High-resolution Synchrotron Radiation Research Articles

Microscopic Views of Atomic and Molecular Oxygen Bonding with epi Ge(001)-2 × 1 Studied by High-Resolution Synchrotron Radiation Photoemission.

In this paper, we investigate the embryonic stage of oxidation of an epi Ge(001)-2 × 1 by atomic oxygen and molecular O2 via synchrotron radiation photoemission. The topmost buckled surface with the up- and down-dimer atoms, and the first subsurface layer behaves distinctly from the bulk by exhibiting surface core-level shifts in the Ge 3d core-level spectrum. The O2 molecules become dissociated upon reaching the epi Ge(001)-2 × 1 surface. One of the O atoms removes the up-dimer atom and the other bonds with the underneath Ge atom in the subsurface layer. Atomic oxygen preferentially adsorbed on the epi Ge(001)-2 ×1 in between the up-dimer atoms and the underneath subsurface atoms, without affecting the down-dimer atoms. The electronic environment of the O-affiliated Ge up-dimer atoms becomes similar to that of the down-dimer atoms. They both exhibit an enrichment in charge, where the subsurface of the Ge layer is maintained in a charge-deficient state. The dipole moment that was originally generated in the buckled reconstruction no longer exists, thereby resulting in a decrease in the ionization potential. The down-dimer Ge atoms and the back-bonded subsurface atoms remain inert to atomic O and molecular O2, which might account for the low reliability in the Ge-related metal-oxide-semiconductor (MOS) devices.

The Kitagawa-Takahashi fatigue diagram to hybrid welded AA7050 joints via synchrotron X-ray tomography

The relationship between the microstructural nature and fatigue resistance was explored for laser welded AA7050-T7451. Based on high-resolution synchrotron radiation X-ray micro computed tomography, it is found that the large surface defects are a controlling factor in fatigue crack initiation. Besides, fine equiaxed grain zone (FQZ) near the fusion line appears to the failure site of hybrid laser welded joints. Particularly for gas pores-free at the weld surface, such FQZ might play a crucial role in degrading the service strength. Research results show that the evolution in microstructure, element and defects due to welding deteriorates the hardness, tensile strength and fatigue properties. Modified Murakami equation and Kitagawa-Takahashi diagram were finally established to correlate the fatigue strength with defects, which provides an important reference to assess the joints.

Characterization of biomimetic silicate- and strontium-containing hydroxyapatite microparticles embedded in biodegradable electrospun polycaprolactone scaffolds for bone regeneration

A significant need exists today to develop novel alternatives to traditional bone grafts. Here, we report the potential use of mechanochemically synthesized hydroxyapatite (HA), silicate-, or strontium-containing HA microparticles and microparticle aggregates in combination with polycaprolactone (PCL) as hybrid scaffolds for filling bone defects. The detailed characterization of scaffolds was performed with high-resolution synchrotron radiation–based microcomputed laminography, XRD, EDX, and FTIR. An in vitro cell-scaffold interaction analysis showed a significant improvement of cell spreading in the case of hybrid scaffolds with silicate- and Sr-containing HA. Scaffolds with Sr- and silicate-containing HA affected the expression of several genes involved in morphogenesis and transcription. Scaffolds with Sr-containing HA increased the expression of markers of the primary component of the extracellular matrix, and scaffolds with Sr-containing HA facilitated cell mineralization via an increase in osteocalcin production. The hybrid scaffolds with silicate- and Sr-containing HA microparticles exerted the highest antibacterial activity against gram-positive bacterium Staphylococcus aureus compared to the unmodified PCL scaffolds. Based on these findings, the obtained scaffolds with Sr- or silicate-containing HA are believed to hold promise for bone tissue regeneration as compared to scaffolds containing pure HA.

Synchrotron radiation computed tomography assessment of calcified plaques and coronary stenosis with different slice thicknesses and beam energies on 3D printed coronary models.

