1 / 40

High-Energy X-ray* Studies of Real Materials under Real Conditions and in Real Time Fermilab Colloquium Series May 11,

High-Energy X-ray* Studies of Real Materials under Real Conditions and in Real Time Fermilab Colloquium Series May 11, 2011. Jonathan Almer Advanced Photon Source Argonne National Laboratory. * From perspective of a materials scientist NOT a high-energy physicist!. Acknowledgements. APS

orrin
Télécharger la présentation

High-Energy X-ray* Studies of Real Materials under Real Conditions and in Real Time Fermilab Colloquium Series May 11,

An Image/Link below is provided (as is) to download presentation Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author. Content is provided to you AS IS for your information and personal use only. Download presentation by click this link. While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server. During download, if you can't get a presentation, the file might be deleted by the publisher.

E N D

Presentation Transcript

  1. High-Energy X-ray* Studies of Real Materials under Real Conditions and in Real TimeFermilab Colloquium SeriesMay 11, 2011 Jonathan Almer Advanced Photon Source Argonne National Laboratory * From perspective of a materials scientist NOT a high-energy physicist!

  2. Acknowledgements • APS • Ulrich Lienert – HEDM program • SarvjitShastri – High-energy optics • Francesco Decarlo – High-energy tomography • Nuclear Materials: Meimei Li (ANL) and Mark Daymond (Queens U) • Nano-synthesis: Bo Iversen (Aarhus U) and Y. Sun (ANL-CNM) • Biomechanics: Stuart Stock and David Dunand (Northwestern U) • Department of Energy, Office of Basic Energy Science Advanced Photon Source

  3. Outline • X-ray techniques: from beginning to the synchrotron • Size and penetration of selected probes • APS Upgrade and high-energy x-ray probes • HE Sources • HE Optics • End Stations • Scientific scope overview and examples • Lightweight materials • Nuclear energy • Batteries / nanoscale materials • Geoscience (carbon sequestration) • Biological materials • Conclusions and outlook Advanced Photon Source Upgrade (APS-U) project

  4. X-ray Vision: The Beginning The first nobel prize in physics (1901) was awarded to Roentgen for the ‘discovery of the remarkable rays subsequently named after him” First radiograph (Mrs. Roentgen) • In subsequent decades the three main uses of x-rays were established: • Imaging (electron density and phase contrast) • Spectroscopy (inelastic scattering - chemical and electronic speciation) • Scattering (elastic scattering - atomic structure) • These modes remain the three ‘pillars’ of x-ray science.

  5. X-ray diffraction (elastic scattering) * Constructive interference between x-rays and atomic spacing (electrons) * Works b/c x-ray wavelength is same order as atomic spacing d

  6. 70 possible x-ray ports • 35 ID, 35 BM • ~43 currently operating • Beam time available through peer reviewed general user proposals • No charge • Operates 5000 hrs/year • Users from around the world • Over 3000 per year • Multidisciplinary Advanced Photon Source • 1-ID (XOR) • High energy x-rays

  7. Why Use a Synchrotron? • Tunable X-ray energy • Large variety of specialized instruments • Much higher intensities than lab sources • 9 orders of magnitude higher brilliance! • Faster experiments • More sensitivity • Small beams • Increased coherence • More penetration • Why not use a synchrotron? • Not portable • Can be tough to get beam time • Small beams • Beam damage

  8. Resolution & penetration depth of selected techniques ‘Wide- angle’ scattering ‘Small-angle’ scattering HE Synchrotron (E = 80 keV) focusing optics USAXS PDF Spatial resolution (1-d or 2-d) 0.1nm 1nm 10nm 100nm 1mm 10mm 100mm 1mm 10mm Surface 1-100nm 1 mm 10 mm 100 mm 1 mm 10 mm 10 cm TEM SEM/Auger Optical Grazing Incidence, Reflectivity Synchrotron (E =10 keV) Focusing optics Penetration depth Neutron Diffraction

  9. APS upgrade and high-energy X-rays APS built ~20 years ago Requesting 350M upgrade to DOE with themes: Real materials under real conditions in real time Understanding hierarchical structures through imaging -50 proposals were ranked by scientific advisory board (top priority shown) Advanced Photon Source

