Certification of Standard Reference Material 660c for powder diffraction.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).

Certification of SRM 640f line position and line shape standard for powder diffraction.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to be used to evaluate specific aspects of the instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 640f, the seventh generation of this powder diffraction SRM, which is designed to be used primarily for calibrating powder diffractometers with respect to line position; it also can be used for the determination of the instrument profile function. It is certified with respect to the lattice parameter and consists of approximately 7.5 g of silicon powder prepared to minimize line broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the Si powder. Both statistical and systematic uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.5431144 ± 0.000008 nm.

Certification of Standard Reference Material 1879b Respirable Cristobalite.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to address specific aspects of the performance of X-ray powder diffraction instruments. This report describes SRM 1879b, the third generation of this powder diffraction SRM. SRM 1879b is intended for use in the preparation of calibration standards for the quantitative analyses of cristobalite by X-ray powder diffraction in accordance with National Institute for Occupational Safety and Health (NIOSH) Analytical Method 7500, or equivalent. A unit of SRM 1879b consists of approximately 5 g of cristobalite powder bottled in an argon atmosphere. It is certified with respect to crystalline phase purity, or amorphous phase content, and lattice parameter. Neutron powder diffraction, both time-of-flight and constant-wavelength, was used to certify the phase purity using SRM 676a as an internal standard. A NIST-built diffractometer, incorporating many advanced design features was used for certification measurements for lattice parameters.

The Lattice Spacing Variability of Intrinsic Float-Zone Silicon.

Precision lattice spacing comparison measurements at the National Institute of Standards and Technology (NIST) provide traceability of X-ray wavelength and powder diffraction standards to the international system of units (SI). Here, we both summarize and document key measurements from the last two decades on six lots of intrinsic float-zone silicon, including unpublished results and recent internal-consistency checks. The comparison measurements link the unknown lattice spacing of a test crystal to a standard crystal for which the lattice spacing has been accurately determined by X-ray/optical interferometry in units traceable to the definition of the meter. The crystal that serves as the standard in all the comparisons is WASO 04, for which the lattice spacing is known with a relative uncertainty of 5 × 10-9. Individual lattice spacing comparison results have typical uncertainties of 1 ×10-8; taking material variability into account, measurements yield relative uncertainties for the test materials of a few tens of nanometers. It is observed that in the case of nearly perfect modern intrinsic float-zone silicon, the variability of the lattice spacing is sufficiently small that for most diffraction applications, a recommended reference value may be used.

Synthesis and Characterization of the New Li1+xAl1+xSi1-xO4 (x = 0-0.25) Solid Electrolyte for Lithium-Ion Batteries.

A systematic study was performed to investigate the effect of the sintering temperature, sintering duration, and aluminum doping on the crystalline structure and ionic conductivity of the Li1+xAl1+xSi1-xO4 (LASO; x = 0-0.25) solid electrolyte. There was a strong indication that an increase in the sintering temperature and sintering time increased the ionic conductivity of the electrolyte. In particular, the doping concentration and composition ratio (Li1+xAl1+xSi1-xO4; x = 0-0.25) were found to be crucial factors for achieving high ionic conductivity. The sintering time of 18 h and lithium concentration influenced the lattice parameters of the LASO electrolyte, resulting in a significant improvement in ionic conductivity from 2.11 × 10-6 (for pristine LASO) to 1.07 × 10-5 S cm-1. An increase in the lithium concentration affected the stoichiometry, and it facilitated a smoother Li-ion transfer process since lithium served as an ion-conducting bridge between LASO grains.

Enhancement of antimicrobial properties by metals doping in nano-crystalline hydroxyapatite for efficient biomedical applications.

In this study, we have introduced a method for the synthesis of various metal-doped nano-crystalline hydroxyapatites (HAp) using a standard wet chemical precipitation technique. Both divalent (Ni and Zn) and trivalent (Al and Fe) metals were selected for the doping process. Additional research work was also conducted to assess the antimicrobial efficacy of these doped-HAps against a range of gram-positive and gram-negative microorganisms. All the synthesized metal-doped hydroxyapatite (HAp) exhibited notable antibacterial characteristics against gram-negative bacterial strains, namely Escherichia coli (E. coli) and Salmonella typhi (S. typhi), outperforming the pure HAp. The inhibition zone observed for the metal-doped HAp ranged from 14 to 16 mm. The Fe ion displayed a notable inhibitory zone measuring 16 mm, proving to be the most expansive among all tested ions against both E. coli and S. typhi bacterial strains. The Zn-HAp exhibited a comparable inhibitory zone size of 14 mm against both S. typhi and E. coli. Additional characterization methods, such as X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and Scanning electron microscopy (SEM), were used to validate the structural properties of the synthesized metal-doped hydroxyapatite (HAp) samples. The biocompatibility assessment of metal-doped hydroxyapatite (HAp) samples was carried out by haemolysis tests, which revealed that all synthesized hydroxyapatite (HAp) samples have the potential to serve as reliable biomaterials.

