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A Deep Look Into Materials: High Energy X-rays in Metallurgy

• H. Reichert

X-RAY SCIENCE

The electromagnetic spectrum

X-RAY SOURCE DEVELOPMENT : STORAGE RINGS ……..

Averge Brillance (photons/s/mm2/mrad2/0.1%BW)

1900 1920 1940 1960 1980 2000

Synchrotron Radiation

Third Generation Second generation First generation X-ray tubes ESRF (2015) ESRF (1994)

1 2 1 1 1 1 1 1 1 1 1 1 1 8 1 2 1 2 1 2 1 1 1 1 1 1 1 1 1 1 1 9 1 7 1 6

ESRF UP (2015)

storage ring performance (ESRF)

AN INTERNATIONAL GOVERNANCE

13 Member states: France 27.5 % Germany

24 %

Italy 13.2 % United Kingdom 10.5 % Russia 6 %

Benesync 5.8 %

(Belgium, The Netherlands)

Nordsync 5 %

(Denmark, Finland, Norway, Sweden)

Spain 4 % Switzerland 4 % 8 Associate countries: Israel 1.5 % Austria 1.3 % Centralsync 1.05%

(Czech Republic, Hungary, Slovakia)

Poland 1 % Portugal 1 % South Africa 0.3 % Legal status: Private non-profit civil company subject to French law

21 PARTNER COUNTRIES

• Partnership between 21 countries
• World’s most productive synchrotron laboratory
• Research in all areas involving condensed

matter, materials, and living matter

• ~30 public beamlines (instruments); 14 CRG

beamlines (national teams)

• 600 Staff: 500 with a technical background,

60 post-docs, 40 PhD students

• ~8000 user visits for ~1500 projects
• ~1900 publications / year
• Annual budget: ~100 M€ including the Upgrade Programme

THE ESRF IN A NUTSHELL

Beamline portfolio

Ima magi ging Diffra ract ctio ion Spectro rosco copy py UP PI 2013: new beamline’s portfolio

HIGH ENERGY X-RAYS

ID16A+B ASD

beam size cm – mm – µm – nm up to 700 keV

• Diffraction peaks arising from

all phases measured simultaneously by two Ge solid- state detectors

• Energy range: 50-500keV
• Spatial resolution

0.05×0.05×0.50mm3 − 0.2×0.2×2.0mm3

• Acquisition time per point:

30-200s

STRAIN SCANNING BY ENERGY DISPERSIVE DIFFRACTION

STRAIN SCANNING

AIRBUS LANDING GEAR PISTON ROD ROLLS ROYCE TRENT-700 CHORD

FAN BLADE (TI-6AL-4V)

900×400×20mm3 DUNLOP AIRCRAFT WHEEL (Ø50cm×50cm, 30KG)

STRAIN SCANNING BY ENERGY DISPERSIVE DIFFRACTION

• Large samples: penetration up to 10 cm of steel
• Spatial resolution down to 0.05×0.05×0.50mm3
• Strain resolution: 2 .10-4

• GAUGE VOLUME DEFINED BY SLITS AND THE ANALYSER CRYSTAL

⇒ NO “PSEUDOSTRAIN” DUE TO PARTIALLY FILLED GAUGE

VOLUME NEAR THE SURFACE

• SUPERIOR RESOLUTION ENHANCES THE STRAIN RESOLUTION AND

ENABLES PEAK SHAPE ANALYSIS

• DEPTH SENSITIVITY BY CHANGING THE ENERGY AND EXPLOITING

THE ABSORPTION EDGES

Radial strain FWHM

Single Laser Shock Peened impact on Ti-6Al-4V

Koichi Akita, Tokyo Institute of Technology

STRAIN MAPPING NEAR THE SURFACE HARD X-RAYS FOR SURFACE SENSITIVITY HIGH ENERGY X-RAYS FOR DEEP PENETRATION

The ESRF has a long-standing tradition in in-situ materials testing

We study the evolution of the structure of a wide range of Materials

• Metals/alloys
• Composites
• Polymers
• Semiconductors
• Biomaterials

under

• mechanical,
• thermal,
• electrical load
• r in changing environmental conditions

