neutron scattering structure studies of materials loaded ...neutron scattering structure studies of...
TRANSCRIPT
![Page 1: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/1.jpg)
Neutron scattering structure studies of materialsloaded by high neutron fluence in NPI ŘežPavol Mikula, Petr Lukáš, P. Strunz, J. Šaroun, Miroslav Vrána
Nuclear Physics Institute AS CR v.v.i., 250 68 Řež, Czech RepublicResearch Centre Řež, Ltd., 250 68 Řež, Czech Republic
![Page 2: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/2.jpg)
mean reactor power 10 MW
thermal flux in the core 1x1018 ns-1m-2
beam tube 1 1013 ns-1m-2
fuel enrichment 36% 235U
tank type
light water moderated and cooled
Reactor LVR 15, NRI Řež p.l.c.
![Page 3: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/3.jpg)
Neutron diffraction laboratoryBNCT
HR-SANS
test diffractometer neutron depth
profiling
powder diffractometer
HK9
HK8
HK6 HK3
HK2
HK4
powder diffractometer
strain diffractometer
strain scanner
10 2 m
C0 + C3H3BO3
![Page 4: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/4.jpg)
Residual strain/stress measurement
![Page 5: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/5.jpg)
Plane-wave diffractionIn diffraction neutron is considered as a (matter) waveAtoms/nuclei are scattering centres Scattered waves interfereBragg condition provides the angles where interference maxima can be foundStress in the material brings about the change of the position of atoms in the crystalline lattice – deformation, strain ∆dhkl/dhkl
Position of the interference maxima are sensitive to the value of the lattice spacing => strain component perpendicular to the lattice planes is measured
λ – neutron wavelength, θ – Bragg angle, dhkl – lattice spacing
Q
![Page 6: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/6.jpg)
PSD
Monochromator Neutron beam from source
Gauge volume
Beam defining optics for the incident beam
and shielding
Beam defining optics for the
diffracted beam and shielding
Specimen
Q
2θ
Beam stop
Conventional neutron strain scanner
Diffraction profileseen by PSD at someBragg angle θB
Irradiated part of thepolycrystalline material
Strains are of the order of 10-3 – 10-4, high angular resolution is required
θB
![Page 7: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/7.jpg)
beam shutter
positionsensitive detectorsample
Neutron strain scanner• high-resolution ∆d/d≈2x10-3
• neutron flux 106 n s-1cm-2
• gauge volume 1-300 mm3
• two-wavelength sandwichmonochromator
• linear position-sensitive detector• x,y,z linear stage• two-circle goniometer
88 90 920.0
0.4
0.8
2θ / deg
100% α 32.6% α + 67.4% γ
α 2111.65A
rel. in
tensit
y
2θ / deg96 98 100
0.0
0.4
0.8
1.2 32.8% γ + 67.2% α 100% γ
γ 2002.7A
γ 3111.65A
Sandwich monochromatorSi111(2.7A) & Si220(1.65A)Si111(2.7A) & Ge311(1.45A)
SPN-100 high-resolution diffractometer
![Page 8: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/8.jpg)
monochromator
Slits
sample
PSD detector
αM αS
αM,S beam divergence, LM distance monochromator-specimen, RM monochromator bending radius, θM,,SBragg angle - monochromator, specimen
−
−= 1
sin12
MM
M
M
SMS R
Ltgtg
θθθαα
−
=S
MM
MM
tgtg
LRθθθ
21sin
αs=0 ⇒
Neutron diffraction optics using bent perfect Neutron diffraction optics using bent perfect Si/GeSi/Ge single crystalssingle crystals
Focusing condition for qFocusing condition for quasiparalleluasiparallel beambeam
High resolution instrumentation
![Page 9: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/9.jpg)
Neutron diffraction stress/strain determination
♦ elastic strains only♦ one component of the elastic strain
tensor only is obtained in a single measurement♦ strains can be converted to stresses
using appropriate elastic moduli♦ determined selectively only from
grains which are suitably oriented with respect to the scattering vector♦ averaged strain values over those
grains
Characteristics
dhkl - lattice spacing, θhkl - diffraction angle, εhkl -lattice strain, λ - neutron wavelength
hklhkl
hkl
hkl
hklhklhkl d
