Robin Woracek - Start€¦ · Neutron Imaging & Diffraction This presentation was mainly concerned...

$: Robin Woracek - Start€¦ · Neutron Imaging & Diffraction This presentation was mainly concerned with imaging. Diffraction was covered by Jochen Fenske (HZG) and Joe Kelleher (STFC).$
Neutron Imaging & Diffraction This presentation was mainly concerned with imaging. Diffraction was covered by Jochen Fenske (HZG) and Joe Kelleher (STFC). We can share additional information on diffraction as well.

www.europeanspallationsource.se

Robin Woracek

Instrument Class Coordinator Imaging & Engineering

Point of contacts (within BIR2 platform):

Robin Woracek

[email protected]

Markus Strobl (Head of Neutron Imaging Group at PSI)

[email protected]

BIR2Gain workshop: Welding and Corrosion Challenges, Lund 1-2 June 2017

mailto:[email protected]


Some references related to Neutron Imaging

A

Corrosion

• H. Berger, Advances in neutron radiographic techniques and applications: a method for nondestructive testing, Applied radiation and isotopes,

61 (2004) 437-442.

• D. Mannes, E. Lehmann, A. Masalles, K. Schmidt-Ott, K. Schaeppi, F. Schmid, S. Peetermans, K. Hunger, The study of cultural heritage

relevant objects by means of neutron imaging techniques, Insight-Non-Destructive Testing and Condition Monitoring, 56 (2014) 137-141.

• Examples herein

Welding

• E.H. Lehmann, S. Peetermans, L.Josic , H. Leber, H. van Swygenhoven, Energy-selective neutron imaging with high spatial resolution and its

impact on the study of crystalline-structured materials, NIMA, 2014

• N. Kardjilov, I. Manke, A. Hilger, S. Williams, M. Strobl, R. Woracek, M. Boin, E. Lehmann, D. Penumadu, and J. Banhart , "Neutron Bragg-

edge mapping of weld seams", International Journal of Materials Research, 2012

• A.S. Tremsin, S. Ganguly, S.M. Meco, G.R. Pardal, T. Shinohara, W.B. Feller, Investigation of dissimilar metal welds by energy-resolved

neutron imaging, Journal of Applied Crystallography, 49 (2016).

Hyrogen studies

• H. Rauch, A. Zeilinger, Hydrogen transport studies using neutron radiography. Atomic energy review 15, 249 (1977).

• H. Rauch, in Proceedings of the second summer school on neutron scattering: neutron scattering from hydrogen in materials. (1994).

• C. Grünzweig, D. Mannes, A. Kaestner, F. Schmid, P. Vontobel, J. Hovind, S. Hartmann, S. Peetermans, E. Lehmann, Progress in Industrial

Applications using Modern Neutron Imaging Techniques, Physics Procedia, 43 (2013) 231-242

• A. Griesche, E. Dabah, T. Kannengiesser, N. Kardjilov, A. Hilger, I. Manke, Three-dimensional imaging of hydrogen blister in iron with neutron

tomography, Acta Materialia, 78 (2014) 14-22.

• Imaging of an operating LaNi4.8Al0.2–based hydrogen storage container, International Journal of Hydrogen Energy, (2011).

• C. Pohlmann, K. Herbrig, Ł. Gondek, N. Kardjilov, A. Hilger, H. Figiel, J. Banhart, B. Kieback, I. Manke, L. Röntzsch, In operando visualization

of hydride-graphite composites during cyclic hydrogenation by high-resolution neutron imaging, Journal of Power Sources, 277 (2015) 360-369.

Strain Mapping

• A. Tremsin, T. Yau, W. Kockelmann, Non‐destructive Examination of Loads in Regular and Self‐locking Spiralock® Threads through

Energy‐resolved Neutron Imaging, Strain, 52 (2016) 548-558.

• A.S. Tremsin, S. Ganguly, S.M. Meco, G.R. Pardal, T. Shinohara, W.B. Feller, Investigation of dissimilar metal welds by energy-resolved

neutron imaging, Journal of Applied Crystallography, 49 (2016).