  10. High Energy X-ray Undulator Sources • Request canted undulators & long straight section: • superconducting (fixed period w/3rd harmonic ~70 keV) • revolver PM (2.3 & 2.5 cm) for continuous coverage • Heat loads more tolerable with short-period devices • 1.6cm SCU 300kW/mrad2 at min gap 9.5mm Specialized undulators will increase brilliance by 5-10x at high energies, providing the highest brilliance at 100keV worldwide Advanced Photon Source Upgrade (APS-U) project

  11. High Energy X-ray Optics • Mono2: Bent double-Laue geometry • Continuously tunable from 40-140 keV • Bending on-rowland conditions results in 10x increase in flux w/o divergence increase • Source-preservation demonstrated Combining HR mono and focusing optics (sawtooth lens as virtual parabolic lens) Laue optics preserve brilliance enabling mm-level focusing at 100 keV and flexibility to combine optical elements for highest q-resolution. Advanced Photon Source Upgrade (APS-U) Project

  12. Polycrystal Techniques for microstructural mapping • Absorption or phase tomography • Full field 2D image (mm^2) of direct beam • Absorption contrast (near) to phase contrast (far) by changing sample-detector • Take image and rotate M times (M images) • Reconstruct ->3D volume • Diffraction tomography (High Energy Diffraction Microscopy- HEDM) • Thin beam (~ 1mm x 5um) • Take image at N different distances and rotate Mtimes (NxMimages) • Reconstruct distinct spots on detector - >2D diffraction contrast • Move sample vertically to build up 3D sample volume • Semi-transparent beamstop for simultaneous AT 1-3mm Rotation & loading axis Bulk samples (mm’s) Incident beam E= 50-80 keV Scattering angles <10 deg Advanced Photon Source

  13. Combining techniques for in situ studies W beamstop (0.5-2 mm dia) Irradiated specimen loaded in a shielded containment Beam from optimized HE undulator & monochromator E ~ 50-100 keV SAXS CCD 1×1k, 22.5 mm pixels Translating full field imaging detector 2×2k pixels, 1 m resolution Quad-paneled array for WAXS/SAXS four 22k detectors, each 4040 cm (active) MTS mechanical test frame Ion chamber Defining slits Guard slits • In situ measurements of bulk, irradiated materials under thermo-mechanical loading • Simultaneous WAXS/SAXS and full-field imaging • WAXS: lattice strain, texture, phases • SAXS: nanoscale voids, bubbles, particles • Imaging: microsize cracks, porosity • 2D detector array for long sample-detector distance • High-resolution data (small beams) • Ability to use large beam (imaging) w/sufficient WAXS resolution for combined studies • improved signal-to-background ratio

  14. SOFC (battery) • Controlled porosity • Thermal mismatch • Chemical durability • Mechanical integrity e- e- H2O & CO2 O= H2 & CO O2 Porous cathode Porous Anode Dense electrolyte Scientific scope • New lightweight composites • Optimizing metal sheet forming • Energy: efficiency • High specific strength materials • Thermal barrier coatings for engine efficiency • Energy: production/storage • Batteries and fuel cells • Fossil fuel extraction (high-pressure oil/coal/gas properties) • Nuclear materials • damage tolerant materials for new reactors • degradation of existing materials (corrosion/void formation/etc) • Energy: environment • CO2 sequestration (fluid movement in rock/capillary trapping) • Biology • Response of bone and teeth to applied load, environment, dose • High-energy scattering and imaging: • Penetrating in situ probes -> real conditions • High flux -> real time • High q-resolution -> real/complex materials Advanced Photon Source

  15. High Energy Tomography: Mechanical Properties of MMCs real size samplesin real operational conditions Metal Matrix Composite Materials transportation technology, new material, industrial applications 3D Analysis of Probability of Cracking as a Function of Particle Size and Aspect Ratio Acta Mater. 58 (18), 6194-6205 (2010) Use of new advanced weight-saving alloys in vehicles is limited by the inability to determine the mechanical properties under load, to monitor creep/fatigue interaction, crack formation and sample expansion during temperature cycles and the evolution of defects during loading and corrosion of real size samples.