To investigate the effect of different slice thicknesses and beam energies on the visualization and assessment of coronary artery stenosis caused by calcified plaques using synchrotron radiation computed tomography (CT) based on 3D printed coronary artery models. Patient-specific 3D coronary models were created based on 3 sample coronary CT angiographic cases with calcified plaques in the left coronary arteries. In addition to the original significant coronary stenosis (>70%) shown on these CT images, stenoses of <50% and >90% were created in the segmented coronary models for simulation of different degrees of stenosis. The coronary lumen and calcification were printed with soft and rigid materials to simulate properties of coronary wall and calcified plaque, respectively. The models were scanned with synchrotron radiation CT with beam energies of 30, 40 and 50 keV and spatial resolution of 0.019×0.019×0.019 mm3 voxel size. Original high-resolution images were reconstructed with slice thicknesses of 0.095, 0.208, 0.302 and 0.491 mm to determine the effect of spatial resolution on plaque and coronary stenosis assessment based on 2D axial and 3D virtual intravascular endoscopy (VIE) images. Three coronary artery models were successfully printed with plaques placed in the coronary arteries to simulate different degrees of stenosis. 2D and 3D VIE images reconstructed with slice thicknesses of 0.095, 0.208 and 0.302 mm allowed for accurate assessment of coronary plaques and lumen stenosis with no significant differences (P>0.05). Synchrotron radiation CT images reconstructed with a slice thickness of 0.491 mm resulted in overestimation of coronary stenosis when compared to other images on 2D and 3D VIE views (<50% vs. 55-72%; 70-79% vs. 80-90%) with significant differences (P<0.05). Similarly, irregular plaque appearances were observed on 2D and 3D VIE images with a slice thickness of 0.491 mm when compared to others using thin slice thicknesses. The scanning protocol with beam energy of 30 keV provided optimal visualization of coronary lumen and plaque appearances. This study shows the feasibility of using 3D printed coronary artery models to simulate calcifications and different degrees of coronary stenosis. High resolution synchrotron radiation CT imaging with the 30 keV beam energy enables accurate assessment of coronary stenosis in the presence of calcification, thus highlighting the importance of high spatial resolution in the diagnosis of calcified coronary plaques.

(De)Lithiation Mechanism of Hierarchically Layered LiNi1/3Co1/3Mn1/3O2 Cathodes during High-Voltage Cycling

In view of the requirements for high-energy lithium ion batteries (LIBs), hierarchically layered LiNi1/3Co1/3Mn1/3O2 (NCM111) cathode materials have been prepared using a hydroxide coprecipitation method and subsequent high-temperature solid-state reaction. The diffraction results show that the synthesized NCM111 has a well-defined layered hexagonal structure. The initial specific discharge capacity of a Li/NCM111 cell is 204.5 mAh g−1 at a current density of 28 mA g−1 between 2.7 and 4.8 V. However, the cell suffers from poor capacity retention over extended charge-discharge cycles. The structural evolution of NCM111 electrode during electrochemical cycling is carefully investigated by in situ high-resolution synchrotron radiation diffraction. It is found that the nanodomain formation of a layered hexagonal phase H3 and a cubic spinel phase after charging to voltages above 4.6 V is the main source for the structural collapse in c direction and the poor cycling performance. This process is accompanied by the removal of oxygen, the transition metal (TM) migration and the crack generation in the nanodomains of the primary particles. These results may help to better understand the structural degradation of layered cathodes in order to develop high energy density LIBs.

Germanene Epitaxial Growth by Segregation through Ag(111) Thin Films on Ge(111).

Large-scale two-dimensional sheets of graphene-like germanium, namely, germanene, have been epitaxially prepared on Ag(111) thin films grown on Ge(111), using a segregation method, differing from molecular beam epitaxy used in previous reports. From the scanning tunneling microscopy (STM) images, the surface is completely covered with an atom-thin layer showing a highly ordered long-range superstructure in wide scale. Two types of protrusions, named hexagon and line, form a (7√7 × 7√7) R19.1° supercell with respect to Ag(111), with a very large periodicity of 5.35 nm. Auger electron spectroscopy and high-resolution synchrotron radiation photoemission spectroscopy demonstrate that Ge atoms are segregated on the Ag(111) surface as an overlayer. Low-energy electron diffraction clearly shows incommensurate "(1.35 × 1.35)" R30° spots, corresponding to a lattice constant of 0.39 nm, in perfect accord with close-up STM images, which clearly reveal an internal honeycomb arrangement with corresponding parameter and low buckling within 0.01 nm. As this 0.39 nm value is in good agreement with the theoretical lattice constant of free-standing germanene, conclusively, the segregated Ge atoms with trivalent bonding in honeycomb configuration form a characteristic two-dimensional germanene-like structure.

