Orientation Of Crystallites Research Articles

Interdependence of Support Wettability ‐ Electrodeposition Rate‐ Sodium Metal Anode and SEI Microstructure

AbstractThis study examines how current collector support chemistry (sodiophilic intermetallic Na2Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm−2, 0.5–3 mA cm−2) representative of commercially relevant mass loading in anode‐free sodium metal battery (AF‐SMBs) are analyzed. Synchrotron X‐ray nanotomography and grazing‐incidence wide‐angle X‐ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo‐FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te−Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

Interdependence of Support Wettability - Electrodeposition Rate- Sodium Metal Anode and SEI Microstructure.

This study examines how current collector support chemistry (sodiophilic intermetallic Na2Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm-2, 0.5-3 mA cm-2) representative of commercially relevant mass loading in anode-free sodium metal battery (AF-SMBs) are analyzed. Synchrotron X-ray nanotomography and grazing-incidence wide-angle X-ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo-FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te-Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

Orientation Distribution of Crystalline β-Sheet Domains in Bombyx mori Silk Fiber Studied with Vibrational Sum Frequency Generation Spectroscopy.

Silk fibers have good biocompatibility and mechanical properties, which make them attractive in biomaterial applications as well as textile industries. It is believed that the superior mechanical property is associated with the crystalline β-sheet structure in the fiber; but a deeper understanding of the structure-property relationship is still needed for full exploitation of its physical properties. Especially, accurate information on hydrogen-bonding interactions within β-sheet domains at the nanoscale and their spatial distributions at the mesoscale are critically needed. In this study, we demonstrate the selective detection of crystalline β-sheet domains in Bombyx mori silk fiber using sum frequency generation (SFG) spectroscopy and its use to determine the angular distribution of the β-sheet crystallites with respect to the fiber axis. Numerical simulations of the SFG signal of the amide-I band were carried out using tensors based on the B2 symmetry of the D2 point group and compared with experimental data. This comparison found that the crystalline β-sheet domains are aligned along the fiber axis with a standard deviation of ∼27° and parallel to the fiber surface with a standard deviation of ∼5°. It was also found that the amide bands in the SFG spectra cannot be fully explained with the assumption that the crystalline β-sheet vibrations can be described with the D2 point group. Being able to monitor the amide group vibrations sensitive to both interchain hydrogen bonding and crystallite orientations, SFG analysis has a potential to unveil the structure-mechanical property relationship that may not be readily assessable with other characterization techniques.

Correlation of Processing and Structure in an Ethylene-Glycol Side-Chain Modified Polythiophene via Combined X-Ray Scattering and 4D Scanning Transmission Electron Microscopy.

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. The effects of heat treatment on the distribution and type of crystallites present in the films isdetermined.

Energy-dispersive Laue diffraction analysis of the influence of statherin and histatin on the crystallographic texture during human dental enamel demineralization.

Energy-dispersive Laue diffraction (EDLD) is a powerful method to obtain position-resolved texture information in inhomogeneous biological samples without the need for sample rotation. This study employs EDLD texture scanning to investigate the impact of two salivary peptides, statherin (STN) and histatin-1 (HTN) 21 N-terminal peptides (STN21 and HTN21), on the crystallographic structure of dental enamel. These proteins are known to play crucial roles in dental caries progression. Three healthy incisors were randomly assigned to three groups: artificially demineralized, demineralized after HTN21 peptide pre-treatment and demineralized after STN21 peptide pre-treatment. To understand the micro-scale structure of the enamel, each specimen was scanned from the enamel surface to a depth of 250 µm using microbeam EDLD. Via the use of a white beam and a pixelated detector, where each pixel functions as a spectrometer, pole figures were obtained in a single exposure at each measurement point. The results revealed distinct orientations of hydroxyapatite crystallites and notable texture variation in the peptide-treated demineralized samples compared with the demineralized control. Specifically, the peptide-treated demineralized samples exhibited up to three orientation populations, in contrast to the demineralized control which displayed only a single orientation population. The texture index of the demineralized control (2.00 ± 0.21) was found to be lower than that of either the STN21 (2.32 ± 0.20) or the HTN21 (2.90 ± 0.46) treated samples. Hence, texture scanning with EDLD gives new insights into dental enamel crystallite orientation and links the present understanding of enamel demineralization to the underlying crystalline texture. For the first time, the feasibility of EDLD texture measurements for quantitative texture evaluation in demineralized dental enamel samples is demonstrated.