Effects of isotropic stress on the band structure elastic, optical, thermal, and x-ray diffraction properties of TiSnO3.

BACKGROUND: Cubic perovskite titanium stannous oxide (TiSnO3) is a promising material for various applications due to its functional properties. However, understanding how these properties change under external stress is crucial for its development and optimization. METHOD: This study employed density functional theory calculations to investigate the structural, electronic, optical, thermal, and mechanical properties of TiSnO3 under varying degrees of external static isotropic stress (0-120 GPa). RESULTS: The study reveals a significant decrease in the bandgap of TiSnO3 with increasing stress due to lattice modifications and the formation of delocalized electrons. Partial density of states analysis indicates that Sn and O states play a key role in shaping the electronic band structure. TiSnO3 exhibits increased light absorption with stress, accompanied by a blue shift in absorption peaks, whereas, both polarizability and refractive index decrease with increasing stress. Mechanically, all elastic moduli (bulk, shear, and Young's) show an increase under stress, signifying a stiffening response of the material under stress. Similarly, the Pugh ratio suggests a transition from ductile to brittle behaviour at elevated stress levels. Phonon dispersion calculations indicate the instability of the cubic phase at 0 K. However, a phonon gap emerges at 30 GPa and widens with increasing stress. X-ray diffraction further supports these findings by demonstrating a shift in diffraction peaks towards higher angles with increasing stress, consistent with the applied stress. CONCLUSION: In conclusion, this computational study offers a thorough understanding of how external stress influences the properties of TiSnO3, providing valuable insights for potential applications in various fields.

Variations in the Crystal Lattice of Tb-Dy-Fe Magnetostrictive Materials: The Lattice Constant Disturbance.

In Tb-Dy-Fe alloy systems, Tb0.29Dy0.71Fe1.95 alloy shows giant magnetostrictive properties under low magnetic fields, thus having great potential for transducers, microsensors, and other applications. The C15 cubic crystal structure of Tb-Dy-Fe has long been thought to be the source of giant magnetostriction. It is surprising that such a highly symmetrical crystal structure exhibits such a large magnetostrictive strain. In this work, the lattice parameters of Tb0.29Dy0.71Fe1.95 magnetostrictive materials were studied by processing atomic-resolution images. The selected area diffraction patterns show a face-centered cubic structure, but the fast Fourier transform diagram shows that the cubic structure has obvious distortion. The lattice parameters obtained by geometric phase analysis (GPA) and Gaussian model-based fitting and calculation show that the lattice constants a, b, and c are not strictly equal, and small disturbance of the lattice constants occurs based on the cubic structure. The actual crystal structure of the Tb-Dy-Fe material is a slightly disturbed cubic structure. This variation in the crystal lattice is mainly caused by the inhomogeneous composition and may be related to the giant magnetostrictive properties of Tb-Dy-Fe alloy.

Effect of Blade Geometry on γ' Lattice Parameter and Primary Orientation of SX Cored Turbine Blades (II).

The distributions of the lattice parameter of the γ'-phase (aγ') and angular components of the primary crystal orientation along the lines parallel to the main axis of the single-crystalline CMSX 4-cored turbine blades were studied. The studies were carried out on the regions of the blades located far from the selector and its continuer extension (CE), positioned asymmetrically relative to the blade's axis. It was found that, similarly to the regions of the blade located close to the CE (studied in part I), at the level of the blade related to the change of its cross-section, there were correlated local changes in aγ' and the angular components of the primary crystal orientation representing the bending of the dendrites. However, the correlation was less clear due to the presence of low-angle boundaries (LABs) and the intensification of the consequences of the "fanning effect" in the regions far from the CE. It was found that the range of local changes in aγ' and the angular components of the primary crystal orientation of the blade regions were influenced by both the distance from the CE and the separation of these regions from the CE by surfaces of the cooling bores. It was found that the deviation angle in the [001] direction from the blade axis increased with an increase in the distance from the CE. Based on the aγ' changes, differences in the alloying element concentration near the cooling bores were discussed.