MATERIALS TENSILE TESTING RIGS

50 kN Servo hydraulic ETMT

From static load to dynamic cyclic fatigue

MICRO-COMPRESSION DEVICE

Materials Processing

Nb-Ti SC with 8.3T maximum field strength to be replaced by Nb3Sn (15T) Thermal treatment of Nb3Sn strands leads to formation of voids Void growth in operation leads to degradation and failure Development of optimised heat treatment cycles.

void

Nb3Sn filament

NB3SN SUPERCONDUCTORS

white x-ray beam sample in furnace tomography detector monochromatic x-ray beam 88 keV 2-D diffraction detector Laue mono Laue mono

EXPERIMENTAL SETUP

x-ray microtomography

Cu (3 1 1) Cu (2 2 0) Cu (2 0 0) Cu (1 1 1) Nb (1 1 0) Nb (2 0 0) Nb (2 1 1) Nb (2 0 0) 230 °C 420 °C 540 °C 5 h-540 °C Sn (2 0 0) Sn (1 0 1) Sn (2 1 1) Cu6Sn5 (2 0 2) Cu6Sn5 (2 0 6) Cu3Sn (0 8 3) Cu3Sn (0 16 0) Cu5.6Sn (1 1 2)

Cu5.6Sn (1 1 1) Cu5.6Sn (2 0 0)

Cu5.6Sn (1 1 3)

Cu541Sn11 (6 6 0)

x-ray diffraction

3D view of the voids formed inside the IT strand at different HT temperatures. Variation of the diffraction patterns of the IT Nb3Sn strand during Cu–Sn mixing HT cycle.

The void formation mechanisms could be identified by correlating the quantitative void growth results (tomography) with the quantitative description of the phase transformations (diffraction) Void volume is clearly correlated with the Cu3Sn content in the strand.

• Superconductors based on

Bi2Sr2CaCu2Ox (Bi-2212) can achieve high critical current densities at very high magnetic fields

• Bi-2212 is the only high temperature

superconductor that can be produced in the form of round wires, which makes Bi-2212 particularly interesting for high energy physics applications, MRI scanners, power infrastructures in densely populated urban areas, etc

• In order to achieve Bi-2212 filament

connectivity, the Powder-in-Tube wire is submitted to a heat treatment, during which the powder melts at about 880 °C. Tomographic cross section through an as-drawn Bi-2212 PIT wire (before HT) Ag Bi-2212 filaments

• F. Kametani et al., Supercond. Sci. Technol. 24, 075009 (2011)
• C. Scheuerlein et al., Supercond. Sci. Technol. 24 115004 (2011)

XRD-CT PERFORMANCE MELT PROCESSING OF BI-2212 POWDER-IN-TUBE SUPERCONDUCTORS

Sequence of diffractograms acquired during in-situ HT of a Bi-2212 wire in air Transverse tomographic cross section through a fully processed Bi-2212 PIT wire The void and phase evolution is studied by combined diffraction and tomography with a monochromatic 70 keV beam.

EXPERIMENTAL

ramp rate 25 K/h in air

Tomographic cross sections acquired before and after in-situ HT to Tmax = 875 °C (partial Bi-2212 melting) and Tmax = 915 °C (complete Bi-2212 melting).

• Bi-2212 melts in the temperature range 867-882 °C.

Bi-2212 re-nucleation during cooling is observed between 863-842 °C. Bi-2201 is detected during cooling below 850 °C.

• During the melt processing of Bi-2212 superconductors large voids agglomerate

from residual powder porosity.

• These voids reduce the filament connectivity and have been identified as major

current limiting mechanism in round Bi-2212 wires.