dd
dd θθε ∆−=∆=−
= hklcot ,0,0
,0
Bragg law 2dsinθ=λ
Lattice strain
![Page 10: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/10.jpg)
Macrostrain scanning (from the peak shift)
dhkl - lattice spacing, θhkl - diffraction angle, εhkl - lattice strain
hklhkl
hkl
hkl
hklhklhkl d
dd
dd θθε ∆−=∆=−
= hklcot ,0,0
,0 hklhklhkl
hkl
hkl
hklhklhkl cot
dd
ddd
θθε ∆−=∆=−
= ,0,0
,0
Elastic strains only One component of the elastic strain tensor only is obtained in a single measurement Strains can be converted to stresses using appropriate elastic modules Determined selectively only from grains which are suitably oriented with respect
to the scattering vector Averaged strain values over those grains
![Page 11: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/11.jpg)
Strain - stress conversion
Experimental quantity – strain tensor component
Engineer’s task – strain tensor component
hklijε
ijσ
Theory of elasticity ∑=αβ
αβαβσε,ijij S
∑=αβ
αβαβεσ,ijij C
αβ,ijS
αβ,ijC
Elastic compliance constants
Elastic constants
[ ])()1()1)(21( zyxx
xE
εενεννν
σ ++−+−
=Principal components
Ex − diffraction Young modulus, ν − Poisson ratio
![Page 12: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/12.jpg)
Neutron diffraction stress/strain determination
Theory of elasticity
Experimental quantity - strain tensor component
[ ])()1()1)(21( zyxx
xE
εενεννν
σ ++−+−
=
∑=αβ
αβαβεσ,ijij C
∑=αβ
αβαβσε,ijij S
hklijε
Engineer’s task - stress tensor ijσ
Hook’s law αβ,ijS elastic compliance constants
elastic constantsαβ,ijC
Principal components
Ex diffraction Young modulus, ν Poisson ratio
![Page 13: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/13.jpg)
Three different components of the strain tensor should be measured.
x y
z
x
yz
x
yz
scanning direction
scanning direction
scann
ing di
rectio
nin c id e n t b e a m
in c id e n t b e a m
in c id e n t b e a m
scatte
ring v
ector
scattering vector
scattering vector
d if f r acted b eamd if f r acted b eam
d if f r acted b eam
Xcomponent
Zcomponent
Ycomponent
![Page 14: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/14.jpg)
![Page 15: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/15.jpg)
αM αS
Sample
Monochromator
Slits
PSD detector
Incident beam
Diffracted beamFocusing beam
−
=S
MM
MM
2tgθtgθ1sinθ
LRαs= 0
αM,S -beam divergence, LM - distance monochromator-sample, RM - monochromator bending radius, θM,S - Bragg angle at the monochromator/specimen
High-resolution strain scanningRay opticsBragg diffraction optics using bent perfect Si-crystal
PSD
Monochromator Neutron beam from source
Gauge volume
Beam defining optics for the incident beam
and shielding
Beam defining optics for the
diffracted beam and shielding
Specimen
Q
2θ
Beam stop
![Page 16: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/16.jpg)
Neutron strain scanner I
Neutron strain scanner• high-resolution ∆d/d≈2x10-3
• neutron flux 106 n s-1cm-2
• gauge volume 1-300 mm3
• two-wavelength sandwich monochromator
• linear position-sensitive detector
• x,y,z linear stage• two-circle goniometer
![Page 17: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/17.jpg)
Sample environment
![Page 18: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/18.jpg)
Weld deposited passPlate: 15Ch2MFA, 7 mm thicknesswelding material Inconel 52, (steel usedfor construction of reactor vessels)
Gauge volume2x2x10 mm3
![Page 19: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/19.jpg)
Lattice strains
400 450 500 550 6000
50
100
150
200
250
300
350
position -15 mm position 0 mm
Reflection (110)
Inten
sity /
1 80
0 s
Channel number
-20 -15 -10 -5 0 5 10 15 20 25 30-1,0
-0,5
0,0
0,5
1,0
1,5
2,0
2,5
3,0
ε / 1
0-3
mm
7 mm thick steel plate with a weld deposited pass
εx εz εy
-20 -15 -10 -5 0 5 10 15 20 25-1,0
-0,5
0,0
0,5
1,0
1,5
2,0
2,5
3,0
ε / 1
0-3
mm
7 mm thick steel plate with a weld deposited pass
εx εz εy
Sample I Sample II
-
-1
0
1
2
3
4
-4 -2 0 2 4 6 8 10x / mm
y / m
m
initial
1 2 3 4
56
A diagram displaying the course of the welding.