Lattice Deformation of Tb0.29Dy0.71Fe1.95 Alloy during Magnetization.

In Tb-Dy-Fe alloy systems, Tb0.29Dy0.71Fe1.95 alloy shows giant magnetostrictive properties under low magnetic fields, thus having great potential for transducer and sensor applications. In this work, the lattice parameters of Tb0.29Dy0.71Fe1.95 compounds as a function of a magnetic field were investigated using in situ X-ray diffraction under an applied magnetic field. The results showed that the c-axis elongation of the rhombohedral unit cell was the dominant contributor to magnetostriction at a low magnetic field (0-500 Oe). As the magnetic field intensity increased from 500 Oe to 1500 Oe, although the magnetostrictive coefficient continued to increase, the lattice constant did not change, which indicated that the elongated c-axis of the rhombohedral unit cell rotated in the direction of the magnetic field. This rotation mainly contributed to the magnetostriction phenomenon at magnetic fields of above 500 Oe. The structural origin of the magnetostriction performance of these materials was attributed to the increase in rhombohedral lattice parameters and the rotation of the extension axis of the rhombohedral lattice.

Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 1. Where is the Bragg angle?

The derivation of a crystal structure and its phase-specific parameters from a single wide-angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern-forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.

Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 2. Offset corrections.

A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low-Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit-cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Z max, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset-corrected lattice parameter deviation is Δa/a < 1.5%. The lattice parameter ratios, and the angles α, ß and γ between the basis vectors, are not affected at all.

Effect of Residual Oxygen Concentration on the Lattice Parameters of Aluminum Nitride Powder Prepared via Carbothermal Reduction Nitridation Reaction.

Residual oxygen in wurtzite-type aluminum nitride (AlN) crystal, which significantly affects phonon transport and crystal growth, is crucial to thermal conductivity and the crystal quality of AlN ceramics. In this study, the effect of residual oxygen on the lattice of AlN was examined for as-synthesized and sintered samples. By controlling reaction time in the carbothermal reduction nitridation (CRN) procedure, AlN powder was successfully synthesized, and the amount of residual oxygen was systematically controlled. The evolution of lattice parameters of AlN with respect to oxygen conc. was carefully investigated via X-ray diffraction analysis. With increasing amounts of residual oxygen in the as-synthesized AlN, lattice expansion in the ab plane was induced without a significant change in the c-axis lattice parameter. The lattice expansion in the ab plane owing to the residual oxygen was also confirmed with high-resolution transmission electron microscopy, in contrast to the invariant lattice parameter of the sintered AlN phase. Micro-strain values from XRD peak broadening confirm that stress, induced by residual oxygen, expands the AlN lattice. In this work, the lattice expansion of AlN with increasing residual oxygen was elucidated via X-ray diffraction and HR-TEM, which is useful to estimate and control the lattice oxygen in AlN ceramics.

Formation Mechanism and Lattice Parameter Investigation for Copper-Substituted Cobalt Ferrites from Zingiber officinale and Elettaria cardamom Seed Extracts Using Biogenic Route.

Biogenic routes for the synthesis of nanoparticles are environmentally friendly, nontoxic, biocompatible, and cost-effective compared to traditional synthesis methods. In this study, cobalt ferrite was synthesized using Zingiber officinale and Elettaria cardamom Seed extracts. Effect of copper contents (x = 0.0, 0.3, 0.6 and 0.9) on the plant extracted Cux(Co1-xFe2O4) was investigated by XRD, SEM, EDX, UV-Vis., PL, FE-SEM, FTIR and photocatalytic activity. XRD results revealed that nanoparticles exhibit a cubical spinel structure with an average diameter of 7-45 nm, calculated by the Debye Scherer formula. The value of the lattice parameter decreased from 8.36 Å to 8.08 Å with substitution of copper, which can be attributed to mismatch of ionic radii of Cu2+ (0.73 Å) and Co2+ (0.74 Å) ions. SEM analysis showed that nanoparticles exhibit a spherical shape (~13 nm diameter) for undoped samples and low Cu concentration, while they changed to a hexagonal structure at higher Cu concentration (x = 0.9) with a diameter ~46 nm and a decreased degree of agglomeration. FE-SEM further confirmed the nanoparticles' size and shape. EDX analysis confirmed the presence of cobalt, iron, and oxygen without contamination. The optical absorption spectra of UV-vis and PL showed red-shift, which can be accredited to larger crystalline sizes of nanoparticles. FTIR spectra showed two main bands at 410 and 605 cm-1, indicating the presence of intrinsic vibrations of the octahedral and tetrahedral complexes, respectively. The photocatalytic activity of Co0.4Cu0.6 Fe2O4 nanoparticles was investigated using methylene blue (MB) and methyl orange (MO) dyes under visible light irradiation. The degradation rate (93.39% and 83.15%), regression correlation coefficient (0.9868 and 0.9737) and rate constant (0.04286 and 0.03203 rate·min-1) were calculated for MB and MO, respectively. Mechanisms for the formation and photocatalytic activity of Cu-substituted plant-extracted cobalt ferrite were discussed. The Co0.4Cu0.6 Fe2O4 nanoferrite was found to be an efficient photocatalyst, and can be exploited for wastewater treatment applications for MB/MO elimination.

