Advanced Photon Source Research Articles

In situ synchrotron tensile investigations on ultrasonic additive manufactured (UAM) zirconium

The microstructure evolution during room temperature uniaxial tensile straining of ultrasonic additive manufactured (UAM) zirconium was evaluated using the Advanced Photon Source (APS) facility. Miniature dog-bone tensile specimens of two orientations were cut from a UAM-fabricated zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stages of plastic deformation, which become candidate necking positions and eventually lead to failure. Fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvements of the UAM zirconium fabrication process.

Design study and test of input coupler for 500 MHz five-cell cavity

This paper presents an optimized design and preliminary test result of a high-power input coupler. The design is motivated by five-cell Petra-type cavities operating in the Southern Advanced Photon Sources booster. We optimize the design of the high-power input coupler from the prototype, including the window geometry redesign and multipacting analysis to meet a 250 kW operation power upgrade plan. The cooling system of the coupler is redesigned to achieve a low temperature in high-power operation. Design results fulfill the five-cell cavity operation requirement. The corresponding waveguide and coaxial transition structures are developed and tested. We also describe the coupler's coupling coefficient tests and high-power test plans.

An automated approach to the alignment of compound refractive lenses.

Compound refractive lenses (CRLs) are established X-ray focusing optics, and are used to focus the beam or image the sample in many beamlines at X-ray facilities. While CRLs are quite established, the stack of single lens elements affords a very small numerical aperture because of the thick lens profile, making them far more difficult to align than classical optical lenses that obey the thin-lens approximation. This means that the alignment must be very precise and is highly sensitive to changes to the incident beam, often requiring regular readjustments. Some groups circumvent the full realignment procedure by using engineering controls (e.g. mounting optics) that sacrifice some of the beam's focusing precision, i.e. spot size, or resolution. While these choices minimize setup time, there are clear disadvantages. This work presents a new automated approach to align CRLs using a simple alignment apparatus that is easy to adapt and install at different types of X-ray experiments or facilities. This approach builds on recent CRL modeling efforts, using an approach based on the Stochastic Nelder-Mead (SNM) simplex method. This method is outlined and its efficacy is demonstrated with numerical simulation that is tested in real experiments conducted at the Advanced Photon Source to confirm its performance with a synchrotron beam. This work provides an opportunity to automate key instrumentation at X-ray facilities.

Quantitative analysis of diffraction by liquids using a pink-spectrum X-ray source

A new approach for performing quantitative structure-factor analysis and density measurements of liquids using X-ray diffraction with a pink-spectrum X-ray source is described. The methodology corrects for the pink beam effect by performing a Taylor series expansion of the diffraction signal. The mean density, background scale factor, peak X-ray energy about which the expansion is performed, and the cutoff radius for density measurement are estimated using the derivative-free optimization scheme. The formalism is demonstrated for a simulated radial distribution function for tin. Finally, the proposed methodology is applied to experimental data on shock compressed tin recorded at the Dynamic Compression Sector at the Advanced Photon Source, with derived densities comparing favorably with other experimental results and the equations of state of tin.

Model predictive control of long Transfer-line cooling process based on Back-Propagation neural network

• A model predictive control (MPC) method based on back-propagation (BP) neural network as a surrogate inversion model was designed to improve the automation of the long transfer-line pre-cooling process. • A one-dimensional simulation model based on unsteady flow and heat transfer process was used to generate training datasets for BP neural networks, and reasonable cleaning rules are the key to obtain better training results. • Simulation and test results show that the MPC method can be applied to the automatic control of nonlinear large hysteresis dynamical systems such as the long transfer-line pre-cooling process. As the scale of large cryogenic systems continues to expand, the thermal inertia and nonlinear characteristics of the pre-cooling process of long-distance cryogenic transfer-line become obvious, and the traditional control methods are less effective in controlling such nonlinear large hysteresis time-varying systems. To improve the automation of the pre-cooling process, a Model Predictive Control (MPC) method based on Back-Propagation (BP) neural network as a surrogate inversion model was designed and deployed on a large helium cryogenic system of the Platform of Advanced Photon Source (PAPS). Simulation and test results show that the MPC method can be applied to the automatic control of nonlinear large hysteresis dynamical systems; the BP neural network as a surrogate model can invert the one-dimensional flow heat transfer model better. The actual test results on the PAPS cryogenic system show that the method can realize the automatic pre-cooling of long transfer-line, and the overall cooling effect is stable and efficient, with the maximum absolute temperature difference of no more than 3.2 K and the maximum relative temperature difference of no more than 2.1% from the ideal cooling line.