![Page 20: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/20.jpg)
10
x
30075
150
3
z
y
Schematic sketch of the welded plate specimen, used system of coordinates
and localization of the measuring points
Optimization of the welding technologies(high-strength ferritic steel WELDOX700)
Location ofmeasurements
150 mmTest weld
150 mm
2 mm3 mm10 mm
Three components of the residual stress scanned along the line perpendicular to the weld point
The usefulness of the neutron diffraction technique was demonstrated on the study of possible modification of the residual stress distribution in the vicinity of the single pass weld by weld-metal chemical composition. All three stress components sx, sy and sz were measured after releasing the test specimens from the test frame i.e. after removing the external restraint.
![Page 21: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/21.jpg)
Sample 1C Si Mn Cr Ni Mo0.100 - 1.85 0.42 1.94 0.39Sample 2C Si Mn Cr Ni Mo0.102 - 0.76 0.27 3.94 0.24Chemical composition of the weld metal labeled as OK 75.78 (weight %)
Sample 1-40 -30 -20 -10 0 10 20
-200
0
200
400
600
800 x component Y component z component
Stre
ss /
MPa
x / mm-3 0 -2 0 -1 0 0 1 0 2 0 3 0
-2 0 0
0
2 0 0
4 0 0
6 0 0
8 0 0
Stre
ss /
MPa
x / m m
x co m p one n t y co m p one n t z co m p on en t
Sample 2The result of the residual stress scans
C Si Mn P S Cr Ni Mo0.144 0.314 1.004 0.006 0.0013 0.372 0.057 0.019V Ti Cu Al Nb B N Ca0.047 0.015 0.016 0.043 0.020 0.0015 0.005 0.0024Chemical composition of the WELDOX700 steel (weight %).
Neutron diffraction technique was applied on stress scanning on two samples with the weld carried out by two different electrodes of different Ni content
![Page 22: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/22.jpg)
NPIResidual strain mapping: Austenite protection welded on a ferrite
AusteniteAusteniteFerriteFerrite
5 mm5 mm15 mm15 mm
Scanning pointsScanning points
110, 111 110, 111 -- reflection planesreflection planes
-5 0 5 10 15 20-4
-2
0
2
4
6
8
110 tangential 110 radial 111 tangential 111 radial
∆d /
d x
10-4
mm
Radial componentRadial component
Tangential componentTangential component
![Page 23: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/23.jpg)
Horizontally focusing monochromator
Monochromator shielding
Deformation machine
SamplePosition sensitive detector
NPI - TKSN-400 Strain/Stress Diffractometer
TKSN-400 Strain/Stress Diffractometer
Tensile force
Tensile force
![Page 24: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/24.jpg)
1V, 1500A
Neutron diffraction profile intensity phase volume fraction position strain/stress width/shape microstrain
Termo-mechanical loading
![Page 25: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/25.jpg)
Special deformation rig for tension/compression loading
Thermocouples Resistant heating system Water cooling system
Tension-compression rig
![Page 26: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/26.jpg)