Size-Dependent Persistent Luminescence of YAGG:Cr3+ Nanophosphors.

In the current work, YAGG:Cr3+ nanophosphors were synthesized by the Pechini method and then annealed at different temperatures in the range 800-1300 °C. The structure and morphology of the samples were characterized by X-ray Powder Diffraction (XRPD). The lattice parameters and average crystalline sizes as site occupation by Al3+ and Ga3+ ions were calculated from the Rietveld refinement data. To investigate the effect of crystalline size of the materials on their optical properties: excitation and emission spectra were recorded and analyzed. Finally, the effect of crystalline size on the probability of carrier recombination leading to PersL was determined experimentally with thermoluminescence analyses. The Tmax-Tstop method was applied to determine the trap type and particle size (calcination temperature) effect on their redistribution. A correlation between structural changes and trap redistribution was found. In particular, the extinction of high-temperature TL maximum with increasing annealing temperatures is observed, while low-temperature TL maximum increases and reaches a maximum when the lattice parameter reaches saturation.

Correlation between the Dendritic Structure and Lattice Parameter of γ'-Phase in Single-Crystalline Turbine Blades Made of Superalloys.

The dendritic structure and the distribution of the γ'-phase lattice parameter (aγ') along selected lines of the longitudinal section in a model single-crystalline blade made of CMSX-4® nickel-based superalloy were studied. It was established that there is a correlation between the value of the aγ' and the predomination of initial or ending fragments of the secondary dendrite arms. It is most noticed for the areas where the dendrite growth conditions are similar to steady. They are located in the center and near the root's selector extension (SE) area. The correlation has been related to the dendritic segregation mechanism. It was shown that in the single-crystalline blades obtained by the directional crystallization using a spiral selector, the "walls" of the primary dendrite arms that grow at a low angle to the blade axis are created. It was found for the first time that the value of the lattice parameter aγ' is decreased near such "walls". Additionally, it was found that competitive growth of the dendrites may occur at a distance of even several millimeters from the bottom surface of the root. The first-time applied X-ray diffraction measurements of aγ' made in a single-pass along the line allow the analysis of the dendritic segregation in the whole blade cast.

Effects of Co/Mn Content Variation on Structural and Electrochemical Properties of Single-Crystal Ni-Rich Layered Oxide Materials for Lithium Ion Batteries.

The development of single-crystal nickel-rich layered LiNixCoyMn1-x-yO2 materials (S-NCMs) represents the most significant progress for the electrification applications of nickel-rich ternary materials. There has been prior research on the important role of transition metal elements in agglomerated materials, supplemented by surface and internal lattice optimization to drive the performance improvements. However, studies on S-NCMs, especially on the role of transition metals (TM, i.e., Co and Mn), have not been reported. In this study, we synthesized four kinds of S-NCMs with different Co/Mn contents and studied their structural, electrochemical, kinetic, and thermodynamic properties with different Co/Mn contents. The results were as follows: (1) Electrochemically, Co was more effective than Mn at 25 °C at enhancing the intercalation/deintercalation kinetics, which resulted in an increased discharge capacity, an improved rate capability, and a reduced energy loss. (2) Thermodynamically, Mn was more effective at maintaining a higher thermal stability than Co, especially at a low cutoff voltage, but at a high cutoff voltage, the difference between the action of Co and Mn decreased. The main finding of this work was the enhanced structural stability provided by Co, which could be attributed to the following: (i) the absence of the H2/H3 phase transformation when Co exceeded 15%, which inhibited the irreversible phase transformation and reduced the volume strain, and (ii) the lower degrees of decrease in the cell parameters a and c with higher contents of Co, which contributed to a low cracking degree along the (003) crystal plane. The current work provides an important reference for the single-crystallization strategy of nickel-rich materials.