Phase Mapping

• R. Woracek, D. Penumadu, N. Kardjilov, A. Hilger, M. Boin, J. Banhart, I. Manke, 3D Mapping of Crystallographic Phase Distribution using

Energy-Selective Neutron Tomography, Advanced Materials, 26 (2014) 4069-4073.

• R. Woracek PhD thesis, available: http://trace.tennessee.edu/utk_graddiss/3375/

http://trace.tennessee.edu/utk_graddiss/3375/

http://trace.tennessee.edu/utk_graddiss/3375/

AGENDA

ESS: The most intense neutron source for material research

Why Neutrons?

o Example: Neutron Diffraction for residual stress

o Example: Neutron Imaging to detect hydrogen

Introduction: Neutron Imaging (Absorption Contrast)

o Examples 1-5: Corrosion in metals

Introduction: Diffraction Contrast in Neutron Imaging

o Examples 6-8: Phase transformations, Welds

Summary & Discussion

Some references

A

Existing Neutron Sources

OECD recommendation 2006

“The Neutron Sources Working Group recommends a scenario which aims at the construction of

advanced neutron sources in each of the three regions Asia/Pacific rim, Europe and North America, to be

operational within 20 years, and catering for regional needs in a wide range of scientific and

technological applications.”

• J-PARC, Japan

• SNS, USA

• ESS, Europe

Source influences the neutron imaging (diffraction) experimental setup

Sweden and Denmark: 47,5% Construction 15-20% Operations

Partner Countries: 52,5% Construction 80-85% Operations

1843 M€ construction 140 M€/yr operations

ESS - A European Big Science Project • 5 MW proton accelerator • rotating tungsten target

2

Neutron Sources

Introduction

3

September 2016 4

AGENDA


Why Neutrons?








A

Properties of neutrons for measurements

Some Background

Attenuation characteristics

2

High contrast for heavy elements

High transparency for hydrogenous / organic material

High sensitivity for hydrogenous / organic material

High transparency for heavy elements


Some Background

• Different interaction behavior results in different interaction

probabilities and attenuation coefficients for the different elements:

X-ray


Some Background

Neutrons

• Different interaction behavior results in different interaction

probabilities and attenuation coefficients for the different elements:

x-ray

neutron

x-ray neutron

neutron

Courtesy of PSI, NIST

Some Background


Neutrons ‘see’ light elements

4

Charge neutral Deeply penetrating

H motion in fuel cells

Improve electric cars

Nuclear scattering Sensitive to light

elements and isotopes

Active sites in proteins

Better drugs

Magnetic moment (spin)

Probe of magnetism

Solve the high-temperature

Superconductivity puzzle

Efficient high-speed trains

Urate oxidase


Introduction

4

Multi-Purpose Imaging

General-Purpose SANS

Broadband SANS

Surface Scattering

Horizontal Reflectometer

Vertical Reflectometer

Thermal Powder Diffractometer

Bispectral Power Diffractometer

Monochromatic Powder Diffractometer

Materials Science Diffractometer

Extreme Conditions Diffractometer

Single-Crystal Magnetism Diffractometer

Macromolecular Diffractometer

Cold Chopper Spectrometer

Bispectral Chopper Spectrometer

Thermal Chopper Spectrometer

Cold Crystal-Analyser Spectrometer

Vibrational Spectroscopy

Backscattering Spectrometer

High-Resolution Spin-Echo

Wide-Angle Spin-Echo

Fundamental & Particle Physics

life sciences magnetism & superconductivity

soft condensed matter engineering & geo-sciences

chemistry of materials archeology & heritage conservation

energy research fundamental & particle physics

Spectr

oscopy

Larg

e-S

cale

Str

uctu

res

Diffr

action

ESS: Specialized instruments and methods

Introduction

5

ODIN

SKADI

LOKI

Surface Scattering

FREIA

ESTIA

HEIMDAL

DREAM

Monochromatic Powder Diffractometer

BEER

Extreme Conditions Diffractometer

MAGIC

NMX

C-SPEC

VOR

T-REX

BIFROST/CAMEA

VESPA

MIRACLES

High-Resolution Spin-Echo

Wide-Angle Spin-Echo

Fundamental & Particle Physics

Larg

e-S

cale

Str

uctu

res

Diffr

action

Spectr

oscopy

life sciences magnetism & superconductivity

soft condensed matter engineering & geo-sciences

chemistry of materials archeology & heritage conservation

energy research fundamental & particle physics


Introduction

5

Beamline for European Materials Engineering Research (BEER)