915 °C 875 °C 20 °C

RESULTS

• Extensive porosity found in the wire

processed under 1 bar

• No porosity and high density found

in a wire processed at 100 bar

1 bar 100 bar X-ray tomograms Overall conductor current

• D. C. Larbalestier et al., Nature Materials, 13 (2014) 375-381

Ag Bi-2212 pores

The eightfold increase in JE is due to the elimination of leakage and suppression of the void porosity New method found for processing round wires of Bi-2212 to increase current density by means of a very high overpressure process during the heat treatment of the material The use of HTS is limited by their high cost and laborious fabrication process HTS-based conductors can be fabricated only as thin, flat tapes in which grain boundary alignment plays a dominant role for the ability to carry large currents. HIGH TEMPERATURE SUPERCONDUCTORS FOR HIGH MAGNETIC FIELDS

Beamline portfolio

UP PI 2013: new beamline’s portfolio

ID16A+B

Time resolution spans 15 orders of magnitude! 10-10 - 105 sec Imaging Crystallography Scattering Spectroscopy

TIME RESOLUTION

from milli-seconds to nano-seconds

Sample: Fe–Cr–17.3% Ni–11.1% Mo–2.1% C < 0.1% austenitic steel Beam energy : 50-150keV Beam size : 1 x 0.1 mm2 Detector: CMOS sensor coupled to Imaging Intensifier Frame rate: 1kHz FUSION WELDING – MILLISECOND RANGE

IN-SITU MEASUREMENT

Time evolution of angular velocities for six re-orienting crystals. weld cross-section micrographs sectioned along the beam direction. (a) Full weld cross-section from a post-experimental sample. (b) Half-cross section detailing an experimental weld pool. The grains form predominantly at the melt–solid interface and grow into the X-ray illuminated region

Bragg spot angular rotations are up to 104 times larger than expected from thermal contraction, stresses or any

• ther change of the lattice

parameter

Ultrafast moving free crystals Moving columnar crystals Blocked columnar crystals (only thermal contraction)

RESULTS

→ mainly due to rigid body rotation

Evolution of growth and tilting for four representative columnar type crystals.

Conclusion: substantial crystal rotation, tilting and motion occurs, especially in the earlier stages of solidification

• W. U. Mirihanage et al., Acta Mater. 68 (2014) 159-168

RESULTS

strong influence on the transient behavior of growing crystals in welds

• Metals coalesce via extremely rapid solidification
• Liquid → solid phase transformations is controlled by mass and heat

transport under conditions far from equilibrium.

• Transport conditions are decisive for the microstructure of the advancing

solidification fronts, (including chemical segregation)

• Mechanical properties of the weld are dictated by the full dynamic history of

the growth processes.

• Simulation models developed for solidification processes at cooling rates

that are orders of magnitude lower than those that apply to real welds

• The high cooling rates have made direct in situ experimental studies of the

solidification part of the process extremely demanding.

TIME-RESOLVED X-RAY DIFFRACTION STUDIES OF WELDING

Fusion-Welding

Solidification dynamics or individual grain growth in actual metallic welds has not yet been studied in any detail

30

WELDING & BENDING STEAL – KHZ RADIOSCOPY @ 120 KEV

Aucott, Dong, Marsden et al., University Leicester, UK & Dr. S. Wen, Tata Steel Experiment at ID19 (ESRF)

8×8 mm2 stainless steal

X-ray

WELDING & BENDING STEAL – KHZ RADIOSCOPY @ 120 KEV

120 keV (pink), 7.2 m propagation distance, 10 µm pixel size, 1000 images/s, 600 images

SOLIDIFICATION – MILLISECOND RANGE

solidification of an Al – Cu alloy formation of solid crystal dendrites

white beam mode indirect detection

Verification of solidification models

HIGH-SPEED ELECTRICAL FUSE BREAKING – MICROSECOND RANGE

• X. Just, P. Lhuissier, J.-M. Chaix (SIMAP), J.-L. Gelet, F. Balboni, M. Morati (Mersen)

MEGAFRAME-RATE RADIOSCOPY

• X. Just, P. Lhuissier, J.-M. Chaix (SIMAP), J.-L. Gelet, F. Balboni, M. Morati (Mersen)
• A. Rack, M. Olbinado, E. Boller, J. Morse (ESRF)
• approx. 30 keV (pink/white)
• 6.5 µm pixel size
• 1 000 000 image/s rate

(256 images buffer)