Real-time streaming tomographic reconstruction with on-demand data capturing and 3D zooming to regions of interest.

Complex dynamic tomographic experiments at brilliant X-ray light sources require real-time feedback on the sample changes with respect to environmental conditions, selecting representative regions of interest for high-resolution scanning, and on-demand data saving mechanisms for storing only relevant projections acquired by fast area detectors and reducing data volumes. Here the implementation details of a 3D real-time imaging monitoring instrument, with zooming to a volume of interest with easy-to-use visualization via ImageJ, a tool familiar to most beamline users, is presented. The instrument relies on optimized data flow between the detector and processing machines and is implemented on commodity computers. The instrument has been developed at beamline 2-BM of the Advanced Photon Source, where the automatic lens changing mechanism for zooming is implemented with an Optique Peter microscope. Performance tests demonstrate the ability to process more than 3 GB of projection data per second and generate real-time 3D zooming with different magnification. These new capabilities are essential for new APS Upgrade instruments such as the projection microscope under development at beamline 32-ID. The efficacy of the proposed instrument was demonstrated during an in situ tomographic experiment on ice and gas hydrate formation in porous samples.

Collimator irradiation studies in the Argonne Advanced Photon Source at energy densities expected in next-generation storage ring light sources

The Advanced Photon Source (APS) team is building a fourth-generation storage ring (4GSR), replacing the present double-bend achromat lattice with a multibend achromat system thereby allowing the production of ultrabright x-ray beams. The new lattice enables a 2-order-of-magnitude reduction in horizontal beam emittance and a factor of two increase in beam current. The result is an electron beam of very high energy and power densities. Initial predictions suggest many common ultrahigh-vacuum-compatible materials struck by the full-intensity electron beam will be damaged. Two experimental beam abort studies have been conducted on collimator test pieces in the present APS SR to inform the design of a fully-functional machine protection system for APS 4GSR operations at 200 mA. A comprehensive suite of diagnostics was utilized during the studies. The diagnostics used in these experiments are not new, but employed in different ways to obtain unique data sets. With these sets now in hand, we are developing new numerical tools to guide collimator design using pelegant [M. Borland, elegant: A flexible SDDS-compliant code for accelerator simulation, Technical Report No. LS-287, Advanced Photon Source, 2000; Y. Wang and M. Borland, Implementation and performance of parallelized elegant, in Proceedings of the 2007 Particle Accelerator Conference, http://cern.ch/AccelConf/p07/PAPERS/THPAN095.PDF, pp. 3444--3446], mars [N. V. Mokhov and S. I. Striganov, Fermilab-conf-07/008-ad, AIP Conf. Proc. 896, 50 (2007)], and flash [B. Fryxell et al., flash: An adaptive mesh hydrodynamics code for modeling astrophysical thermonuclear flashes, Astrophys. J. Suppl. Ser. 131, 273 (2000); P. Tzeferacos et al., Laboratory evidence of dynamo amplification of magnetic fields in a turbulent plasma, Nat. Commun. 9, 591 (2018)].

A field programmable gate array-based timing and control system for the dynamic compression sector.

A field programmable gate array (FPGA)-based timing and trigger control system has been developed for the Dynamic Compression Sector (DCS) user facility located at the Advanced Photon Source (APS) at Argonne National Laboratory. The DCS is a first-of-its-kind capability dedicated to dynamic compression science. All components of the DCS laser shock station-x-ray choppers, single-shot shutter, internal laser triggers, and shot diagnostics-must be synchronized with respect to the arrival of x rays in the hutch. An FPGA synchronized to the APS storage ring radio frequency clock (352 MHz) generates trigger signals for each stage of the laser and x-ray shutter system with low jitter. The developed FPGA-based control system was the first system used to control the laser and the shutter system since its commissioning, and it has been developing since then to improve the timing jitter. The system is composed of a Zynq FPGA, a debug card, line drivers, and a power supply. The delay and offsets of the trigger signals can be adjusted by using a user-friendly graphical user interface with high precision. The details of the system architecture, timing requirements, firmware, and software implementation along with the performance evaluation are presented in this paper. The system offers low timing jitter (15.5 ps rms) with respect to the APS 352 MHz clock, suitable for the 100 ps (FWHM) x-ray bunch duration at the APS.