Optical and Diffraction Imaging with Neutrons (ODIN)


Introduction

5

AGENDA


Why Neutrons?








A

In general, compressive stresses at a surface are beneficial and enhance resistance to failure.

Tensile stresses (especially near surface) can aid the onset of cracking which can cause premature failure.

RS superpose external load stresses under service conditions.

Residual Stress: Introduced during manufacture and/or during use by e.g. mechanical forming processes, welding and heat treatments. Residual stresses are present in virtually every solid material or component.

Diffraction: Residual Stress

Neutrons for Engineering

8

Courtesy of M.Boin

Surface

Angle dispersive X-ray methods

Energy range 5 – 17 keV

Information depth (steel) 15 µm

y

Intermediate zone

Energy dispersive X-ray diffraction

Energy up to about 120 keV

Information depth (steel) 100 µm

z Bulk

Neutron diffraction

(High energy synchrotron diffraction)

Information depth (steel): some cm

z

Penetration depth

Nondestructive characterization from surface to volume!



9

Courtesy of M.Boin

Nondestructive characterization from surface to volume!

X-ray lab

Synchrotron

nm

cm

Neutrons



9

Courtesy of M.Boin

Measure Strain and then convert to Stress

𝑛𝜆 = 2𝑑ℎ𝑘𝑙 𝑠𝑖𝑛 𝜃

Bragg's Law:

1sin

sin0

0

d

d

Elastic strain:

)()21)(1(1

zyxii

EE

Triaxial stress:

𝐸 − 𝑌𝑜𝑢𝑛𝑔′𝑠 𝑚𝑜𝑑𝑢𝑙𝑢𝑠 𝑣 − 𝑃𝑜𝑖𝑠𝑠𝑜𝑛′𝑠 𝑟𝑎𝑡𝑖𝑜

Hooke’s Law σij = Cijkl εkl

Residual Stress determination

Neutrons for Engineering Courtesy of M.Boin

AGENDA


Why Neutrons?








A

5 m

m

Hydrogen loading of duplex stainless steel

Electrochemically loaded

H2 (~ 100 wt. ppm)

Resolution: 15 µm (pixel size: 6.5 µm), FOV: 13 x 13 mm2, 600 proj. x 60 s

A. Griesche et al., Acta Materialia 78 (2014)

Imaging: Hydrogen embrittlement of steels


10

Volume registration

Charged Annealed

Quantification

kmol/m3

6023.0

.*)/(

,

3

totalHM

wtatmmol

vo

lum

e d

ensi

ty, k

mo

l/m

3

Hydrogen density kmol/m3

1 mm

A. Griesche et al., Acta Materialia 78 (2014)

Imaging: Hydrogen embrittlement of steels


11

L. Gondek et al.,International Journal

of Hydrogen Energy 36 (2011)

Hydrogen Storage Materials

(LaNi4.8Al0.2)

Courtesy of N. Kardjilov Neutrons for Engineering

AGENDA


Why Neutrons?








A

Introduction

Neutron Imaging

13

ld

L D

L – Distance Collimator-Object

l – Distance Object-Detector

D – Collimator aperture

dxxeI

)(

0~

I0 – primary beam

(x) – attenuation coefficient

Spatial Resolution

Spatial Resolution

more: www.psi.ch/niag/

http://www.psi.ch/niag/

SANS regime

15μm

Spatial resolution vs ‘spatial sensitivity’

Neutron Imaging

• ‘Contrast’ due to small spatial features • Usually averaged over several mm3

• Contrast from features (>spatial resolution) resolved in real space

M. Strobl & F. Grazzi (2015) From scattering in imaging to prospects at pulsed sources, Neutron News 26

AGENDA


Why Neutrons?








