Dubna material studies activity

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Dubna material studies activity in the frame of
IAEA and ISTC research projects
Anatoly Balagurov Frank Laboratory of Neutron
Physics Joint Institute for Nuclear
Research bala_at_nf.jinr.ru Dubna, Moscow
reg. Danas Ridikas Physics Section,
Division of Physical and Chemical
Sciences D.Ridikas_at_iaea.org Department of
Nuclear Applications and Science IAEA, Vienna

• High-resolution neutron diffraction
• Strain Size effects in diffraction patterns
• IAEA activity Coordinated Research Projects
• ISTC activity Research Project
• Collaboration with JINR Member States

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Neutron diffraction for material science
Crystal structure Magnetic structure -
crystal lattice - magnetic lattice -
crystal symmetry - magnetic symmetry -
atomic coordinates - magnetic moments
values - thermal parameters - magnetic
moments direction - occupancy factors Local
structure Microstructure - local
distortions - phase composition -
local correlations - crystallographic
texture - local disorder -
macrostresses - size strain
effects - structural defects
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High-resolution diffraction for peak shift and
broadening effects
I. Macrostress ? Peak shift ?a/a ?/E
For ?min 20 MPa and E 201010 Pa 200 GPa
(steel) we need in ?a/a 0.001
II. Peak broadening effects
Microstresses ? ?a/a Const 0.001
Size effect ? ?d/d d/2pWx
d 2 Å, Wx 300 Å, ?d/d 0.001
Very high resolution, R 0.001 or better, is
needed!
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High-resolution neutron powder diffraction
Short Pulse Sources ISIS, SNS, J-SNS,
Long Pulse Sources IBR-2, ESS,
Continuous Sources ILL, FRM-II, SINQ,
W 2 5 MW ?t0 (300 1500) µs
W 10 100 MW ?t0 8
W 0.1 1.2 MW ?t0 (15 30)? µs
Long FP L 100 m or fast chopper (Fermi /
Fourier)
? const diffractometer
TOF diffractometer
- ? 1.9 Å - Monochromator take-off angle
120º
- ? 0.5 - 4 Å - Flight-pass 20 m
Neutron pulse after fast chopper ?t0 (10 50)
µs
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Resolution of TOF-diffractometer
R(t, ?) ?d/d (?t0/t)2 (??/tg?)21/2
t Lsin?, R ? 0 if ?t0 ? 0 or L ? ?
and ?? ? 0 or ? ? ?/2
TOF-diffractometer ?d/d const 0.001 for d gt
2 Å.
HRFD, TOF, 20 m (IBR-2)
HRPD, TOF, 100 m (ISIS)
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NAC standard (Na2Al2Ca3F14) on TOF and ?0
diffractometers
HRPT (?0) ?01.886 Å, 2?10-165?
HRFD (TOF) 2?0152?, ?1.27.2 Å
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Neutron spectrometers on the IBR-2M reactor
Diffraction (6) HRFD, DN-2, SKAT, EPSILON,
FSD, DN-6 SANS (2) YuMO, SANS-C Polarized
neutron reflectometry (3) REMUR, REFLEX,
GRAINS Inelastic scattering (2) NERA, DIN
13 spectrometers (3 new) 3 cold moderators (new)
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TOF diffractometers at the IBR-2M
1. HRFD high resolution Fourier
diffractometer crystal structure of powders,
anisotropic broadening
2. DN-2 multi-purpose diffractometer single
crystals, magnetic structures, real-time studies
3. DN-12 (DN-6) diffractometer for
microsamples high pressure experiments
4. FSD Fourier (RTOF) stress diffractometer int
ernal stresses in bulk samples
5. EPSILON TOF stress diffractometer internal
stresses in bulk samples
6. SKAT texture diffractometer texture of
rocks and bulk samples
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Diffraction at the IBR-2M. Resolution.
HRFD powders, stresses FSD stresses DN-2 real-ti
me, multilayers DN-6 high-pressure EPSILON
stresses SCAT textures
Resolution becomes better for longer d-spacing!
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HRFD High Resolution Fourier Diffractometer at
IBR-2
Put into regular operation in 1994 by
collaboration FLNP (Dubna), PNPI (Gatchina),
VTT (Espoo), IzfP (Dresden).
HRFD (Dubna) lt2?gt 152º ?t0 const ? 10 ?s
L ? 21 m ?d/d const 0.001 for d gt 2 Å
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Fast Fourier chopper at HRFD (Dubna)
0.7 mm
Rotor
Stator
Dubna chopper Al-alloy ? 50 cm N 1024 ltdgt
0.7 mm Vmax 6000 rpm O 100 kHz ?t0 10
µs Transmission 0.25 Sbeam 3x30 cm2
7.5 kW motor
Triangular chopper transmission function
T(t) 1 sin ?t
Binary pick-up signals for RTOF analyzer
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Rietveld analysis of the HRFD data (MRIA package)
Diffraction pattern obtained with NAC-standard,
?d/d 0.001
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HRFD detectors around sample position
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Size and strain broadening of diffraction
lines
W2 C1 C2d 2 C3d 2 C4d 4
Size of domains, C4 (1/L)2
Microstresses, C3 (?a/a)2
Resolution function of TOF-diffractometer
W2(d 2) function for NAC and Al2O3 standard
samples
Peak width for nanosized Ni with ltDgt 380 Å.
Microstresses in CaCuMn6O12 for two temperatures
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Applied researches at the IBR-2
steel
Zr
A part of the real VVER-1000 vessel(built-up
welding stainless steel)
Cross-section of the bimetallic steel-zirconium
adapter
Perforators striker
Biaxially fatigued stainless steel sample of
cruciform geometry
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IAEA project D2.01 Enhancement of research
reactor (RR) utilization and applications