  16. Combining HE tomography with diffraction microscopy • ‘Near field’ diffraction - Non-destructive EBSD –type info. Raw image (shock-deformed copper) Attenuated direct beam Carnegie Near-field orientation map Tomographic reconstruction Mellon MRSEC Advanced Photon Source (U. Lienert, A. Khounsary and P. Kenesei)

  17. HEDM reveals in-situ microstructural evolution vs temperature • Annealing response Misorientation Carnegie Mellon MRSEC • orientation changes • located at boundaries • * Information is being used to drive and test computational materials science predictions • 4 degcolor scale • 2 deg boundaries

  18. SOFC (battery) • Controlled porosity • Thermal mismatch • Chemical durability • Mechanical integrity e- e- H2O & CO2 O= H2 & CO O2 Porous cathode Porous Anode Dense electrolyte Scientific scope • New lightweight composites • Optimizing metal sheet forming • Energy: efficiency • High specific strength materials • Thermal barrier coatings for engine efficiency • Energy: production/storage • Batteries, fuel cells, material discovery • Fossil fuel extraction (high-pressure oil/coal/gas properties) • Nuclear materials • damage tolerant materials for new reactors • degradation of existing materials (corrosion/void formation/etc) • Energy: environment • CO2 sequestration (fluid movement in rock/capillary trapping) • Biology • Response of bone and teeth to applied load, environment, dose • High-energy scattering and imaging: • Penetrating in situ probes -> real conditions • High flux -> real time • High q-resolution -> real/complex materials Advanced Photon Source

  19. Combined Approaches Towards a Hierarchical Understanding of Battery Materials Hard x-ray tools can probe different length scales Challenges in energy storage span multiple length scales Rmc methods allow combined analysis of variety of data Impacts spanning many strategic areas In situ EXAFS Li+ insertion ~ nm • Insight into challenges in battery technology • Infrastructure for research in electrical energy storage • New RMC computational algorithms capable of addressing large systems • A versatile experimental+analytical tool applicable to diverse challenges in materials science PDF Reverse Monte Carlomodeling of ALL data SAXS Grain fracturing ~ μm Imaging Li+ diffusion ~ mm +Echem LDRD: Hard X-ray Sciences Initiative, 2010-074-R1

  20. In-situ synthesis of nano-particles for Li-ion batteries Advanced Photon Source

  21. In-situ synthesis of LiCoO2nano-particles for Li-ion batteries SAXS WAXS Precursor CoOOH Time (s) suppression of steel suppression of steel Intermediate Co3O4 Final LiCoO2 Intermediate disappears. Channels

  22. ? Second Generation of nanoparticles: Shape Control First Generation of nanoparticles: Size Decrease Application? Third Generation? 2009+ 2000 ? ? ? ? ? ? ? In situ tools to control nanoparticle formation • Joint effort between APS (characterization) and ANL-Center of Nanoscale Materials (synthesis) • Goal: control shape and size of nanoparticles for functional application (catalysis, photonics, etc) • Needed: real-time probe of morphology during nucleation and growth in solution Current limitations - impurity - low reproducibility - wide distribution Xia, Sun, Yang, Murphy, Mirkin, et al.

  23. Probing nanophase evolution at semiconductor interface • Nucleation and growth of anisotropic Ag nanoplates on GaAs distinguished (1s resolution) • Additional nanoparticles of Ag7NO11 formed; x-ray generated oxidation; x-ray nano-patterning application? • Future: real-time feedback and msec resolutions; tweak process variables (eg. temp) to produce desired properties (sizes, morphology, etc) Advanced Photon Source Y. Sun et al, Nanoletters10 (2010), 3747-3753.