• 500 ns exposure time
• Shimadzu HPV-X2
• LYSO:Ce 250 μm

500 µm 0 µs 1 µs 2 µs

1 bunch 100 ps

before upgrade UPBL11 XAS at ID24 XRD at ID09

(012) reflection from a Bi target

Bismuth – 1 bunch XRI at ID15A/ID19

breaking glass with bunch clock resolution

PUSHING THE LIMITS

GAS GUN FOR SHOCK COMPRESSION

Eakins & Chapman, RSI 85 (2014)

MI-1224 - Eakins, Chapman et al., Imperial College London

GAS GUN: INSTALLATION AT ID19 (8 h set-up time

SHOCK WAVE PROPAGATION (BIMODAL POWDER BED)

Eakins, Chapman et al., Imperial College London

MATERIALS SCIENCE & ENGINEERING: A MULTI-SCALE PROBLEM

DNA PROTEIN CELL ORGAN BASE UNIT GRAIN MICROSTRUCTURE COMPONENT Displacement: 10-13-10-14 m determines properties of component on scale 100 m and up

MATERIALS ENGINEERING WITH SYNCHROTRONS

Stress & Strain Microstructure Visualisation Material (mechanical) Properties

X-ray Absorption & Phase Contrast X-ray Fluorescence X-ray Diffraction

3D morphology 3D chemistry 3D crystal phases

“Easy” & fast Towards routine Time consuming State of the art but time consuming

Golosio et al, APL

• P. Bleuet et al., Nature Materials 7, 468 - 472 (2008)

41

Courtesy of P. Bleuet

in 2010

Diffraction Tomography

X-RAY MICRO-TOMOGRAPHY METHODS

• Mimic the real conditions as closely as

possible - i.e. real samples (not just powder models)

• Look at the chemistry in different parts of the

sample

• Combine diffraction with tomography to map

chemistry in time and space

Real industrial catalyst body

2θ X-ray beam sample diffraction signal 2θ intensity tomographic algorithm total signal voxel signal

DYNAMIC XRD-COMPUTED MICRO-TOMOGRAPHY DYNAMIC XRD-CT

Heterogeneous catalysts Metals and metal oxides anchored to porous support materials

• S. D. M. Jacques et al., Angew. Chem. Int. Ed. 50, (2011) 10148–10152

XRD µ-CT

Crystallite size evolution

• Ni(en)xCO3
• Ni(en)(CO3)xCl2(1-x).xH2O
• Ni(en)(CO3)xCl2(1-x)
• Ni(en)0.5(O)xCl2(1-x)
• Ni(en)Cl2
• hcp Ni
• fcc Ni

Phase evolution

“Traditional” in-situ result XRD-CT in-situ result

• Two routes to the formation of metallic fcc

Ni active phase from two different decompositions of the precursor (green and cyan)

• different spatial distribution (core-shell)
• different nano particle size.
• important implications for the

activity/selectivity in a catalytic reaction.

43

Diffraction Tomography

DIFFRACTION TOMOGRAPHY

X-Ray Imaging

Hard X-ray Diffraction Microscopy

BRIGHT FIELD IMAGING - SAXS MICROSCOPY

• reciprocal space (top) and direct space (bottom) modes of operation
• 3D self-assembled systems,

e.g. bio-minerals, photonic crystals, colloidal systems

• at the borderline between bright field and dark field microscopy
• A. Bosak et al., “A new tool for mesoscopic materials,” Adv. Mat. 22, 3256 (2010)

Diffraction based Transmission X-ray Microscopy

Optics < 15 keV : zone plates 10 nm > 15 keV : compound refractive lenses 100 nm => 20 nm

HARD X-RAY DIFFRACTION MICROSCOPE (HXDM)

Composites Batteries Fuel cells Superconducting for wind cables

Cell stack

HXDM – MATERIALS & MULTISCALE STUDIES

Hard X-ray microscopy: multiscale structural mapping

• H. Simons et al. Nat. Comm. (2015)

Grain mapping Zoom on one grain Zoom on sub-grains 2 µm 200 nm 200 nm 0.5 deg 0.15 deg 0.02 deg 3D Orientation mapping of Al1050 sample deformed 6%:

HXDM – MATERIALS & MULTISCALE STUDIES Collaboration with DTU

• H. Poulsen

Objective Sample Condenser

Optimize relative stability of Condenser, Sample and Objective

• Short term(vibrations) and long term (thermal drift)
• Relative movements are increased by the geometrical magnification of the objective
• Common mode movements are not magnified and are therefore less critical.