Laser Use in Endodontic for Increase the Adhesion of Root Canal Filling. A synchrotron radiation micro tomography study

The aim of the present paper is to explore, through a high-resolution synchrotron radiation-based micro computed tomography experiment, the efficiency of the Er:YAG laser involvement in the debridement of the root canal of pathologic teeth, applied after the chemo-mechanical treatment of the canal. The adhesion quality of root canal filling is the consequence of the root canal cleaning and shaping, thus preventing the leakage. Twelve extracted single-rooted teeth were considered. The first 5 mm of the roots, corresponding to the apical region of the teeth, were initially investigated through high-resolution synchrotron radiation phase-contrast micro computed tomography. Afterwards, a chemo-mechanical endodontic treatment was performed and the same region of the teeth was imaged again. Finally, an Er:YAG laser with PIPS tip treatment was applied on the same teeth and a last tomographic scan was done. The chemo-mechanical treatment properly removed the necrotic tissue only in the upper part of the apical area of root canal, but tissue debris were found in the lower and partially also in the medium and upper part of the apical region, especially when the apical area exhibited a larger curvature. The laser treatment applied afterwards gave good results in terms of removing the debris from the apical area of root canal, mainly when they remained in the main canal. The present study proves the capability of Er:YAG with PIPS tips laser treatment to enhance the removing of tissue debris from the apical region of root canals after a chemo-mechanical treatment. The high-resolution synchrotron radiation-based phase contrast micro computed tomography is the most powerful tool for a non-destructive 3D investigation method of the root canal morphology analysis and a proper characterization technique for the assessment of the endodontic treatment.

High-quality thulium iron garnet films with tunable perpendicular magnetic anisotropy by off-axis sputtering \u2013 correlation between magnetic properties and film strain

Thulium iron garnet (TmIG) films with perpendicular magnetic anisotropy (PMA) were grown on gadolinium gallium garnet (GGG) (111) substrates by off-axis sputtering. High-resolution synchrotron radiation X-ray diffraction studies and spherical aberration-corrected scanning transmission electron microscope (Cs-corrected STEM) images showed the excellent crystallinity of the films and their sharp interface with GGG. Damping constant of TmIG thin film was determined to be 0.0133 by frequency-dependent ferromagnetic resonance (FMR) measurements. The saturation magnetization (Ms) and the coercive field (Hc) were obtained systematically as a function of the longitudinal distance (L) between the sputtering target and the substrate. A 170% enhancement of PMA field (H⊥) was achieved by tuning the film composition to increase the tensile strain. Moreover, current-induced magnetization switching on a Pt/TmIG structure was demonstrated with an ultra-low critical current density (jc) of 2.5 × 106 A/cm2, an order of magnitude smaller than the previously reported value. We were able to tune Ms, Hc and H⊥ to obtain an ultra-low jc of switching the magnetization, showing the great potential of sputtered TmIG films for spintronics.

Direct Formation of C-C Double-Bonded Structural Motifs by On-Surface Dehalogenative Homocoupling of gem-Dibromomethyl Molecules.

