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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.

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Presentation on theme: "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."— Presentation transcript:

1 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!

2 Acknowledgements  APS –Ulrich Lienert – HEDM program –Sarvjit Shastri – 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 2

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 3 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 6 1-ID (XOR) High energy x-rays 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

7 7  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 Why Use a Synchrotron?

8 Resolution & penetration depth of selected techniques Surface 1-100nm 1  m 10  m 100  m 1 mm 10 mm 10 cm 1nm10nm100nm1m1m1mm10  m100  m10mm TEM SEM/Auger Optical Penetration depth Spatial resolution (1-d or 2-d) Synchrotron (E =10 keV) Neutron Diffraction Grazing Incidence, Reflectivity Focusing optics 0.1nm HE Synchrotron (E = 80 keV) focusing optics PDF ‘Wide- angle’ scattering ‘Small-angle’ scattering USAXS

9 APS upgrade and high-energy X-rays Advanced Photon Source 9 CDRTitlePanelPriority 4.2.2SPX Hard X-ray - Diffraction & Imaging1A SPX Hard X-ray - Spectroscopy1A Wide-Field Imaging Beamline4A High-Energy Tomography4A ,4.3.8In Situ Nanoprobe/Cryonanoprobe (NGN)4A Resonant Inelastic X-ray Scattering (MERIX)3A High-Energy Diffraction2A Magnetic Spectroscopy3A XIS - Tunable ID Beamlines2A Micro and 3D Diffraction2A Cryo Sample Preparation Facility5A Enhanced SAXS/WAXS5A Microfocus MX Beamline5A Enhanced Pump/Probe for Physical Sciences1A Enhanced Time-Resolved MX Beamline5A1 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)

10 High Energy X-ray Undulator Sources Advanced Photon Source Upgrade (APS-U) project 10 Request canted undulators & long straight section: (i)superconducting (fixed period w/3 rd harmonic ~70 keV) (ii)revolver PM (2.3 & 2.5 cm) for continuous coverage Heat loads more tolerable with short- period devices 1.6cm SCU 300kW/mrad 2 at min gap 9.5mm Specialized undulators will increase brilliance by 5-10x at high energies, providing the highest brilliance at 100keV worldwide

11 High Energy X-ray Optics Advanced Photon Source Upgrade (APS-U) Project 11 Mono2: Bent double-Laue geometry Continuously tunable from 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  m-level focusing at 100 keV and flexibility to combine optical elements for highest q-resolution.

12 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 M times (NxM images) –Reconstruct distinct spots on detector - >2D diffraction contrast –Move sample vertically to build up 3D sample volume –Semi-transparent beamstop for simultaneous AT Advanced Photon Source 12 Incident beam E= keV Scattering angles <10 deg Polycrystal 1-3mm Bulk samples (mm’s) Rotation & loading axis

13  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 Combining techniques for in situ studies W beamstop (0.5-2 mm dia) Translating full field imaging detector 2×2k pixels, 1  m resolution Ion chamber Guard slits Beam from optimized HE undulator & monochromator E ~ keV Defining slits Quad-paneled array for WAXS/SAXS four 2  2k detectors, each 40  40 cm (active) MTS mechanical test frame SAXS CCD 1×1k, 22.5  m pixels Irradiated specimen loaded in a shielded containment

14 Scientific scope  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 –CO 2 sequestration (fluid movement in rock/capillary trapping)  Biology –Response of bone and teeth to applied load, environment, dose Advanced Photon Source 14 Porous Anode Porous cathode H 2 & CO O2O2 e-e- H 2 O & CO 2 e-e- O=O= Controlled porosity Thermal mismatch Chemical durability Mechanical integrity Dense electrolyte SOFC (battery) New lightweight composites Optimizing metal sheet forming High-energy scattering and imaging: Penetrating in situ probes -> real conditions High flux -> real time High q-resolution -> real/complex materials

15 real size samples in real operational conditions 3D Analysis of Probability of Cracking as a Function of Particle Size and Aspect Ratio Metal Matrix Composite Materials transportation technology, new material, industrial applications Acta Mater. 58 (18), (2010) High Energy Tomography: Mechanical Properties of MMCs 15 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 16 Raw image (shock-deformed copper) Attenuated direct beam Near-field orientation mapTomographic reconstruction  ‘Near field’ diffraction - Non-destructive EBSD –type info. Advanced Photon Source (U. Lienert, A. Khounsary and P. Kenesei) Carnegie Mellon MRSEC

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

18 Scientific scope  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 –CO 2 sequestration (fluid movement in rock/capillary trapping)  Biology –Response of bone and teeth to applied load, environment, dose Advanced Photon Source 18 Porous Anode Porous cathode H 2 & CO O2O2 e-e- H 2 O & CO 2 e-e- O=O= Controlled porosity Thermal mismatch Chemical durability Mechanical integrity Dense electrolyte SOFC (battery) New lightweight composites Optimizing metal sheet forming High-energy scattering and imaging: Penetrating in situ probes -> real conditions High flux -> real time High q-resolution -> real/complex materials