  24. SOFC (battery) • Controlled porosity • Thermal mismatch • Chemical durability • Mechanical integrity e- e- H2O & CO2 O= H2 & CO O2 Porous cathode Porous Anode Dense electrolyte Scientific scope • New lightweight composites • Optimizing metal sheet forming • Energy: efficiency • High specific strength materials • Thermal barrier coatings for engine efficiency • Energy: production/storage • Batteries, fuel cells, material discovery • Fossil fuel extraction (high-pressure oil/coal/gas properties) • Nuclear materials • damage tolerant materials for new reactors • degradation of existing materials (corrosion/void formation/etc) • Energy: environment • CO2 sequestration (fluid movement in rock/capillary trapping) • Biology • Response of bone and teeth to applied load, environment, dose • High-energy scattering and imaging: • Penetrating in situ probes -> real conditions • High flux -> real time • High q-resolution -> real/complex materials Advanced Photon Source

  25. Fiber-matrix interactions in CMCs (Faber) Hydride formation and growth at stress concentrations (Daymond and Motta 2008-2010) Tomography to study intergranular stress corrosion cracking (King et al 2008) Irradiated materials: scientific challenges • Irradiation causes serious degradation of mechanical properties • Delayed hydride formation & cracking in Zr-alloys • Stress-corrosion cracking • Predictions of materials long-term performance and development of high-performance, radiation-resistance materials in nuclear environments requires a mechanistic understanding • ‘Radiation resistant’ materials e.g. ODS steels • CMCs for higher temperature operation/efficiency • Desire microstructural-level understanding of deformation and fracture mechanisms and phase stability under stress and temperatures

  26. Integrated approach of theory, modeling and experiment B. Wirth et al, J. Nucl. Mater. 329-333 (2004) 103

  27. Reactors World Wide Nuclear materials: understanding Zr-hydrides • Zircaloy Fuel Cladding • Pressurized or unpressurizedH2O coolant • Temperatures range from 100 to greater than 300oC Corrosion reaction at Zr surface: Zr + 2H2O  ZrO2 + 4H Need to measure hydrogen concentrations at ~100ppm corresponding to hydride phase fractions below 1% -> high flux!

  28. Hydride Diffraction Pattern 2D pattern Integrate segments • Single peak fits (GSAS and Matlab) • Diffraction directly measures the elastic strain in the lattice – internal strain gage • Plastic behavior only inferred through load transfer behavior • For comparison to elastic strain in Finite Element (FE) calculations, a weighted average of single diffraction peaks was used (multiplicity, texture, etc) MR Daymond, Journal of Applied Physics 96 (2004) 4263

  29. 50 mm2 spot size 20 mm2 spot size 200 mm HE Diffraction: Hydride Strain Mapping 30% Overload (relative to hydride growth) eyy – ZrHx {111} Y-Axis (eyy) X-Axis (exx)

  30. Hydride Fracture 30% Overload relative to hydride growth load 20% Overload relative to hydride growth load eyy ZrHx {111} eyy Zr (Avg) • At a 20% overload, hydride is intact at the notch • At a 30% overload, the notch tip hydride has fractured transferring load to the surrounding matrix • Data combined with FE analysis used to derive critical hydride size for fracture (~4um) Kerr et al, J. Nuc. Mat. (2008)

  31. SOFC (battery) • Controlled porosity • Thermal mismatch • Chemical durability • Mechanical integrity e- e- H2O & CO2 O= H2 & CO O2 Porous cathode Porous Anode Dense electrolyte Scientific scope • New lightweight composites • Optimizing metal sheet forming • Energy: efficiency • High specific strength materials • Thermal barrier coatings for engine efficiency • Energy: production/storage • Batteries and fuel cells • Fossil fuel extraction (high-pressure oil/coal/gas properties) • Nuclear materials • damage tolerant materials for new reactors • degradation of existing materials (corrosion/void formation/etc) • Energy: environment • CO2 sequestration (fluid movement in rock/capillary trapping) • Biology • Response of bone and teeth to applied load, environment, dose • High-energy scattering and imaging: • Penetrating in situ probes -> real conditions • High flux -> real time • High q-resolution -> real/complex materials Advanced Photon Source

  32. Thermal expansion cracking in rocks in-situ studies of real size samples Carbon sequestration, mine and oil exploration The pores distribution of large samples are now only possible in static conditions and after a lengthy and disruptive sample preparation process. µm 4.5 4.0 3.5 3.0 2.5 1.5 1.0 0.5 2 cm 100 um 100 um 200 C 395 C Nature Vol. 459 18 June 2009 • Understanding thermal cracking in fine-grained granite: increase in porosity with temperature facilitates the percolation of fluid through the rock. Advanced Photon Source Upgrade (APS-U) project