In Situ XAS Investigation of K4Fe(CN)6·xH2O and K3Fe(CN)6 Redox Activity in Solid-State Supercapacitors

We examined the redox activity of commercially obtained K4Fe(CN)6·xH2O and K3Fe(CN)6 incorporated in an asymmetric solid-state supercapacitors (SCs) using combined cyclic voltammetry and X-ray absorption spectroscopy (XAS) under in situ conditions. The cyclic voltammetry measurements were done at 10 mV s−1 between −2 and + 2 V while the XAS measurements were conducted in transmission mode at the Advanced Photon Source. The asymmetric SCs were constructed with one electrode containing activated carbon (AC) and another electrode containing a mixture of AC and K4Fe(CN)6·xH2O or K3Fe(CN)6 sandwiched between a PVDF/LiTFS membrane. We show that K4Fe(CN)6·xH2O is stable while Fe(III) in K3Fe(CN)6 is reduced to Fe(II) as a result of the electrode synthesis procedures. The complete reduction of Fe(III) to Fe(II) in K3Fe(CN)6 during the synthesis procedures is believed to be due to the interaction with lithium from the LiTFS salt and the formation of LiK3Fe(CN)6. Based on the energy shifts in the XANES data, about 50% of the Fe in both K4Fe(CN)6·xH2O and the reduced form of K3Fe(CN)6 is oxidized and reduced between Fe(III) and Fe(II) during electrochemical cycling between −2 and +2 V. The associated changes in the coordination distances and disorders of the first (Fe-C) and second (Fe-N) shells were also quantified and discussed.

Partnership for eXtreme Xtallography (PX2)—A state-of-the-art experimental facility for extreme-conditions crystallography: A case study of pressure-induced phase transition in natural ilvaite

Single-crystal x-ray diffraction (SCXRD) is an important tool to study the crystal structure and phase transitions of crystalline materials at elevated pressures. The Partnership for eXtreme Xtallography (PX2) program at the GSECARS 13-BM-C beamline of the Advanced Photon Source aims to provide state-of-the-art experimental capabilities to determine the crystal structures of materials under extreme conditions using SCXRD. PX2 provides a focused x-ray beam (12 × 18 µm2) at a monochromatic energy of 28.6 keV. High-pressure SCXRD experiments are performed with a six-circle diffractometer and a Pilatus3 photon-counting detector, facilitated by a membrane system for remote pressure control and an online ruby fluorescence system for pressure determination. The efficient, high-quality crystal structure determination at PX2 is exemplified by a study of pressure-induced phase transitions in natural ilvaite [CaFe2+2Fe3+Si2O7O(OH), P21/a space group]. Two phase transitions are observed at high pressure. The SCXRD data confirm the already-known ilvaite-I (P21/a) → ilvaite-II (Pnam) transformation at 0.4(1) GPa, and, a further phase transition is found to occur at 22.8(2) GPa where ilvaite-II transforms into ilvaite-III (P21/a). The crystal structure of the ilvaite-III is solved and refined in the P21/a space group. In addition to the ilvaite-I → ilvaite-II → ilvaite-III phase transitions, two minor structural modifications are observed as discontinuities in the evolution of the FeO6 polyhedral geometries with pressure, which are likely associated with magnetic transitions.

Fast automated energy changes at synchrotron radiation beamlines equipped with transfocator or focusing mirrors.

Algorithms and procedures to fully automate retuning of synchrotron radiation beamlines over wide energy ranges are discussed. The discussion is based on the implementation at the National Institute of General Medical Sciences and the National Cancer Institute Structural Biology Facility at the Advanced Photon Source. When a user selects a new beamline energy, software synchronously controls the beamline monochromator and undulator to maintain the X-ray beam flux after the monochromator, preserves beam attenuation by determining a new set of attenuator foils, changes, as needed, mirror reflecting stripes and the undulator harmonic, preserves beam focal distance of compound refractive lens focusing by changing the In/Out combination of lenses in the transfocator, and, finally, restores beam position at the sample by on-the-fly scanning of either the Kirkpatrick-Baez mirror angles or the transfocator up/down and inboard/outboard positions. The sample is protected from radiation damage by automatically moving it out of the beam during the energy change and optimization.

Diffuse X-ray scattering from polished silicon: application of the distorted wave Born approximation.