A

Corrosion

Examples 1-5: Neutron Imaging

13

• Neutrons penetrate metals quite easy, while

providing contrast forlight elements.

• Well suited to investigate corrosion

• Was a ‘hot topic’ some decades ago, but

applications with industrial background

were rather limited in the last few years…

• X-rays complementary

X-rays

Neutrons

Corrosion in cultural heritage objects

Example 1: Neutron Imaging

Questions:

Identification of - shape/size of lead

sheets; inner wood sculpture

- Mounting points / joints (nails and soldering)

- Extent of carbonate corrosion

Strategy for restauration

Lead/Wood sculpture “the violinist”

by Pablo Gargallo MNAC, Barcelona

Dimensions: 55 cm x 32 cm x 22 cm

Appraisal as basic information for:

Decision for conservatory treatment

Development of new conservatory treatments

Courtesy of

Corrosion in cultural heritage objects


Mannes et al. (2014) INSIGHT, 56 (3): 137-141

inner wooden kernel

areas affected by corrosion (red) fixation by nails and soldering (blue)

Courtesy of

55cm

Corrosion: Documentation of processes


X-ray information on density

Neutrons information on element changes (i.e. H, Cl,…)

X-ray Neutrons

Courtesy of M. Jacot, C. Gervais, K. Schmidt-Ott

Courtesy of



Plan of experiment

X-r

ay t

om

og

rap

hy

Neutr

on t

om

ogra

phy

X-r

ay t

om

ogra

phy

Neutr

on t

om

ogra

phy

Dechlorination

treatment

(≈3 months)


Courtesy of



Before Before After After Difference

X-ray Neutron

Before-After > 0

Before-After < 0


Courtesy of



Uncorroded iron

Residual ground material

Iron corrosion products (with chlorides)

Variable concentration of iron and chloride blur the interpretation Courtesy of M. Jacot, C. Gervais, K. Schmidt-Ott

Information from X-ray & neutron CT

Verification

Base for segmentation

Courtesy of

Corrosion of AL


Corrosion process in brass


Joint project of Bern University of the arts, ETH Zurich, PSI, SNM (Funded by Swiss National Science Foundation):

“Brass instruments of the 19th and early 20th centuries between long-term conservation and use in historically informed performance practice”

Neutron imaging monitoring of the corrosion in brass instruments (Neutron-CT at the start of the project and at the end)

22

Courtesy of



Start End

Courtesy of



24

Corrosion of steel in concrete


Corrosion of the steel in concrete (collaboration between PSI and P. Chang, Y. Wang, China)

25

Courtesy of

Corrosion of steel in concrete


Courtesy of Peng and Wittmann

Corrosion of Steel within concrete matrix

Visualised 3D-evaluation of Neutron-CT

Concrete

Steel

Corroded areas

Courtesy of

AGENDA


Why Neutrons?








A

magn. fields

SANS regime

M. Strobl & F. Grazzi (2015) From scattering in imaging to prospects at pulsed sources, Neutron News 26

Diffraction Contrast

“Bragg Edge Imaging”

• Contrast from features (<spatial resolution) resolved in real space

Spatial resolution vs ‘spatial sensitivity’

Advanced Neutron Imaging

Phase Texture Strain

Bragg Edge Imaging

Advanced Neutron Imaging

AGENDA


Why Neutrons?








A

Phase Transformation: TRIP steel

Example 6: Bragg Edge Imaging

Metastable austenitic stainless (TRIP) steel: FCC Austenite

transforms to HCP and BCC Martensites under strain

1.4

0.6

30

• 44kN

• 11Nm (110Nm)

• tomography





Tor-

max

Ten

-max

Vir

gin

50m

m

Ø8mm

Phase transformation clearly observed!