Ferroelectric Al0.85Sc0.15N and Hf0.5Zr0.5O2 Domain Switching Dynamics.

The capability to reliably program partial polarization states with nanosecond programming speed and femtojoule energies per bit in ferroelectrics makes them an ideal candidate to realize multibit memory elements for high-density crossbar arrays, which could enable neural network models with a large number of parameters at the edge. However, a thorough understanding of the domain switching dynamics involved in the polarization reversal is required to achieve full control of the multibit capability. Transient current integration measurements are adopted to investigate the domain dynamics in aluminum scandium nitride (Al0.85Sc0.15N) and hafnium zirconium oxide (Hf0.5Zr0.5O2). The switching dynamics are correlated to the crystal structure of the films. The contributions of domain nucleation and domain wall motion are decoupled by analyzing the rate of change of the time-dependent normalized switched polarization. Thermally activated creep domain wall motion characterizes the Al0.85Sc0.15N switching dynamics. The statistics of independently nucleating domains and the domain wall creep motion in Hf0.5Zr0.5O2 are associated with the spatially inhomogeneous distribution of local switching field due to polymorphism, absence of preferential crystallite orientation, as well as defects and charges that can be located at the grain boundaries. The c-axis texture, single-phase nature, and strong likelihood of less fabrication process-induced defects contribute to the homogeneity of the local switching field in Al0.85Sc0.15N. Nonetheless, defects generated and redistributed upon bipolar electric field switching cycling result in Al0.85Sc0.15N domain wall pinning. The wake-up effect in Hf0.5Zr0.5O2 is explained thorough the continuous addition of switchable regions associated with two independent distributions of characteristic switching times.

Harvesting of shear piezoelectricity in a molded multicomponent crystal disc

Biomolecular piezoelectrics, such as amino acids and peptides, exhibit significant shear piezoelectric responses in single crystal form. However, naturally occurring longitudinal piezoelectricity is rare and, when present, is dampened due to the multi-directional self-assembly in polycrystalline device layers. Here we utilise cocrystallisation to engineer a multicomponent crystalline salt hydrate of S(+)Mandelic Acid and LLysine, S-Mand•L-Lys•5H2O (1). This material exhibits a predicted single crystal longitudinal piezoelectric response of d33 = 3.5 pC/N. In polycrystalline form, 1 grows as an assembly of plates which increases the measured longitudinal piezoelectricity to 11 pC/N in its macroscopic solid-state. This is due to contributions from the shear piezoelectric response d36 = 10.8 pC/N, originating from the presence of plates oriented at acute angles relative to the surface. The brittleness of the crystals (E = 37 GPa) is overcome by reinforcing the substrate-free piezoelectric disc with a thin polymer coating to prevent flaking. Structural analysis confirms that the triclinic structure of 1 gives rise to this increased response due to the relative orientations of individual crystallites. Confined crystallisation of this multi-component form with a plate-like morphology, results in macroscopic self-assembly of an amino acid cocrystal that allows for the harvesting of higher shear piezoelectricity, but in a facile longitudinal configuration.

Unveiling the microscopic compression failure behavior of mesophase-pitch-based carbon fibers for improving the compressive strength of their polymer composites