( ) [ ]( )ξξ LGVRdd hkl ⊗⊗=Ω/ΣModeling in reciprocal space
( )
⟩⟨−−
−
−
2
02/12
0
22
21~
hkl
hkl
ddexpG πε
πξξ ( ) ( ) ( )220 221~
effhkl DdL
+−−
πξξ
⟨ε2⟩1/2 root-mean-square microstrainDeff effective dimension of coherently
diffracting blocks
Gaussian Lorentzian
Analysis of diffraction lineprofiles
Indirect deconvolution method
![Page 27: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/27.jpg)
Diffraction-line broadening
Observed profile Fexp(2θ)=[Finst⊗Fspec](2θ)Finst(2θ) = [Fwavelengtht⊗Faberration](2θ)
Specimen broadened profile Fspec
Size effect (Schrerrer, 1918)
θθβλcos)2(
KD =
Strain effect (Stokes&Wilson, 1944)“apparent strain”
Deconvolution Stokes method (Fourier transform) )()()(
exp
nFnFnF inst
spec=
Two-step indirect deconvolution method
e=β(2θ)cotgθ
![Page 28: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/28.jpg)
Energy-Dispersive Neutron-Transmission Diffraction
2dhkl sin Θ hkl = λ Θ hkl = 90ο λ =2dhkl
Diffraction edge I(λ) modulation
Instrumental resolution ∆d/d=5.7x10-4
![Page 29: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/29.jpg)
200 250 300 350
0.00
0.05
0.10
0.15Standard sample1 mm slit
Amplitud
e
Channel number
Sample thickness dependence of Ao
200 220 240 260 280 300 320 340-0.05
0.00
0.05
0.10
0.15
0.20
0.25
Standard sample2 mm slit
Amplitud
e
Channel number
FWHM=5.7x10-4 rad
FWHM=12.5x10-4 rad
200 250 300 350-0.2
-0.1
0.0
0.1
0.2
0.3
0.4
0.5 Fe(321) t=12 mm t=24 mm t=36 mm
Amplitud
e
Channel number
225 250 275 300 325-0,05
0,00
0,05
0,10
0,15
0,20
Deriv
ative
Channel number
ARMCO standard
Ampli
tude
Channel number
250 300-0,02
-0,01
0,00
ARMCO standard
EDNTD examplesBragg diffraction edge of a 8 mm thick sample
![Page 30: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/30.jpg)
Energy-Dispersive Neutron-Transmission Diffraction
1.5201.5221.5241.5261.5281.5301.5320.280.300.320.340.360.38
prestrain 10%tra
nsmiss
ion
wavelength (Å)
1.5201.5221.5241.5261.5281.5301.5320.320.340.360.380.40 prestrain 0%
trans
miss
ion
wavelength (Å)
1.5201.5221.5241.5261.5281.5301.5320.280.300.320.340.36 prestrain 2%
trans
miss
ion
wavelength (Å)
1.5201.5221.5241.5261.5281.5301.5320.280.300.320.340.360.38
prestrain 5%
trans
miss
ion
wavelength (Å)
low-carbon steel 0.22% C, 0.64% Mn, 0.41% Si, 0.035% P, 0.04% S (in wt.%) Fe (321) diffraction edges
![Page 31: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/31.jpg)
Comparison of the EDNTD and BDAA techniques
0 5 10 15 200.000.250.500.751.001.251.50
diffraction edge diffraction profile
micro
strain
< ε2 >1
/2 (1
0-3)
prestrain (%)
46.4 46.8 47.2 47.6 48.0
0
2
4
6
8
10
12int
ensity
/ rel
units
2θ / deg
5% strain
1% strain
110 reflection
![Page 32: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/32.jpg)
Residual stresses in highly radioactive materials
![Page 33: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/33.jpg)
Residual stresses in highly radioactive materials
Motivation...
