordered FCC to a mixture of disordered BCC and ordered B2 structures. While the onset of BCC/B2 formation was consistent with previously repor…
The atomistic structure of metallic glasses is closely related to properties such as strength and ductility. Here, Ni1-xBx metallic glass nanoparticles of two different sizes are compressed under quasi-hydrostatic high-pressure conditions in order to understand structural changes under stress. The structural changes in the nanoparticles were tracked using in situ high-pressure X-ray diffraction (XRD). The ambient pressure pair-distribution functions generated from XRD showed that the smaller sized nanoparticles had a more compact amorphous structure with lower coordination number. XRD showed t…
Textured alumina ceramics were obtained by Spark Plasma Sintering (SPS) of undoped commercial a-Al2O3 powders. Various parameters (density, grain growth, grain size distribution) of the alumina ceramics, sintered at two typical temperatures 1400°C and 1700°C, are investigated. Quantitative textural and structural analysis, carried out using a combination of Electron Back Scattering Diffraction (EBSD) and X-ray diffraction (XRD), are represented in the form of mapping, and pole figures. The mechanical properties of these textured alumina ceramics include high elastic modulus and hardness value …
Understanding the creep mechanisms and deformation response at different stresses and temperatures is crucial for design using nickel-base superalloys for high-temperature applications. In this study, the creep behaviour of a newly designed superalloy (nominated Alloy 11) at different stress and temperature was systematically investigated using SEM, STEM, EBSD and synchrotron X-ray diffraction. Material properties and mechanical response were analysed by considering such properties as lattice parameters and misfit, phase volume fraction, microstrain in reference and crept samples. Detwinning a…
Combining Synchrotron X-ray Diffraction, Mechanistic Modeling, and Machine Learning for In Situ Subsurface Temperature Quantification during Laser Melting
This study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defe…
New boron-rich sulfide B6S and selenide B6Se have been discovered from high pressure - high temperature synthesis combined with ab initio evolutionary crystal structure prediction, and studied by synchrotron X-ray diffraction and Raman spectroscopy at ambient conditions. As it follows from Rietveld refinement of powder X-ray diffraction data, both chalcogenides have orthorhombic symmetry and belongs to Pmna space group. All experimentally observed Raman bands have been attributed to the theoretically calculated phonon modes, and the mode assignment has been performed. Prediction of mechanical …
Alpha-Fe2O3 and alpha-Cr2O3 has been mechanical alloyed to prepare Fe1-xCrxO3 oxides for x = 0.2-0.8. Synchrotron X-ray diffraction and Raman spectra have shown inhomogeneous structure of α-Fe2O3 and α-Cr2O3 phases in as-alloyed samples. The as-alloyed samples have shown soft ferromagnetic properties with signature of two Morin transitions. The heat treatment of as-alloyed samples has homogenized structure and successfully incorporated the Cr atoms into the lattice sites of Fe atoms in α-Fe2O3. The magnetic and electrical properties have been modified in the heat treated samples. For example, …
Ultra-low density polymers, metals, and ceramic nanofoams are valued for their high strength-to-weight ratio, high surface area and insulating properties ascribed to their structural geometry. We obtain the labrynthine internal structure of a tantalum oxide nanofoam by X-ray diffractive imaging. Finite element analysis from the structure reveals mechanical properties consistent with bulk samples and with a diffusion limited cluster aggregation model, while excess mass on the nodes discounts the dangling fragments hypothesis of percolation theory.