19 LDRD: Hard X-ray Sciences Initiative, R1 Li + insertion ~ nm Grain fracturing ~ μm Li + diffusion ~ mm SAXS PDF Imaging EXAFS In situ R everse M onte C arlo modeling of ALL data +Echem C HALLENGES IN ENERGY STORAGE SPAN MULTIPLE LENGTH SCALES H ARD X - RAY TOOLS CAN PROBE DIFFERENT LENGTH SCALES R MC METHODS ALLOW COMBINED ANALYSIS OF VARIETY OF DATA → 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 I MPACTS SPANNING MANY STRATEGIC AREAS Combined Approaches Towards a Hierarchical Understanding of Battery Materials

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

21 Precursor CoOOH Intermediate Co 3 O 4 Final LiCoO 2 Intermediate disappears. Time (s) Channels SAXSWAXS suppression of steel In-situ synthesis of LiCoO 2 nano-particles for Li-ion batteries

22 22 ? ? ? ? ? ? ? Xia, Sun, Yang, Murphy, Mirkin, et al. ? First Generation of nanoparticles: Size Decrease Second Generation of nanoparticles: Shape Control Application? Third Generation? 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

23 Probing nanophase evolution at semiconductor interface Advanced Photon Source 23 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) Y. Sun et al, Nanoletters 10 (2010),

24 Scientific scope  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 –CO 2 sequestration (fluid movement in rock/capillary trapping)  Biology –Response of bone and teeth to applied load, environment, dose Advanced Photon Source 24 Porous Anode Porous cathode H 2 & CO O2O2 e-e- H 2 O & CO 2 e-e- O=O= Controlled porosity Thermal mismatch Chemical durability Mechanical integrity Dense electrolyte SOFC (battery) New lightweight composites Optimizing metal sheet forming High-energy scattering and imaging: Penetrating in situ probes -> real conditions High flux -> real time High q-resolution -> real/complex materials

25 25 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 Tomography to study intergranular stress corrosion cracking (King et al 2008) Hydride formation and growth at stress concentrations (Daymond and Motta ) Fiber-matrix interactions in CMCs (Faber)

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

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

28 Hydride Diffraction Pattern 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) D pattern Integrate segments

29 HE Diffraction: Hydride Strain Mapping 200  m 50  m 2 spot size 20  m 2 spot size  yy – ZrH x {111} Y-Axis (  yy ) X-Axis (  xx ) 30% Overload (relative to hydride growth)

30 Hydride Fracture  yy Zr (Avg)  yy ZrHx {111} 20% Overload relative to hydride growth load 30% Overload relative to hydride growth load 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 Scientific scope  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 –CO 2 sequestration (fluid movement in rock/capillary trapping)  Biology –Response of bone and teeth to applied load, environment, dose Advanced Photon Source 31 Porous Anode Porous cathode H 2 & CO O2O2 e-e- H 2 O & CO 2 e-e- O=O= Controlled porosity Thermal mismatch Chemical durability Mechanical integrity Dense electrolyte SOFC (battery) New lightweight composites Optimizing metal sheet forming High-energy scattering and imaging: Penetrating in situ probes -> real conditions High flux -> real time High q-resolution -> real/complex materials

32 in-situ studies of real size samples The pores distribution of large samples are now only possible in static conditions and after a lengthy and disruptive sample preparation process. Carbon sequestration, mine and oil exploration Nature Vol June 2009 Thermal expansion cracking in rocks 32 Advanced Photon Source Upgrade (APS-U) project 200  C395  C 100 um 2 cm Understanding thermal cracking in fine-grained granite: increase in porosity with temperature facilitates the percolation of fluid through the rock µm

33 Scientific scope  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 –CO 2 sequestration (fluid movement in rock/capillary trapping)  Biology –Response of bone and teeth to applied load, environment, dose Advanced Photon Source 33 Porous Anode Porous cathode H 2 & CO O2O2 e-e- H 2 O & CO 2 e-e- O=O= Controlled porosity Thermal mismatch Chemical durability Mechanical integrity Dense electrolyte SOFC (battery) New lightweight composites Optimizing metal sheet forming High-energy scattering and imaging: Penetrating in situ probes -> real conditions High flux -> real time High q-resolution -> real/complex materials

34 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 High-energy X-ray scattering gives distinct information from the mineral, collagen fibril and implant phases. HAP lattice planes diffract WAXS pattern SAXS pattern ~67 nm

35 Phase response vs load Model Setup L R spring HAP collagen 67 nm Interstitial space E WAXS =39.6GPa E SAXS =19.8GPa 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 Nanoscale model and experimental validation

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

37 Bone Implant – highest level of hierarchy Structure bone screw head implant  Bone: bovine femur  Screw head: solid cp-3 Ti  Implant: porous cp-1 Ti HAP Strain Distribution implant boundary mapping boundary 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, msec resolution –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 38

39 Some common technical challenges / opportunities Advanced Photon Source 39  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

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


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