Conductive polymers are of great importance in a variety of chemistry-related disciplines and applications. The recently developed bottom-up on-surface synthesis strategy provides us with opportunities for the fabrication of various nanostructures in a flexible and facile manner, which could be investigated by high-resolution microscopic techniques in real space. Herein, we designed and synthesized molecular precursors functionalized with benzal gem-dibromomethyl groups. A combination of scanning tunneling microscopy, noncontact atomic force microscopy, high-resolution synchrotron radiation photoemission spectroscopy, and density functional theory calculations demonstrated that it is feasible to achieve the direct formation of C-C double-bonded structural motifs via on-surface dehalogenative homocoupling reactions on the Au(111) surface. Correspondingly, we convert the sp3-hybridized state to an sp2-hybridized state of carbon atoms, i. e., from an alkyl group to an alkenyl one. Moreover, by such a bottom-up strategy, we have successfully fabricated poly(phenylenevinylene) chains on the surface, which is anticipated to inspire further studies toward understanding the nature of conductive polymers at the atomic scale.

Synchrotron radiation computed tomography versus conventional computed tomography for assessment of four types of stent grafts used for endovascular treatment of thoracic and abdominal aortic aneurysms.

To determine the accuracy of synchrotron radiation computed tomography (CT) for measurement of stent wire diameters for in vitro simulation of endovascular aneurysm repair by four different types of stent grafts when compared to conventional CT images. This study was performed using an aorta model with implantation of four aortic stent grafts for endovascular treatment of thoracoabdominal and abdominal aortic aneurysms. The aorta model was scanned using synchrotron radiation CT with beam energies ranging from 60 to 90 keV with 10 keV increment at each scan and spatial resolution of 41.6 µm per pixel. Stent wire diameters were measured at the top and body regions of each stent graft based on 2-dimensional (2D) axial and 3-dimensional (3D) reconstruction images, with measurements compared to those obtained from 128-slice CT images which were acquired with slice thickness of 0.5 mm. Synchrotron radiation CT images clearly demonstrated stent graft details with accurate assessment of stent wire diameters, with measurements at the top of stent grafts (between 0.32±0.02 and 0.47±0.02 mm) similar to the actual diameters (between 0.32±0.01 and 0.48±0.01 mm) when the beam energies of 70 and 80 keV were used, regardless of the types of stent grafts assessed. A beam energy of 60 keV resulted in stent wires thicker than the actual sizes, although this did not reach statistical significance (P=0.07-0.29), while the beam energy of 90 keV led to stent wires smaller than the actual sizes at the top (P=0.16) and body region (P=0.02) of stent grafts on 2D axial images. The stent wire sizes measured at the body region of stent grafts on 3D synchrotron radiation images (between 0.19±0.02 and 0.43±0.02 mm) were significantly smaller than the actual diameters (P=0.02-0.04). Stent wires were overestimated on conventional CT images with diameters more than 2-fold larger than the actual sizes (P=0.007-0.03) at both top and body regions of all four stent grafts. This study further confirms the accuracy of high-resolution synchrotron radiation CT in image visualization and size measurement of different aortic stent grafts with measured wire diameters similar to the actual ones, thus allowing for more accurate assessment of stent wire details for endovascular repair of aortic aneurysms.

Dl-3-N-butylphthalide attenuates ischemic reperfusion injury by improving the function of cerebral artery and circulation

Dl-3-N-butylphthalide (NBP) is approved in China for the treatment of ischemic stroke. Previous studies have shown that NBP promotes recovery after stroke via multiple mechanisms. However, the effect of NBP on vascular function and thrombosis remains unclear. Here, we aim to study the effect of NBP on vascular function using a rat model of transient middle cerebral artery occlusion (MCAO) and a state-of-the-art high-resolution synchrotron radiation angiography. Eighty SD rats underwent MCAO surgery. NBP (90 mg/kg) was administrated daily by gavage. Synchrotron radiation angiography was used to evaluate the cerebral vascular perfusion, vasoconstriction, and vasodilation in real-time. Neurological scores, brain infarction and atrophy were evaluated. Real-time PCR was used to assess the expression levels of thrombosis and vasoconstriction-related genes. Results revealed that NBP attenuated thrombosis after MCAO and reduced brain infarct and atrophy volume. NBP administrated at 1 and 4 h after MCAO prevented the vasoconstriction of the artery and maintained its diameter at normal level. Administrated at one week after surgery, NBP functioned as a vasodilator in rats after MCAO while displayed no vasodilating effect in sham group. Our results suggested that NBP attenuates brain injury via increasing the regional blood flow by reducing thrombosis and vasoconstriction.