reactor construction materials radiation damage - material degradation during
service monitoring of residual stress level with operation
time and neutron fluence component integrity assessment, support of
operation prolongation
![Page 34: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/34.jpg)
Dedicated shielding container
neutron beam n e ut ro
n be a m
specimen
shieldingshutter,collimator
linear stage
linear stagesteppingmotor
easy specimen installationin the hot cells
remote control of beamshutters and collimators
specimen positioning
![Page 35: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/35.jpg)
dedicated facility - shielding box, beam shutters, specimen manipulators
Residual stresses in radioactive reactor components
![Page 36: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/36.jpg)
First testing experiment
CT specimens from the steelA347 weld joint irradiated in experimental
reactor LWR-15 to 6.2 1020 n/cm-2
tested inside the in-pile reactor water-loop BWR-2 final fractured by fatigue at room
temperature in air total specimen activity of 11 GBq
weld metal
x z ybase metal
fusionline
fracturesurface
notch
![Page 37: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/37.jpg)
First testing experiment
0 10 20 30 40-300
-200
-100
0
100
200
300
400
µ strain
(a) active CT
x / mm0 10 20 30 40
-300
-200
-100
0
100
200
300
400
µ strain
x / mm
(b) reference CT
Scan of the residual strain component perpendicular to the fracture surface in the active specimen (a) and the reference specimen (b).Tensile residual strains of the same amplitude of ε ~3 10-4 located in the vicinity of the crack tip. Localization of the strain maximum is slightly different - irregular propagation of the crack tip
![Page 38: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/38.jpg)
Residual stresses in highly radioactive materials
Conclusions
All functions of the new experimental container have been proved
good shielding capacity mechanical functions in the hot cells easy and safe opening and closing the container installation of the specimen into the specimen holder
by using a mechanical manipulator remote control of specimen positioning and beam shutters
![Page 39: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/39.jpg)
Small-angle neutron scatteringmethod and its applications
![Page 40: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/40.jpg)
SANS instrumentation
i n c i d e n t b e a m
specimen
2-d PSD detector
Collimator system – pin hole geometry
![Page 41: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/41.jpg)
SANS instrumentationCollimator type SANScamera, slit geometry
Double bent crystalHigh-resolution SANScamera
Ultra high resolutionBonse-Hart SANS camera
![Page 42: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/42.jpg)
SANS instrumentation
SANS technique size rangeCollimator instruments 1 nm .. 100 nmDC diffractometers with bent crystals 10 nm .. 1 µmDC diffractometers with perfect crystals (Bonse-Hart) 1 µm .. 10 µm
Developed experimentaltechnique
Advanced data evaluationmethod & software− multiple scattering− Non-linear data fitting
of a single model tomultiple data sets
![Page 43: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/43.jpg)
-0.005 0.000 0.005 0.010
-0.005
0.000
0.005
0.010-0.005 0.000 0.005 0.010
-0.005
0.000
0.005
0.010
Q y (Å-1 )
Qx (Å-1)
14
56
2.2E2
8.9E2
3.5E3
-0.005 0.000 0.005 0.010
-0.005
0.000
0.005
0.010-0.005 0.000 0.005 0.010
-0.005
0.000
0.005
0.010
[111]
Q y (Å-1 )
Qx (Å-1)
Example of data taken by a neutron diffractometer and by a pin-hole instrument
![Page 44: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/44.jpg)
Example: Study of porosity in plasma-sprayed ceramics
1 10 1000.010.1
110
1001000
10000 z=5 mm
z=2.5 mm
empty beam
T=1730 oC
z dΣ
/dθ
Qx [ µm-1]
Bonse-Hart Collimator instruments0.01 0.1 1
0
20
40
60
80
100
120
140
0.1 10
5
10
15
as sprayed 1300 oC 1520 oC 1730 oC
D(R)
[10-2
µm-1]
R [µm]
SANS data for various resolutions and sample thickness fitted to a single model.