Mesophase-pitch-based carbon fiber (MPCF) reinforced polymer (MPCFRP) composites show great potential for aerospace applications due to their excellent thermal conductivity and dimensional stability. However, the low compressive strength severely limits their application in high load-bearing areas. To address this issue, MPCF-A with a split-radial structure and MPCF-B with a skin-core structure were meticulously prepared by fiber structure regulation. The compression failure behavior of MPCFs at the monofilament and the microregion levels was investigated using the tensile recoil method and in-situ micropillar compression technique. MPCF-A exhibits the failure mode of petal-like lamellar separation due to axial crack penetrating along the (002) crystal plane of graphite layers, with the compressive strength of the core region (391 MPa) being higher than that of the skin region (360 MPa). Conversely, MPCF-B demonstrates a large transverse fracture in the skin region during damage, along with uniform microcracks in the core region. Notably, the compressive strength of the core region (547 MPa) significantly exceeds that of the skin region (456 MPa). Furthermore, the compressive strength of MPCF-B monofilaments (583 MPa) is higher than that of MPCF-A (462 MPa), attributed to factors such as the smaller graphite crystallite size (La = 36.54 nm, Lc = 26.75 nm), lower crystallite orientation (Z = 10.21°, R = 0.25), smaller pore size (Rg = 9.56 nm), and higher amorphous carbon content (g = 69.77%, K = 20.38). Consequently, the compressive strength of MPCFRP-B (232 MPa) is enhanced by 30.3% compared to MPCFRP-A.

Enhancing the corrosion resistance of mild steel coated zinc studies

In the presence of a newly created brightener, the zinc metal is coated on steel using the electro deposition process. Experiments using hull cells are used to optimize the settings and components of plating baths. Tafel Polarization and EIS techniques were used to conduct corrosion experiments, which made it possible to investigate the brilliant zinc coating's effective corrosion resistance. SEM and Reflectance spectroscopy both confirm that the bright zinc coating has modified surface morphology. XRD analysis is used to study and validate changes in crystallite orientation and phase structure. Electrochemical methods and theoretical molecular dynamic (MD) simulations were used to examine the interaction between Zn and the metal surface. FTIR spectroscopy has been used in blend investigations which impacts on the physical characteristics of polymer blends. The results of these research showed how novel brighteners can improve zinc deposits' brightness and corrosion resistance when applied to mild steel substrates.

Simulating multipulse NMR spectra of polycrystalline solids in the frequency domain.

An approach is presented for simulating multipulse nuclear magnetic resonance (NMR) spectra of polycrystalline solids directly in the frequency domain. The approach integrates the symmetry pathway concept for multipulse NMR with efficient algorithms for calculating spinning sideband amplitudes and performing interpolated finite-element numerical integration over all crystallite orientations in a polycrystalline sample. The numerical efficiency is achieved through a set of assumptions used to approximate the evolution of a sparse density matrix through a pulse sequence as a set of individual transition pathway signals. The utility of this approach for simulating the spectra of complex materials, such as glasses and other structurally disordered materials, is demonstrated.

Scanning WAXS microscopy of regenerated cellulose fibers at mesoscopic resolution.

In this work, regenerated cellulose textile fibers, Ioncell-F, dry-wet spun with different draw ratios, have been investigated by scanning wide-angle X-ray scattering (WAXS) using a mesoscopic X-ray beam. The fibers were found to be homogeneous on the 500 nm length scale. Analysis of the azimuthal angular dependence of a crystalline Bragg spot intensity revealed a radial dependence of the degree of orientation of crystallites that was found to increase with the distance from the center of the fiber. We attribute this to radial velocity gradients during the extrusion of the spin dope and the early stage of drawing. On the other hand, the fiber crystallinity was found to be essentially homogeneous over the fiber cross section.

Crystallographic Texture Evolution in 3D Printed Polyethylene Reactor Blends.