Measured diffuse X-ray scattering data for a `smooth' as well as for a `rough' silicon sample were fit to theoretical expressions within the distorted wave Born approximation (DWBA). Data for the power spectral density (PSD) for both samples were also obtained by means of atomic force microscopy and optical interferometry. The Fourier transforms of trial correlation functions were fit to the PSD data and then applied to the DWBA formalism. The net correlation functions needed to fit the PSD data for each sample comprised the sum of two terms with different cutoff lengths and different self-affine fractal exponents. At zero distance these correlation functions added up to yield net values of σ2 = (2)2 and (71)2 Å2 for the smooth and rough samples, respectively. X-ray scattering data were obtained at beamline 1-BM of the Advanced Photon Source. Data and fits at values of qz = 0.05 and 0.10 Å-1 for the smooth sample are reported. Good fits for the smooth sample were obtained at both qz values simultaneously, that is, identical fitting parameters were applied at both values of qz. The smooth sample also exhibited weak Yoneda wings and a clear distinction between the strong specular scattering and the weak diffuse scattering. Data for the rough sample were qualitatively different and exhibited very weak scattering at the specular condition in contrast to extremely large Yoneda wings. Fits for the rough sample are reported for qz = 0.04, 0.05, and 0.06 Å-1. Although the large Yoneda wings could be fit quite well in both position and amplitude, scattering near the specular condition could not be equally well fit by applying the same fitting parameters at all values of qz. Albeit imperfect, best-fitting results at the specular condition were obtained by invoking only diffuse scattering, that is, without including a separate theoretical expression for specular scattering.

Microstructure and energy dispersive diffraction reconstruction of 3D patterns of crystallographic texture in a shark centrum.

Purpose: Tomography using diffracted x-rays produces reconstructions mapping quantities such as crystal lattice parameter(s), crystallite size, and crystallographic texture, information quite different from that obtained with absorption or phase contrast. Diffraction tomography is used to map an entire blue shark centrum with its double cone structure (corpora calcerea) and intermedialia (four wedges). Approach: Energy dispersive diffraction (EDD) and polychromatic synchrotron x-radiation at 6-BM-B, the Advanced Photon Source, were used. Different, properly oriented Bragg planes diffract different x-ray energies; these intensities are measured by one of ten energy-sensitive detectors. A pencil beam defines the irradiated volume, and a collimator before each energy-sensitive detector selects which portion of the irradiated column is sampled at any one time. Translating the specimen along , and axes produces a 3D map. Results: We report 3D maps of the integrated intensity of several bioapatite reflections from the mineralized cartilage centrum of a blue shark. The axis reflection's integrated intensities and those of a reflection with no axis component reveal that the cone wall's bioapatite is oriented with its axes lateral, i.e., perpendicular to the backbone's axis, and that the wedges' bioapatite is oriented with its axes axial. Absorption microcomputed tomography (laboratory and synchrotron) and x-ray excited x-ray fluorescence maps provide higher resolution views. Conclusion: The bioapatite in the cone walls and wedges is oriented to resist lateral and axial deflections, respectively. Mineralized tissue samples can be mapped in 3D with EDD tomography and subsequently studied by destructive methods.

Observations on the deformation of metal microspheres in shock-driven polymer flows

Solid particles can be fragmented by a fast-moving fluid if their velocity difference is great enough, such as during the atmospheric entry of meteoroids or the shock compression of engineered particulate composites. The extent of particle deformation and breakup in such systems is poorly understood because the necessary extreme conditions make observation difficult and data scarce. To meet this need, experiments combining ultrafast synchrotron-based radiography with plate impact loading were performed at the dynamic compression sector at the advanced photon source. Metal microspheres of several densities and strengths (Au, Ta, and W) were placed inside a polymer matrix. A planar shock wave was then produced in the polymer by the impact of a gun-launched flyer plate. X-ray images of the resulting flow were collected at ∼150 ns intervals. These images document the progression of particle deformation across a range of flow conditions and particle materials. They show that the extent of deformation is sensitive to the ratio of drag stress to particle strength. The deforming particle's shape is determined by the initial shock–particle interaction, fluid stagnation pressure, and vorticity, each acting on its own timescale. A set of scaling relationships is presented to capture these observations and enable comparison with prior hydrodynamic data. The result is a framework for predicting the conditions under which strong particles are severely deformed by a shock-driven flow.