Size distribution of pores in plasma-sprayed Al2O3
![Page 45: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/45.jpg)
• High creep resistance• High-temperature applications (turbines)• Microstructure:
– two-phases: γ-phase matrix strengthened by γ’ precipitates or other phases
– Precipitate size: nm-µm, depending on heat treatment
– heat treatment: to optimize microstructure
• Characteristics of γ’ and/or other strenghtening phases essential formechanical properties
Ni-base superalloys
Composition: e.g. Cr 8.0, Co 4.0, Mo 0.5, Al 5.7, W 9.0, Ti 0.7, Ta 5.7, Ni balance; in wt%
![Page 46: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/46.jpg)
Ex-situ samples DT706, SANS
0.010.1
1
10
100
azimuthal average
Qx (Å-1)
dΣ/dΩ
(cm
-1sr-1
)
B DA-1 C B ST C B MST C B MST-1 C
0 500 10000.0001
0.001
0.01
size (Å)
volum
e dist
ributi
on (
dimen
sionle
ss)
volume distribution B DA-1 B ST B MST B MST-1
Model: dense spheres (γ’) with log-normal size distribution, large inhomogeneities, incl. η(Q-4 scattering)
STDAMST MST-1
![Page 47: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/47.jpg)
DT706
• Electron microscopy: uncertain about existence of precipitates in DA• Cooling/heating rate important (not only the hold temperature and time)• We can model well the data => in-situ behavior can be well assessed
0 500 1000 1500 2000 2500 30000
500
1000
1500
2000
2500
3000
DA-1
0.540 -- 0.600 0.480 -- 0.540 0.420 -- 0.480 0.360 -- 0.420 0.300 -- 0.360 0.240 -- 0.300 0.180 -- 0.240 0.120 -- 0.180 0.060 -- 0.120 0 -- 0.060
y (Å)
x (Å)0 2000 4000 6000 80000
2000
4000
6000
8000
ST
0.900 -- 1.00 0.800 -- 0.900 0.700 -- 0.800 0.600 -- 0.700 0.500 -- 0.600 0.400 -- 0.500 0.300 -- 0.400 0.200 -- 0.300 0.100 -- 0.200 0 -- 0.100
y (Å)
x (Å)0 2000 4000 6000 80000
2000
4000
6000
8000
MST
0.900 -- 1.00 0.800 -- 0.900 0.700 -- 0.800 0.600 -- 0.700 0.500 -- 0.600 0.400 -- 0.500 0.300 -- 0.400 0.200 -- 0.300 0.100 -- 0.200 0 -- 0.100
y (Å)
x (Å)0 2000 4000 6000 80000
2000
4000
6000
8000
MST-1
0.900 -- 1.00 0.800 -- 0.900 0.700 -- 0.800 0.600 -- 0.700 0.500 -- 0.600 0.400 -- 0.500 0.300 -- 0.400 0.200 -- 0.300 0.100 -- 0.200 0 -- 0.100
y (Å)
x (Å)
Volume fraction 5% 20% 13% 24%
![Page 48: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/48.jpg)
In-situ SANS (HTF furnace)
00:00 12:00 24:00 36:00 48:00 60:00 72:00 84:00-1000500
600
700
800900
1000
1100
1200
0.5 K/min4 K/min20 K/min
temperature
Temp
eratur
e (°C
)
Aim: Cooling rate (from solution treatment temperature) influence on precipitate microstructure
![Page 49: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/49.jpg)
Scattering curves (SDD=5m, λ=4.55Å and SDD=6m, λ=19.6Å)
• Carbides scattering: present even at solution treatment temperature 1080°C• 20 K/min: visible precipitation starts only during the 835°C hold, not before• 4 K/min: precipitation starts at 852°C• 0.5 K/min: Precipitates (majority of volume) created already before holding,
– starting at 890°C - most probably ηprecipitation
– accelerated at 865°C – γ‘ precipitation start.