In this work, crystallographic texture evolution in 3D printed trimodal polyethylene (PE) blends and high-density PE (HDPE) benchmark material were investigated to quantify the resulting material anisotropy, and the results were compared to materials made from conventional injection molded (IM) samples. Trimodal PE reactor blends consisting of HDPE, ultrahigh molecular weight PE (UHMWPE), and HDPE_wax have been used for 3D printing and injection molding. Changes in the preferred orientation and distribution of crystallites, i.e., texture evolution, were quantified utilizing the wide angle X-ray diffraction through pole figures and orientation distribution functions (ODFs) for 3D printed and IM samples. Since the change in weight-average molecular weight (Mw) of the blend was expected to significantly affect the resulting crystallinity and orientation, the overall Mw of the trimodal PE blend was varied while keeping the UHMWPE component weight fraction to 10% in the blend. The resulting texture was analyzed by varying the overall Mw of the trimodal blend and the process parameters in 3D printing and compared to the texture of conventional IM samples. The printing speed and orientation (defined with respect to the axis along the length of the samples) were used as the variable process parameters for 3D printing. The degree of anisotropy increases with an increase in the nonuniform distribution of intensities in pole figures and ODFs. All the highest intensity major texture components in IM and 3D printed samples (0° printing orientation) of reactor blends are observed to have crystals oriented in [001] or [001̅]. Overall, for the same throughput, 3D printed samples in the 0° orientation showed greater texture evolution and higher anisotropy compared to IM samples. Most notably, an increase in 3D printing speed increased the crystalline distribution closer to the 0° direction, increasing the anisotropy, while deviation from this printing orientation reduced crystalline distribution closer to the 0° direction, thus increasing isotropy. This demonstrates that tailoring material properties in specific directions can be achieved more effectively with 3D printing than with the injection molding process. Change in the overall Mw of the trimodal PE blend changed the preferential orientation distribution of the crystal planes to some degree. However, the degree of anisotropy remained the same in almost all cases, indicating that the effect of molecular weight distribution is not as significant as the printing speed and printing orientation in tailoring the resulting properties. The 3D printing process parameters (speed and orientation) were shown to have more influence on the texture than the material parameters associated with the blend.

Effect of processing conditions on the properties of vitrimerized polybutylene terephthalate prepared by reactive extrusion

This study examined the effects of continuous reactive extrusion on the properties of vitrimerized thermoplastics derived from polybutylene terephthalate (PBT). PBT formulations were prepared using epoxy (crosslinker) and zinc acetylacetonate (transesterification catalyst) to form dynamic covalent networks. Reactive extrusion was performed at different screw rotation speeds (50, 100, 200 rpm) with controlled residence times to compare the effects of the shear stress during the formation of crosslinks on the vitrimer properties. The rheological behavior of the extruded vitrimerized PBT suggests that competition between chain scission and branching occurs during the dynamic crosslinking of thermoplastics. Increasing the shear stress and/or time in the extruder was found to favor chain scission over crosslinking which makes gelation unattainable. In the case of injection molded specimens, tensile and X-ray diffraction tests of vitrimerized PBT extruded at different shear stress indicated a significant relationship between the degree of crosslinking, the orientation of crystallites, and the ability of the polymer network to withstand deformation at elevated temperatures.

The influence mechanisms of re-fused scanning on the surface roughness, microstructural evolution and mechanical properties of laser powder bed fusion processed AlMgScZr alloy

Laser powder bed fusion (LPBF) stands out as the foremost method for achieving intricate structure with superior design flexibility among additive manufacturing technologies. Within the LPBF process, surface roughness serves as a critical metric governing both fabrication precision and build quality. This study delves into the evolution of the top and side surface roughness as re-fused scanning times increase in LPBF-fabricated AlMgScZr alloy. Concurrently, the investigation evaluates alterations in microstructural characteristics and mechanical properties. Various characterization techniques, including confocal laser scanning microscope, scanning electron microscope, X-ray diffraction, electron backscatter diffraction, as well as tensile and microhardness tests, are employed. The findings concerning the top surface reveal that the initial application of re-fused scanning contributes to enhanced surface roughness. This improvement stems from refined grain structures and induced lattice distortions, facilitated by rapid heat dissipation and thermal recycling within the solidified layer. Consequently, microhardness increases. However, introducing the subsequent re-fused scanning exacerbates surface roughness and instigates Marongoni flow instability, magnesium depletion, and alterations in lattice structures. Moreover, with increasing the re-fused times, there is a noticeable enhancement in preferential crystallite growth orientation along the (200)α-Al crystal plane. Regarding the side surface, escalating re-fused times correlate with deteriorating roughness and alterations in molten pool shape and size, attributable to successive energy input. Despite these surface variations, minimal differences are observed in yield strength, tensile strength, and elongation. In essence, this research offers valuable insights into selecting optimal scanning methodologies during the LPBF process, thus guiding improvements in fabrication precision and component quality.