User capabilities at the GM/CA@APS Structural Biology Facility at the Advanced Photon Source

The General Medical Sciences and Cancer Institutes’ structural biology facility at the APS (GM/CA@APS) operates a National User Facility for crystallographic structure determination of biological macromolecules, with an emphasis on challenging, high-impact projects. The facility includes canted-undulator beamlines, 23ID-B and 23ID-D, that provide stable, intense X-ray beams of user-selectable size down to 5-micron, an intuitive user interface for experiment control, and an automated data processing pipeline.

Quantification of mineral reactivity using machine learning interpretation of micro-XRF data

Accurate characterizations of mineral reactivity require mapping of spatial heterogeneity, and quantifications of mineral abundances, elemental content, and mineral accessibility. Reactive transport models require such information at the grain-scale to accurately simulate coupled processes of mineral reactions, aqueous solution speciation, and mass transport. In this work, millimeter-scale mineral maps are generated using a neural network approach for 2D mineral mapping based on synchrotron micro x-ray fluorescence (μXRF) data. The approach is called Synchrotron-based Machine learning Approach for RasTer (SMART) mapping, which reads μXRF scans and provides mineral maps of the same size and resolution. The SMART mineral classifier is trained on coupled μXRF and micro-x-ray diffraction (μXRD) data, which is what distinguishes it from existing mapping tools. Here, the SMART classifier was applied to μXRF scans of various sedimentary rock samples including consolidated shales from the Eagle Ford (EFS1), Green River (GRS1), Haynesville (HS1), and New Albany (NAS1) formations and a syntaxial vein from the Upper Wolfcamp formation. The data were obtained using an x-ray microprobe at beamline 13-ID-E at the Advanced Photon Sources. Individual mineral maps generated by the SMART classifier well-captured distributions of both dominant and minor phases in the shale rocks and revealed EFS1 and GRS1 to be carbonate rich shales, and NAS1 and HS1 to be sulfide rich shales. The EFS1 was further characterized for its trace mineral abundances, grain sizes, trace element composition, and accessibility. Approximately 4.4 wt% of the rock matrix were found to be pyrite, with a median grain size of 3.17 μm in diameter and 62% of the grains predicted to be smaller than 4 μm. Quantifications of trace elements in pyrite revealed zinc concentrations up to 4.2 wt%, along with minor copper and arsenic copresence. Mineral accessibility was examined by contact with other phases and was quantified using a new type of image we are calling an adjacency map. Adjacency analyses revealed that of the total pyrite surface present in the EFS1, 28% is in contact with calcite. The adjacency maps are useful for quantifying the likelihood that a mineral could be exposed to fluids after dissolution of a contacting reactive phase like calcite. Lastly, pooling data from different samples was demonstrated by training a classifier using two sets of coupled μXRF-μXRD data. This classifier yielded an overall accuracy of >96%, demonstrating that data pooling is a promising approach for applications to a wide suite of rock samples of different origin, size, and thickness.

Time-Resolved Geometric Feature Tracking Elucidates Laser-Induced Keyhole Dynamics

During laser melting of metals, localized metal evaporation resulting in the formation of a keyhole shaped cavity can occur if processing conditions are chosen with high power density. An unstable keyhole can have deleterious effects in certain applications (e.g., laser powder bed fusion) as it increases the likelihood of producing defects such as porosity. In this work, we propose a pipeline that enables complete segmentation and extraction of various geometric features in keyholing conditions. In situ synchrotron high-speed X-ray visualization at the Advanced Photon Source provides large datasets of experimental images with a high spatio-temporal resolution across a range of laser parameters for Ti-6Al-4V. Computer vision image processing techniques were used to extract time-resolved quantitative geometric features (e.g., depth, width, front wall angle) throughout keyhole evolution which were subsequently analyzed to understand the relationship between the variation of local keyhole geometry and processing conditions. This analysis is the first to employ a data-driven approach to further our understanding of the keyholing process regime.