  33. SOFC (battery) • Controlled porosity • Thermal mismatch • Chemical durability • Mechanical integrity e- e- H2O & CO2 O= H2 & CO O2 Porous cathode Porous Anode Dense electrolyte Scientific scope • New lightweight composites • Optimizing metal sheet forming • Energy: efficiency • High specific strength materials • Thermal barrier coatings for engine efficiency • Energy: production/storage • Batteries and fuel cells • Fossil fuel extraction (high-pressure oil/coal/gas properties) • Nuclear materials • damage tolerant materials for new reactors • degradation of existing materials (corrosion/void formation/etc) • Energy: environment • CO2 sequestration (fluid movement in rock/capillary trapping) • Biology • Response of bone and teeth to applied load, environment, dose • High-energy scattering and imaging: • Penetrating in situ probes -> real conditions • High flux -> real time • High q-resolution -> real/complex materials Advanced Photon Source

  34. Mineralized Tissue and Implants • Bone and dentin have a complex hierarchical structure – composite of mineral (calcium hydroxyapatite), organic protein and water • Macroscopic mechanical properties well studied; properties at the basic level not well understood • Fundamental properties needed for better restoration materials, formulate more accurate models HAP lattice planes diffract SAXS pattern ~67 nm WAXS pattern • High-energy X-ray scattering gives distinct information from the mineral, collagen fibril and implant phases.

  35. Nanoscale model and experimental validation Model Setup Phase response vs load 67 nm ESAXS=19.8GPa EWAXS=39.6GPa • Elastic Properties of Pure Phases: • HAP: E=114 GPa, ν=0.28 • Collagen: E=1 GPa, ν=0.25 • Volume Fraction of HAP: 35% • Dashed lines are simulation results Interstitial space spring HAP collagen L R

  36. Systematic studies have shown dose threshold of ~10kGray (Cancer therapy 5-60 Gray, sterilization 20-100kG) Creep behavior Experiment Simulation Low dose Perfect bonding between HAP and collagen Fibril -1.9 με/min HAP -0.8 με/min High dose Delamination at HAP-collagen interface Fibril HAP

  37. Bone Implant – highest level of hierarchy HAP Strain Distribution Structure screw head implant boundary mapping boundary implant bone • Bone: bovine femur • Screw head: solid cp-3 Ti • Implant: porous cp-1 Ti These studies will focus on interface between implant and bone, to better understand load transfer / implant effectiveness.

  38. Summary • High-energy x-ray techniques provide new insights into complex systems, with particular impact on energy research • Irradiated materials • Batteries/fuel cells • Energy efficiency • Biomechanics • Trend is to combine techniques: High-energy SAXS/WAXS/Imaging • Access a range of length scales (sub-nm to mm) using the same probe, msecresolution • Non-destructive • Microstructural evolution in extreme environments • APS upgrade will provide the brightest source of high-energy x-rays worldwide, allowing us to push spatio-temporal resolution limits. Advanced Photon Source

  39. Some common technical challenges / opportunities • Detectors • Efficient at E>50keV w/good resolution (e.g.structured scintillators) • Readout >=1kHz & >=Mpix • Energy discrimination • In-situ environment ‘centers’ • Capacity to follow processes is often limited by ability to simulate service/ processing conditions • Combined with penetrating x-rays: allow complex development / real conditions • Intermittent use for long-time processes (e.g. creep) • Unite with advanced characterization tools • Analysis & visualization of multi-dimensional datasets • Efficient data reduction • Real time feedback • Interface with materials modeling community Advanced Photon Source

  40. Energy-sensitive detectors for imaging + scattering Energy-discriminating detectors (chemistry+structure) • Triple phase boundaries in SOFCs • SEI in batteries XANES full-field imaging Rau et al, Nuc. Inst. Meth B (2003), 200 Current R&D efforts : CdZnTe sensors Advanced Photon Source

More Related