Half-Heusler phase formation and Ni atom distribution in M-Ni-Sn (M = Hf, Ti, Zr) systems

High resolution synchrotron radiation powder X-ray diffraction (SR-PXD) and scanning transmission electron microscopy (STEM) have been employed for structural characterization of MNiSn, M0.5M′0.5NiSn and M0.5M′0.25M″0.25NiSn (M, M′, M″ = Hf, Ti, Zr) half-Heusler compounds, synthesized by arc melting and thermal annealing. Rietveld refinement results demonstrate that ternary Ti- and Hf-based compositions crystallize with only one half-Heulser phase, while two cubic phases are found in samples with nominal composition ZrNiSn. The performed analysis does not suggest obvious presence of excess Ni in any of the ternary compounds. Instead, it shows disordered distribution of the stoichiometric Ni atoms over 4c and the nominally vacant 4d sites in ZrNiSn as well as formation of Ni vacancies at the 4c site in ZrNi0.98Sn.

Large area planar stanene epitaxially grown on Ag(1 1 1)

Artificial post-graphene elemental 2D materials have received much attention recently. Especially, stanene, the tin analogue of graphene, is expected to be a robust 2D topological insulator, even above room temperature. We have grown epitaxial 2D stanene on a Ag(1 1 1) single crystal template and determined its crystalline structure synergetically by scanning tunneling microscopy, high-resolution synchrotron radiation photoemission spectroscopy, and advanced first principles calculations. From the STM images, we show that stanene forms a nearly planar structure in large domains. A detailed core-level spectroscopy analysis as well as DFT calculations reveal that the stanene sheet lays over an ordered 2D Ag2Sn surface alloy, but not directly on a bulk-terminated Ag(1 1 1) surface. The electronic structure exhibits a characteristic 2D band with parabolic dispersion due to the non-negligible interaction with the underlying surface alloy.

Phase equilibria and crystal chemistry of the CaO-½Gd2O3-CoOz system at 885 °C in air

The CaO-½Gd2O3-CoOz system prepared at 885 °C in air consists of two thermoelectric calcium cobaltate compounds, namely, the 2D thermoelectric oxide solid solution, (Ca3-xGdx)Co4O9-z (0 ≤ x ≤ 0.42) which has a misfit layered structure, and the 1D Ca3Co2O6 compound which consists of chains of alternating CoO6 trigonal prisms and CoO6 octahedra. Ca3Co2O6 was found to be a point compound. In the peripheral binary systems, Gd was not present in the Ca site of CaO, while a small solid solution region was identified for (Gd1-xCax)O(3-z)/2 (0 ≤ x ≤ 0.075). A solid solution region of distorted perovskite, (Gd1-xCax)CoO3-z (0 ≤ x ≤ 0.24, space group Pnma) was established. The structure of a member of the solid solution, (Gd0.92Ca0.08)CoO3-z, was determined using high resolution synchrotron radiation. A ternary oxide compound CaGdCoO4-z which has an orthorhombic structure (Bmab) was found to be stable at this temperature. Five solid solution tie-line regions and six three-phase regions were determined in the CaO-½Gd2O3-CoOz system. A comparison of the phase diagrams of the CaO-½R2O3-CoOz (R = La, Sm and Gd) systems is provided.

Elaborating the Crystal Structures of MgAgSb Thermoelectric Compound: Polymorphs and Atomic Disorders

Gaining insight into crystal structure is essential for understanding thermoelectric transport mechanisms and predicting thermoelectric properties. The main challenge in studying thermoelectric mechanisms is often imprecise or wrong models of the crystal structure. This work examines the structure modifications observed in MgAgSb thermoelectric materials by multitemperature high-resolution synchrotron radiation powder X-ray diffraction (SR-PXRD). Rietveld refinement reveals large atomic displacement parameters (ADPs) of the Ag1 atoms at the 4a position indicating possible atomic disorder, which may contribute to the low thermal conductivity observed in α-MgAgSb. The temperature dependence of anisotropic structural parameters indicates a tendency of increasing structural symmetry in α-MgAgSb with increasing temperature, largely contributing to the temperature evolution of the thermoelectric properties. Two MgAgSb polymorphs (β-MgAgSb and γ-MgAgSb) coexist at 700 K, and only the γ-MgAgSb crystalline phase i...