1E-3 0.01 0.10.01
0.1
1
10
100
1000
DT70620 K/min
Q-4
azimuthalaverage
Q (Å-1)
dΣ/dΩ
(cm
-1sr-1
)measured, fit
1080°C 835°C, 1 min 835°C, 4 min 835°C, 23 min 835°C, 52 min 835°C, 1 h 26 min 835°C, 2 h 06 min 835°C, 3 h 28 min 835°C, 4 h 06 min 835°C, 9 h 32 min 835°C, 10 h 11 min room temperature after
1E-3 0.01 0.10.01
0.1
1
10
100
1000Q-4
DT7064 K/min
azimuthal average
Q (Å-1)
dΣ/dΩ
(cm
-1sr-1
)
measured, fit 1080°C 847°C 835°C, 1 min 835°C, 4 min 835°C, 38 min 835°C, 1 h 17 min 835°C, 8 h 45 min 835°C, 9 h 25 min room temperature after
1E-3 0.01 0.10.01
0.1
1
10
100
1000
Q-4
DT7060.5 K/min
azimuthal average
Q (Å-1)
dΣ/dΩ
(cm
-1sr-1
)
measured, fit 1080°C 857°C 847°C 835°C, 35 min 835°C, 1 h 14 min 835°C, 5 h 17 min 835°C, 6 h 36 min room temperature after
![Page 50: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/50.jpg)
Size (γ‘)
00:00 04:00 08:00 12:00 16:00 20:00 24:00 28:0040050060070080090010001100120013001400
Temp
eratur
e (K) Temperature
00:00 04:00 08:00 12:00 16:00 20:00 24:00 28:000
200
400
600
800
1000
1200
1400size - γ '
Time (hours)
size (
Å)
after coolling rate 0.5 K/min after coolling rate 2.3 K/min after coolling rate 4 K/min after coolling rate 20 K/min
0.0 0.3 0.6 0.9 1.2 1.50.0
0.3
0.6
0.9
1.2
1.5
y (µm
)
x (µm)0.0 0.3 0.6 0.9 1.2 1.5
x (µm)
Model: η and γ’
![Page 51: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/51.jpg)
Outcome
• Evolution of size and volume fraction for various cooling rates
• Microstructure can be tuned (γ’ size, distance) using the results of in situ SANS
• Cooling rate has to be properly chosen and accurately controlled during the heat treatment
• An indication of growth of η on expense of γ’ on holding after slower cooling.
![Page 52: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/52.jpg)
Radiation induced embrittlement in reactor pressure vessel steels
APT observation Nano-sized aggregates of solute atom are formed as a result of diffusion processes in crystal lattice damaged by neutron irradiation. Small-angle neutron scattering(SANS) permits to measure mean size and volume fraction of these aggregates.Additional information on chemical composition of the aggregates is obtained from the ratio of magnetic and nuclear scattering cross-sections
SANS model
ferromagnetic matrix
![Page 53: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/53.jpg)
Ldet = 4 m Ldet = 1.1 m
Measured (greyscale) and fitted (lines) scattering patterns from irradiated A533B steel (C1)
The SANS measurements were carried out at the BENSC-V4 instrument of the HMI Berlin
detector distances: 1.1 m and 4 m neutron wavelength: 0.6 nm horizontal magnetic field: 1.1 T
-3 -2 -1 0 1 2 3-3
-2
-1
0
1
2
3
Qx [nm-1] Q y
[nm-1 ]
-0.6 -0.3 0.0 0.3 0.6
-0.6
-0.3
0.0
0.3
0.6
Qx [nm-1]
Q y [n
m-1 ]
SANS experiments on RPV steels
Volume fraction is evaluated from the magnetic component modulated by ~ sin(α)2.
Mα
Q
![Page 54: Neutron scattering structure studies of materials loaded ...Neutron scattering structure studies of materials ... scanned along the line perpendicular to the weld point The usefulness](https://reader034.vdocuments.us/reader034/viewer/2022042018/5e76717a4790094600526418/html5/thumbnails/54.jpg)
10 1000.0
0.5
1.0
1.5
base
1.12 1024 m-2, 1y 5.89 1024 m-2, 5y 9.96 1024 m-2, 10y 1.411024 m-2, 5y, 475oC/165h 295oC / 10 y
D M(R
) [µm
-1]
R [Å]
Size distributions after subtraction of reference (unirradiated) sample (steel 15Kh2MFA).
10 1000.0
0.5
1.0
1.5
weld
1.22 1024 m-2, 1y 2.20 1024 m-2, 2y 5.26 1024 m-2, 5y 4.78 1024 m-2, 5y, 475oC/165h 295oC / 5 y
D M(R
) [µm
-1]
R [Å]
SANS experiments on RPV steels
Radiation-induced precipitates are recognized as a peak at R~ 0.1 nm