High-precision atomic-scale strain mapping of nanoparticles from STEM images.

Strain is a crucial factor that influences the physicochemical properties of nanoparticles. Being able to precisely measure strain is important in understanding the intrinsic mechanism of the enhanced performance of nanoparticles. Techniques that have been developed for strain analysis using scanning transmission electron microscopy (STEM) images can be categorized into diffraction-based method and imaging-based method. Here, using image simulation techniques, it is found that the measured two-dimensional (2D) displacements from annular dark field (ADF) STEM images of a nanoparticle are a good approximation to a projection of the actual three-dimensional (3D) displacements. A methodology for deformation analysis is presented which is based on the detection of atomic columns from atomic-resolution STEM images in real space. Elastic deformation parameters such as strain are usually defined on the basis of a continuum of deformation. The appropriateness of various deformation parameters for atomic-scale investigation on STEM images is explored and a method for determining these is presented. We found that the local lattice parameter and principal strain components are the most physically meaningful parameters to express the materials distortion behaviour. Apart from the local lattice parameter, the other deformation parameters such as normal strains, shear strains and displacements, heavily rely on the choice of reference lattice. It is also found that different reference grids add a series of uniform offsets to these strain variations. Finally, this approach is applied to a PtCo3 bimetallic nanoparticle to quantify its deformation behaviour.

Effect of Blade Geometry on γ' Lattice Parameter and Primary Orientation of SX Cored Turbine Blades (I).

The γ' lattice parameter aγ' and the α angle defining the primary crystal orientation of the single-crystalline cored turbine blades made of CMSX-4 superalloy were measured in the areas located near the selector situated asymmetrically, considering the top view of the blade. The distributions of the aγ' and the α angle were determined along the lines parallel to the vertical blade axis Z using X-ray diffraction methods. The relations between changes in the aγ'(Z) and α(Z) were analyzed on the Z levels where the shape of the blade's cross-section changes. For the first time, the local increase in aγ'(Z) was found near the root-airfoil connection level and near certain other root levels, which is related to the change in blade section shapes on such levels. The local extremes in α(Z), representing the dendrite bend, were observed at these levels. The increase in the aγ'(Z) with the local bending of dendrites was discussed concerning the local redistribution of alloying elements and local residual stresses of the γ-dendrites. For the first time, a method of analyzing the local bending of the dendrites was proposed by studying the behavior of the α(Z). The presented results concern the first stage of the research covering areas relatively close to the selector, considering the top view of the blades. The second stage will include the analysis of the areas of the blade localized at a longer distance from the selector.

On the Possible Cause of Sudden Storage Modulus Increase during the Heating of PM FeMnSiCrNi SMAs.

A sudden increase in storage modulus (ΔE') was repeatedly recorded during the heating of powder metallurgy (PM) 66Fe-14Mn-6Si-9Cr-5Ni (mass. %) shape memory alloy specimens subjected to dynamic mechanical analysis (DMA), under constant applied strain amplitude and frequency. This instability, exceeding 12 GPa, was associated with the reverse martensitic transformation of α'-body centered cubic (bcc) martensite to γ-face centered cubic (fcc) austenite, overlapped on a magnetic transition. This transition, observed by thermomagnetic measurements (T-MAG), was associated with the temporary spontaneous alignment of magnetic spins, which lasted until thermal movement became prevalent, during heating. ΔE' was located around 250 °C on DMA thermograms and this temperature had the tendency to increase with the solution treatment temperature. On T-MAG diagrams, magnetization saturation temperature decreased from 405 °C to 52 °C with the increase in applied magnetic field from 20 Oe to 1 kOe and the increase in mechanically alloyed powder volume from 20% to 40%. On scanning electron micrographs, the presence of thermally induced α'-bcc martensite was emphasized together with the sub-bands that impede its stress-induced formation during DMA solicitation. On X-ray diffraction patterns of the solution-treated specimens, the presence of 22-82% α'-bcc martensite was identified, together with 8-55% retained austenite. It was assumed that the pre-existence of austenite together with α'-bcc martensite, in the microstructure of the solution-treated specimens, favored the magnetic transition, which destabilized the material and caused the storage modulus increase. The specimen comprising the largest amounts of austenite experienced the largest ΔE'.