High resolution synchrotron radiation Fourier transform infrared spectrum of the COH-bending mode in methanol-D1 (CH2DOH)

In this work the high resolution synchrotron radiation Fourier transform spectrum in the range 1180–1300cm−1 corresponding to the COH-bending vibrational mode has been recorded and analyzed. The spectrum shows a structure analogous to a parallel band. Since the COH bending motion is one of the main contributors to the asymmetry in the torsional hindering potential barrier, the torsional barrier height in the excited state is expected to be quite different from that of the ground state. This makes the spectrum to spread over a wide region. Although the spectrum corresponding to the P- and R-branch looks very complicated, the Q-branches are well resolved and can be identified without much difficulty. It was possible to assign the spectra for K=0 to 10 for the trans- (e0) species. The interesting feature of the spectra is the absence of the lines for two other lower lying gauche symmetry species e1 and o1. The spectra due to any perpendicular transitions were absent as well. However some weak c-type transitions from gauche states (o1 and e1) in the ground state to the trans-species (e0) in the COD bending mode for low K-values ΔK=0 have been seen to be present in the spectra. These along with similar transitions for the OCD vibrational band are under investigation and the results will be communicated elsewhere. In the present work, analysis of the spectrum has been carried out to obtain precise term values and molecular parameters in the excited COH-bending state for the trans-species. The results will be shown valuable to assign similar spectra for the methanol-D2. This work represents the first reported high resolution study of this illusive vibrational mode in methanol-D1.

Deformations of the α-Fe2O3 rhombohedral lattice across the Néel temperature

High-resolution synchrotron radiation powder diffraction patterns of α-Fe2O3 measured between room temperature and 1100 K, i.e. above the Néel temperature T N = 950 K, have been analyzed. The integral breadths of the Bragg peaks show a hkl-dependent anisotropy, both below and above T N. This anisotropy can be quantitatively described by using a statistical peak-broadening model [Stephens (1999). J. Appl. Cryst. 32, 281]. Model calculations show that the rhombohedral α-Fe2O3 lattice is deformed and the deformation leads to a monoclinic lattice with the unique monoclinic axis along the hexagonal [110] direction both below and above T N. The monoclinic symmetry of bulk α-Fe2O3 is compatible with α-Fe2O3 nanowire growth along the [110] direction reported in Fu et al. [Chem. Phys. Lett. (2001), 350, 491].

Iron and niobium based additives in magnesium hydride: Microstructure and hydrogen storage properties

In this study, powder mixtures of MgH2 + 2 mol.% X, with X = Nb, Nb2O5, NbF5, Fe, Fe2O3, FeF3, were processed by mechanical milling at liquid nitrogen temperature (cryomilling). The effect of additives on crystalline structure, thermal properties and hydrogen storage properties of the mixtures were investigated. Morphological investigations indicated a heterogeneous particle size distribution of the powder mixtures and a fine dispersion of additive particles (FeF3) in the MgH2 matrix. High resolution synchrotron radiation X-ray diffraction (SR-XRD) data followed by Rietveld refinements showed a significant reduction on crystallite size for the samples containing fluorides (11 nm) in comparison with the pure MgH2 sample (29 nm). This was related to the mechanical behavior of fluorides during milling with MgH2, which act as a lubricant, dispersing and/or cracking agent during milling, and thus helping to further reduce MgH2 particle size. DSC analysis revealed that fluorides (NbF5, FeF3) are much more effective than oxides (Nb2O5, Fe2O3) and the transition metals (Nb and Fe), respectively, in reduction the desorption temperature. Furthermore, Nb2O5 is more efficient than Fe2O3. Finally, the best results for desorption kinetics were observed for the fluorides: NbF5 and FeF3 (equivalent effect and consistent to the DSC analysis) followed by the oxides: Nb2O5, Fe2O3 and Nb. The addition of Fe was not efficient in comparison with the pure cryomilled sample.