Tomography for further quantification

BC

C (

21

1)

BC

C (

11

0)

BC

C (

20

0)

FCC

(2

00

)

FCC

(2

20

)

FCC

(1

11

)



Torsion Tensile



• R. Woracek, D. Penumadu, N. Kardjilov, A. Hilger, M. Boin, J. Banhart, I. Manke, 3D Mapping of Crystallographic

Phase Distribution using Energy-Selective Neutron Tomography, Advanced Materials, 26 (2014) 4069-4073.

Complementarity of methods…

Different methods provide complementary information and cover

various length scales….

Martensite within a ferrite matrix

x-rays, optical microscopy, electrons, neutrons, …


3D-XRD/DCT

33

• E.H. Lehmann, S. Peetermans, L.Josic , H. Leber, H. van Swygenhoven, Energy-selective neutron imaging with high

spatial resolution and its impact on the study of crystalline-structured materials, NIMA, 2014

• N. Kardjilov, I. Manke, A. Hilger, S. Williams, M. Strobl, R. Woracek, M. Boin, E. Lehmann, D. Penumadu, and J.

Banhart , "Neutron Bragg-edge mapping of weld seams", International Journal of Materials Research, 2012 31

Weld 1

Example 7: Diffraction Contrast

• E.H. Lehmann, S. Peetermans, L.Josic , H. Leber, H. van Swygenhoven, Energy-selective neutron imaging with high

spatial resolution and its impact on the study of crystalline-structured materials, NIMA, 2014

• N. Kardjilov, I. Manke, A. Hilger, S. Williams, M. Strobl, R. Woracek, M. Boin, E. Lehmann, D. Penumadu, and J.

Banhart , "Neutron Bragg-edge mapping of weld seams", International Journal of Materials Research, 2012 32

Weld 2


Dissimilar welds by ToF imaging


• A.S. Tremsin, S. Ganguly, S.M. Meco, G.R. Pardal, T. Shinohara, W.B. Feller, Investigation of dissimilar metal welds

by energy-resolved neutron imaging, Journal of Applied Crystallography, 49 (2016)



37





Spatially resolved strain maps



Dissimilar welds by ToF imagingc


Resonance absorption contrast: Elemental contrast: E.g. check diffusion processes

Strain distribution in threads


• Strain Mapping in a bolt assembly, where a standard thread is compared with ‘spirallock’ thread

• The experimental data visualizes the strain redistribution inside the screw and base plate

• A. Tremsin, T. Yau, W. Kockelmann, Non‐destructive Examination of Loads in Regular and Self‐locking Spiralock®

Threads through Energy‐resolved Neutron Imaging, Strain, 52 (2016)

AGENDA


Why Neutrons?






o Examples 6-8: Phase transformations, Welds, Strain


A

• Neutron Imaging is useful in many scientific areas

• New methods (not covered herein) rapidly evolving : Guidance from

industry needed to develop methods that will benefit society

• Corrosion certainly a topic that should be addressed using neutron

imaging: underrepresented in recent years

• We are no experts in corrosion, welding, hydrogen embrittlement etc…

• We have good collaborations with existing neutron facilities worldwide!

• ESS operates a testbeamline in Berlin: test measurements + feasibility

studies are welcome!

• Design and discuss experiments together! Now is a good time!

• We should strive to take advantage of the possibilities ESS will offer, by

(now) designing suitable experimental setups, sample environments,

modelling tools,…

Contact us: [email protected]

Summary


59

Journey to deliver the world’s leading facility for research using neutrons

2014 Construction Starts

on Green Field Site

2009 Decision to Site

ESS in Lund

2025 ESS

Construction

Phase Complete

2003 European Design of

ESS Completed

2012 ESS Design Update

Phase Complete

2020 Machine Ready for

1st Beam on Target

2023 ESS Starts

User Program

THANK YOU! Courtesy of

44kN tension, 11Nm (110Nm) torsion, tomography mode

Available for joint experiments.

ENGIN-X (ISIS)

Portable loading system

Sample Environment

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