A series on nanocrystalline Fe100-xCrx alloys prepared by mechanical alloying was investigated with X-ray diffraction (XRD), scanning electron microscopy (SEM) and Mössbauer spectroscopy (MS) techniques. XRD and SEM were used to structurally characterize the samples whereas MS permitted phase analysis as well as determination of the Debye temperature, Theta_D. Concerning the latter, an enhancement relative to bulk Theta_D-values was revealed in the range of ca. 40 < x <50. In a sample of Fe55.5Cr44.5 two phases were detected viz. (1) crystalline and magnetic with Theta_D=572(56) K and (2) amor…
Multiphase titanium alloys are critical materials in high value engineering components, for instance in aero engines. Microstructural complexity is exploited through interface engineering during mechanical processing to realise significant improvements in fatigue and fracture resistance and strength. In this work, we explore the role of select interfaces using in-situ micromechanical testing with concurrent observations from high angular resolution electron backscatter diffraction (HR-EBSD). Our results are supported with post mortem transmission electron microscopy (TEM). Using micro-pillar c…
Equiatomic TaNbHfZr refractory high-entropy alloys (HEAs) were synthesized by arc-melting. The HEAs were annealed at 1800°C for different times, at maximum up to 8 days. Their on average body-centered cubic (bcc), solid-solution structure was confirmed by X-ray (XRD) and neutron (ND) diffraction, respectively. The HEAs are characterized by high average values of the static atomic displacements from the ideal lattice positions and the local internal strain. The short-range clustering (SRC) of a subset of atoms, enriched in Hf and Zr takes place perpendicular to the <1 0 0> directions. Furthermo…
On the thermal and mechanical properties of Mg$_{0.2}$Co$_{0.2}$Ni$_{0.2}$Cu$_{0.2}$Zn$_{0.2}$O across the high-entropy to entropy-stabilized transition
James Madison University（詹姆斯麦迪逊大学）；University of Virginia（弗吉尼亚大学）；Colorado School of Mines（科罗拉多矿业学院）；Laser Thermal Incorporated（激光热力学公司）；The Pennsylvania State University（宾夕法尼亚州立大学）
The High Nitrogen Martensitic Stainless Steel (HNMS) was subjected to three different austenitizing cycles of 1050$^\circ$C, 1075$^\circ$C and 1100$^\circ$C followed by subzero treatment at -70$^\circ$C. The fraction of retained austenite has been reduced after sub-zero treatment as revealed by microstructural evolution. The material was subsequently tempered at different temperatures ranging from 180$^\circ$C to 650$^\circ$C and the change in micro-structure, hardness, tensile strength and toughness were investigated after each heat treatment cycle. Optical microscopy, electron microscopy wit…
The tendency for nitrogen deficiency in cubic Cr-Mo-N and Cr-W-N solid solutions is predicted by a comprehensive evaluation of the lattice spacing, mixing thermodynamics, and elastic properties using first-principles calculations and experimentally confirmed by means of X-ray diffraction. A major conclusion is that these systems exhibit significant amount of N vacancies whose amount scales linearly with the TM content, hence making the Cr1-xTMxN1-0.5x chemical formula more precise and informative to describe the chemical composition of cubic Cr-Mo-N and Cr-W-N solid solutions as compared with …
Hafnium orthosilicate (HfSiO4: hafnon) has been proposed as an environmental barrier coating (EBC) material to protect silicon coated, silicon-based ceramic materials at high temperatures and as a candidate dielectric material in microelectronic devices. It can naturally form at the interface between silicon dioxide (SiO2) and hafnia (HfO2). When used in these applications, its coefficient of thermal expansion (CTE) should match that of silicon and SiC composites to reduce the stored elastic strain energy, and thus risk of failure of these systems. The physical, mechanical, thermodynamic and t…
Achieving a combination of high mechanical strength and high electrical conductivity in low-weight Al alloys requires a full understanding of the relationships between nanoscaled features and physical properties. Grain boundary strengthening through grain size reduction offers some interesting possibilities but is limited by thermal stability issues. Zener pinning by stable nanoscaled particles or grain boundary segregation are well-known strategies for stabilizing grain boundaries. In this study, the Al-Ca system has been selected to investigate the way segregation affects the combination of …
Despite the large number of experiments demonstrating that grains in a metallic material can grow at room temperature due to applied mechanical load, the mechanisms and the driving forces responsible for mechanically induced grain coarsening are still not understood. Here we present a systematic study of room temperature grain coarsening induced by cyclic strain in thin polymer-supported gold films. By means of detailed electron backscatter diffraction analysis we were able to capture both the growth of individual grains and the evolution of the whole microstructure on the basis of statistical…
The (Cd, Be)Te semiconductor alloy that exhibits a dramatic mismatch in bond covalency and stiffness clarifying its vibrational and mechanical properties is used as a benchmark to test the limits of the percolation model (PM) worked out to explain the complex Raman spectra of the related but less contrasted (Zn, Be) chalcogenides. The test is done by way of experiment (x smaller than 0.11) combining Raman scattering with X ray diffraction at high pressure and ab initio calculations (x around 0, 0.5 and 1). The (macroscopic) bulk modulus B drops below the CdTe value on minor Be incorporation, a…
We have investigated the structural, mechanical and electronic properties of D-carbon by ab initio calculations, a new phase of crystalline sp3 carbon (pace group D2h5, Pmma-orthorhombic). Total-energy calculations demonstrate that D-carbon is energetically more favorable than previously proposed T6 structure. State-of-the-art theoretical calculations show that this new phase is dynamic, mechanical, and thermal stable at zero pressure, and more stable than graphite beyond 63.7 GPa. Importantly, the calculations reveal that D-carbon possesses high Vickers hardness (86.58 GPa) and bulk modulus (…