Multiscale and multimodality computed tomography for cortical bone analysis

In clinical studies, high resolution peripheral quantitative computed tomography (HR-pQCT) is used to separately evaluate cortical bone and trabecular bone with an isotropic voxel of 82 µm3, and typical cortical parameters are cortical density (D.comp), thickness (Ct.Th), and porosity (Ct.Po).In vitro, micro-computed tomography (micro-CT) is used to explore the internal cortical bone micro-structure with isotropic voxels and high resolution synchrotron radiation (SR); micro-CT is considered the ‘gold standard’.In 16 tibias and 8 femurs, HR-pQCT measurements were compared to conventional micro-CT measurements. To test modality effects, conventional micro-CT measurements were compared to SR micro-CT measurements at 7.5 µm3; SR micro-CT measurements were also tested at different voxel sizes for the femurs, specifically, 7.5 µm3 versus 2.8 µm3.D.comp (r = −0.88, p < 10−3) was the parameter best correlated with porosity (Po.V/TV). The correlation was not affected by the removal of pores under 130 µm. Ct.Th was also significantly highly correlated (r = −0.89 p < 10−3), while Ct.Po was correlated with its counterpart Po.V/TV (r = 0.74, p < 10−3).From SR micro-CT and conventional micro-CT at 7.5 µm3 in matching areas, Po.V/TV and pore diameter were underestimated in conventional micro-CT with mean ± standard deviation (SD) biases of −2.5 ± 1.9% and −0.08 ± 0.08 mm, respectively. In contrast, pore number (Po.N) and pore separation (Po.Sp) were overestimated with mean ± SD biases of +0.03 ± 0.04 mm−1 and +0.02 ± 0.04 mm, respectively. The results from the tibia and femur were similar when the results of SR micro-CT at 7.5 µm3 and 2.8 µm3 were compared. Po.V/TV, specific surface of pores (Po.S/Po.V), and Po.N were underestimated with mean biases of −1.7 ± 0.9%, −4.6 ± 4.4 mm−1, and −0.26 ± 0.15 mm−1, respectively. In contrast, pore spacing was overestimated at 7.5 µm3 compared to 2.8 µm3 with mean biases of 0.05 ± 0.03 mm.Cortical bone measurements from HR-pQCT images provided consistent results compared to those obtained using conventional micro-CT at the distal tibia. D.comp was highly correlated to Po.V/TV because it considers both the micro-porosity (Haversian systems) and macro-porosity (resorption lacunae) of cortical bone. The complexity of canal organization, (including shape, connectivity, and surface) are not fully considered in conventional micro-CT in relation to beam hardening and cone beam reconstruction artifacts. With the exception of Po.V/TV measurements, morphological and topological measurements depend on the characteristics of the x-ray beam, and to a lesser extent, on image resolution.

Distribution of dislocations in AlN crystals grown on evaporating SiC substrates

By the use of high-resolution X-ray diffractometry and synchrotron radiation topography, the distribution of dislocations in AlN crystals grown on evaporating SiC substrates is studied. The growth of AlN layer in one process with the evaporation of SiC substrate gave the possibility to prevent the relaxation of thermal stresses through cracking of AlN during cooling the structure. The continuous 0.2-1.5 mm thick plates were used as the model objects for the study of dislocation structure near the AlN/SiC interface. Analysis of the broadening of the Bragg reflection peaks, the shape of scattering maps in reciprocal space and topographs showed that dislocations formed the mosaic structure, different from the distribution of threading dislocations in GaN epilayers. A theoretical model for misfit strain relaxation in the growing AlN layer is suggested. The results enable to clarify the dislocation processes during sublimation growth of industrial quality AlN crystals.