Effect of layered transition metal dichalcogenide hybrid nanomaterials on the piezoelectric performance of non‐solvent induced phase separated polyvinylidene fluoride

AbstractLayered transition metal dichalcogenides (TMDs) with high aspect ratios enhance the alignment of polymer chains and induce a preferred orientation of the polymeric crystallites when incorporated into polyvinylidene fluoride (PVDF). In addition to offering an effective charge‐transfer mechanism, TMDs give PVDF more rigidity and piezoelectric qualities. This work reports the non‐solvent induced phase separation (NIPS) introduced while developing the PVDF/MoS2 composites. During the NIPS, the PVDF chains become phase‐separated, which induces high polarization in the PVDF matrix. Phase‐separated PVDF/MoS2 composites show high porosity and charge distribution attributed to the enhanced piezoelectric output voltage. While the neat PVDF demonstrated very feeble output voltage generation, the hybrid composite containing 2 wt.% of MoS2/ZnO facilitated almost 20 times higher performance (peak‐to‐peak voltage of 2.4 V). This work yielded a phase‐separated composite that finds uses in energy harvesting, sensors, and actuators, among other fields.Highlights NIPS creates high‐porosity composites with improved charge distribution. Layered TMDs improve charge‐transfer mechanism and PVDF's electrical properties. 2 wt.% MoS2/ZnO exhibits nearly 20 times higher voltage generation than neat PVDF.

Improving the mechanical properties and thermal conductivity of mesophase-pitch-based carbon fibers by controlling the temperature in industrial spinning equipment

Mesophase-pitch-based carbon fibers (MPCFs) were prepared using industrial equipment with a constant extrusion rate of pitch while controlling the spinning temperature. The influence of spinning temperature on their microstructures, mechanical properties and thermal conductivities was investigated. SEM images of the fractured surface of MPCFs show that the graphite layers have a radiating structure at all spinning temperatures, but change from the fine-and-folded to the large-and-flat morphology when increasing the spinning temperature from 309 to 320 oC. At the same time the thermal conductivity and tensile strength of the MPCFs respectively increase from 704 W·m−1·K−1 and 2.16 GPa at 309 oC to 1 078 W·m−1·K−1 and 3.23 GPa at 320 oC. The lower viscosity and the weaker die-swell effect of mesophase pitch at the outlets of the spinnerets at the higher spinning temperature contribute to the improved orientation of mesophase pitch molecules in the pitch fibers, which improves the crystallite size and orientation of the MPCFs.

A microstructure-based model for the thermal conductivity of carbon fibers

In this paper, a model is developed to predict the thermal conductivity of carbon fibers (CFs) based on the microstructure information and phase composition obtained experimentally. The microstructures of four different CFs are investigated by SEM and XRD. The contents of graphite crystallites, amorphous carbon, and microvoids are estimated by the internal standard method. Crystallinity, crystallite size, and the orientation of crystallite are considered in the model. The predicted thermal conductivities are in good agreement with the reported values. The contribution of the microstructural factors on the thermal conductivity is evaluated. It is revealed that crystallinity is the major factor that affects the thermal conductivity of CFs. Furthermore, the predictions of the presented model are also compared with the prediction of empirical models based on the measured electrical resistivity. The results show that the prediction of our model has a higher generality. The fundamental understanding on the thermal conductivity of CFs may benefit the development of high-performance CFs.

Analysis of the turbostratic structures in PAN-based carbon fibers with wide-angle x-ray diffraction