In situ x-ray diffraction of high density polyethylene during dynamic drive: Polymer chain compression and decomposition

Polymers are widely implemented materials often used for safety and security in our daily lives. However, we do not have a thorough understanding of the phase transformations of these materials when exposed to extreme condition, high strain rate events. To study polymers in these severe environments, we performed plate impact experiments that impart a one-dimensional shockwave, at high pressures and temperatures, to observe the materials response. Generally, velocimetry is the experimental diagnostic used to capture the movement of high velocity interfaces to then calculate the mechanical variables associated with shock compression. However, when a material undergoes a phase transition, such as between two crystalline phases or melting to decomposition during shock compression, velocimetry does not explicitly indicate what structural change occurred. At the Dynamic Compression Sector at the Advanced Photon Source, gas gun driven compression has been paired with x-ray diffraction, providing the ability to study both the shock parameters and structural changes concurrently. We explored high density polyethylene (HDPE) both on its reactants Hugoniot (<10.12 GPa) and within its transition region (24.3 GPa) where HDPE is hypothesized to decompose from reactants to products. With x-ray diffraction, we observed both polymer chain compression and crystal structure reorientation from orthorhombic to monoclinic above 6 GPa as well as either a possible phase change or chemical decomposition at 24.3 GPa. With these experiments, we were able to determine the crystalline and amorphous Hugoniot loci at pressures below the polymer transition region.

Experimental Investigation of Mercury's Magma Ocean Viscosity: Implications for the Formation of Mercury's Cumulate Mantle, Its Subsequent Dynamic Evolution, and Crustal Petrogenesis

AbstractMercury has a compositionally diverse surface that was produced by different periods of igneous activity suggesting heterogeneous mantle sources. Understanding the structure of Mercury's mantle formed during the planet's magma ocean stage could help in developing a petrologic model for Mercury, and thus, understanding its dynamic history in the context of crustal petrogenesis. We present results of falling sphere viscometry experiments on late‐stage Mercurian magma ocean analogue compositions conducted at the Advanced Photon Source, beamline 16‐BM‐B, Argonne National Laboratory. Owing to the presence of sulfur on the surface of Mercury, two compositions were tested, one with sulfur and one without. The liquids have viscosities of 0.6–3.9 (sulfur‐bearing; 2.6–6.2 GPa) and 0.6–10.9 Pa·s (sulfur‐free; 3.2–4.5 GPa) at temperatures of 1600–2000°C. We present new viscosity models that enable extrapolation beyond the experimental conditions and evaluate grain growth and the potential for crystal entrainment in a cooling, convecting magma ocean. We consider scenarios with and without a graphite flotation crust, suggesting endmember outcomes for Mercury's mantle structure. With a graphite flotation crust, crystallization of the mantle would be fractional with negatively buoyant minerals sinking to form a stratified cumulate pile according to the crystallization sequence. Without a flotation crust, crystals may remain entrained in the convecting liquid during solidification, producing a homogeneous mantle. In the context of these endmember models, the surface could result from dynamical stirring or mixing of a mantle that was initially heterogeneous, or potentially from different extents of melting of a homogeneous mantle.

Intact archeological human bones and age at death studied with transmission x‐ray diffraction and small angle x‐ray scattering

AbstractHigh‐energy, wide‐angle x‐ray scattering (WAXS, x‐ray diffraction) and small‐angle x‐ray scattering (SAXS) were used to study intact human second metacarpal bones (mc2) from two UK archeological sites. A novel method correcting for irregular mass distribution was applied in these transmission geometry experiments done at beamline 1‐ID of the Advanced Photon Source. The authors asked whether there were age‐at‐death‐related changes in carbonated apatite (cAp) lattice parameters and whether SAXS could detect collagen D‐period peaks in the archeological mc2. For each of the two sites, Ancaster and Wharram Percy in England, six female mc2s were studied; for each site, two were from each of three age‐at‐death cohorts (young, 18–29 years; middle, 30–49 years; old ≥50 years) along with a modern control mc2. The Rietveld method was applied to the WAXS patterns to provide precise lattice parameter values. The cAp lattice parameters did not correlate with age‐at‐death estimated from dental wear. From WAXS and the 00.2 diffraction peak widths, four archeological mc2s possessed coherently scattering domain lengths (crystallite c‐axis sizes) that matched that of the modern mc2; SAXS revealed the same four archeological mc2 had D‐period peak intensities equivalent to that of the modern mc2. The other eight archeological mc2s had significantly larger crystallite sizes (than the modern mc2) and weak or absent D‐period peaks, differences attributed to diagenetic changes. Based on these data, the authors suggest that WAXS 00.2 peak width and SAXS D‐period peak intensity can be used with intact bones to select those likely to retain largely unaltered tissue nanostructure, which might be required for other analyses. Taken as a whole, the results suggest detecting age‐related deterioration in nanostructural features may be difficult in bone showing significant bioerosion.