HARD X-RAY DIFFRACTION MICROSCOPE (HXDM) Collaboration with DTU

• H. Poulsen

Condensing Optics

Objective Sample

xs xd

Low Resolution Diffraction Detector High Resolution Diffraction Detector

High Resolution Imaging Detector

Diffraction/ Full-Field Nanoscopy Setup

O(0.5 m) O(50 m)

DIFFRACTION CONTRAST TOMOGRAPHY

ESRF Upgrade Programme Phase I and ESRF-EBS

2009 2015

Phase I

19 upgraded or deeply refurbished BLs Accelerator and source upgrade Construction programme

Phase II

New storage ring 4 new BLs Enabling technology 2015 2022

X-RAY SOURCE DEVELOPMENT : STORAGE RINGS

Averge Brillance (photons/s/mm2/mrad2/0.1%BW)

Synchrotron Radiation

Third Generation Second generation First generation X-ray tubes ESRF (2015) ESRF (1994)

1 2 1 1 1 1 1 1 1 1 1 1 1 8 1 2 1 2 1 2 1 1 1 1 1 1 1 1 1 1 1 9 1 7 1 6

ESRF EBS (2020)

storage ring performance (ESRF)

1900 1920 1940 196o 1980 2000

ESRF Upgrade Programme

• A factor of ~100 increase in

brillance and coherent flux of the X-ray source

• A new and unique storage ring
• A complete renewal of the

« beamline » portfolio and of the users’ support facilites adapted to the new research

• pportunities

IVUN22 min. gap 6 mm, Kmax=1.7 CPMU14.5 min. gap 4 mm, Kmax=1.7

x 230 x 100

2 M IVUS & CPMUS

Photon Flux density IVUN22 min. gap 6 mm, Kmax=1.7 CPMU14.5 min. gap 4 mm, Kmax=1.7

x 40 x 70

2 M IVUS & CPMUS

Beamline portfolio

UP PI 2013: new beamline’s portfolio

NANOBEAMS @ ESRF

ID16A+B

Energy range spans from 2 keV to 100 keV Imaging Crystallography Scattering Spectroscopy

In situ experiments at ID16A, ID15A and ID19: multiscale aspect

Zoom non-destructively into a region of interest of a device, ,...

Keep sample preparation and measurement straightforward Magnified phase contrast imaging Quantitative reconstruction of the electron density Very high sensitivity

R Mokso et al., APL, 2007, 90, 144104

PHASE NANO-TOMOGRAPHY

• C. Landron, E. Maire, et al., Scripta Materialia 66 (2012) 1077

Martensite 3D micro-structure Ferrite / Martensite contrast

Dual Phase steel 11%vol. martensite High spatial and density resolution

Arcelor Mittal (O. Bouaziz) Application: car frame

DAMAGE IN DUAL-PHASE STEELS

Void density completely underestimated with too poor resolution

DAMAGE IN DUAL-PHASE STEELS

Effect of resolution:

• Nucleation: 1.6 μm not OK for steels
• Growth: OK (growth of largest voids with applied strain)
• 100 nm sufficient ?

Measured void density vs. strain

Largest void sizes vs. strain

100 nm voxel 1.6 µm voxel

N

True Strain True Strain

Deq

Voxel size 1.6µm 100nm Equivalent diameter of the smallest detected cavities 4µm 300nm DAMAGE IN DUAL-PHASE STEELS

FUTURE: COMBINE TECHNIQUES FOR HIGH END MANUFACTURING PROCESSES There are no analytical tools for real-time studies of high-end manufacturing processes

Additive Manufacturing

THANK YOU FOR YOUR ATTENTION!

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