Carbon fiber (CF) is a versatile material renowned for its excellent mechanical, thermal, and electrical properties. Polyacrylonitrile (PAN)-based CFs dominate the market in part due to their high tensile strength, rendering them suitable for structural applications in a wide variety of applications ranging from sporting goods to aerospace. Over five decades of commercial development of PAN-based CF has resulted in a range of varieties with different tensile moduli and tensile strengths. The microstructures, nanostructures, and crystal structures of PAN-based CF all play pivotal roles in the macroscale properties of this material. In particular, the crystal structure and crystallite orientation in CF is closely related to the mechanical properties. The crystal structure of PAN-based CF generally consists of turbostratic carbon, a disordered form of graphite, the characteristics of which can be effectively characterized in a bulk format through wide-angle x-ray diffraction (WAXD). In this work, we employed a three-part approach to the analysis of WAXD patterns collected from four intermediate modulus PAN-based CFs. The approach incorporates a Scherrer analysis, a Debye analysis, and an orientational analysis to provide precise estimates of crystallite sizes, crystallite distributions, and crystallite orientations with the fiber axis. The results presented here suggest that intermediate modulus PAN-based CF mostly consists of small turbostratic crystallites (<4 nm), with larger crystallites having increased orientation with the fiber axis. The results here imply the presence of curvature and/or wrinkling of the turbostratic layers within the CF structure.

Mg incorporation induced microstructural evolution of reactively sputtered GaN epitaxial films to Mg-doped GaN nanorods

Mg-doped GaN films/nanorods were grown epitaxially on c-sapphire by reactive co-sputtering of GaAs and Mg at different N2 percentages in Ar–N2 sputtering atmosphere. Energy dispersive x-ray spectroscopy revealed that the Mg incorporation increases with increase of Mg area coverage of GaAs target, but does not depend on N2 percentage. In comparison to undoped GaN films, Mg-doped GaN displayed substantial decrease of lateral conductivity and electron concentration with the initial incorporation of Mg, indicating p-type doping, but revealed insulating behaviour at larger Mg content. Morphological investigations by scanning electron microscopy have shown that the films grown with 2%–4% Mg area coverages displayed substantially improved columnar structure, compared to undoped GaN films, along with rough and voided surface features at lower N2 percentages. With increase of Mg area coverage to 6%, the growth of vertically aligned and well-separated nanorods, terminating with smooth hexagonal faces was observed in the range of 50%–75% N2 in sputtering atmosphere. High-resolution x-ray diffraction studies confirmed the epitaxial character of Mg-doped GaN films and nanorods, which displayed complete c-axis orientation of crystallites and a mosaic structure, aligned laterally with the c-sapphire lattice. The catalyst-free growth of self-assembled Mg-doped GaN nanorods is attributed to increase of surface energy anisotropy due to the incorporation of Mg. However, with further increase of Mg area coverage to 8%, the nanorods revealed lateral merger, suggesting enhanced radial growth at larger Mg content.

Tooth acellular extrinsic fibre cementum incremental lines in humans are formed by parallel branched Sharpey’s fibres and not by its mineral phase

In humans, the growth pattern of the acellular extrinsic fibre cementum (AEFC) has been useful to estimate the age-at-death. However, the structural organization behind such a pattern remains poorly understood. In this study tooth cementum from seven individuals from a Mexican modern skeletal series were analyzed with the aim of unveiling the AEFC collagenous and mineral structure using multimodal imaging approaches. The organization of collagen fibres was first determined using: light microscopy, transmission electron microscopy (TEM), electron tomography, and plasma FIB scanning electron microscopy (PFIB-SEM) tomography. The mineral properties were then investigated using: synchrotron small-angle X-ray scattering (SAXS) for T-parameter (correlation length between mineral particles); synchrotron X-ray diffraction (XRD) for L-parameter (mineral crystalline domain size estimation), alignment parameter (crystals preferred orientation) and lattice parameters a and c; as well as synchrotron X-ray fluorescence for spatial distribution of calcium, phosphorus and zinc. Results show that Sharpey’s fibres branched out fibres that cover and uncover other collagen bundles forming aligned arched structures that are joined by these same fibres but in a parallel fashion. The parallel fibres are not set as a continuum on the same plane and when they are superimposed project the AEFC incremental lines due to the collagen birefringence. The orientation of the apatite crystallites is subject to the arrangement of the collagen fibres, and the obtained parameter values along with the elemental distribution maps, revealed this mineral tissue as relatively homogeneous. Therefore, no intrinsic characteristics of the mineral phase could be associated with the alternating AEFC incremental pattern.