• List of major activities
• RR coalitions networks
• Research Reactor Data Base (RRDB)
• Coordinated Research Projects
• Technical (TM) and Consultancy (CM) Meetings
• International RR Conference, Workshops, Schools
• Support of national regional TC projects
• Publications, technical reports, brochures

NEW !
More information available at http//www-naweb.ia
ea.org/napc/physics/research_reactors
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New RRDB capability utilization applications
oriented
Available at http//www-naweb.iaea.org/napc/physi
cs/research_reactors/ or USB Memory Stick, lt10MB,
no internet is needed!
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New RRDB capability utilization applications
oriented
44 RRs employ neutron beams they are distributed
over 30 MSs
Available at http//www-naweb.iaea.org/napc/physi
cs/research_reactors/ or USB Memory Stick, lt10MB,
no internet is needed!
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IAEA activity Coordinated Research Projects
CRP 1314 (2006-2009) Development and application
of the techniques of residual stress
measurements in materials
Objectives ? characterization, tests and
development of materials ? development of new
instruments upgrade of existing facilities ?
advanced analysis of material stresses links to
industrial partners ? harmonisation and
standardization procedures (e.g. round robin
experiment) ? 5 Research Contracts 4 Research
Agreements

1. Czech Republic
2. Germany
3. Hungary
4. India
5. The Netherlands
6. Pakistan
7. Romania
8. Russian Federation
9. South Africa

Main achievements/outlook ? Creation of network
on residual stress ? Transfer of know-how from
RA holders to RC (developed ? developing) ?
Round Robin experiments are ongoing (USA,
Australia, UK) ? Project report for Technical
Report Series is in preparation
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Application of Reverse Time of Flight (RTOF)
Neutron Diffraction for Residual Stress
Investigations
The main tasks of the project were devoted to
modernization of the main units of FSD
diffractometer 1) Installation of new detector
modules 2) Precise sample alignment system
improvement 3) Adaptation of the new mechanical
testing machine for tensile/compressive test
with force and temperature control.
90º-detector system based on ZnS(Ag) scintillator
with wavelength-shifting fibers
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FSD diffractometer
Backscattering detector
Status of the detector system Six modules of
ZnS(Ag) 90 (on the left) and -90 (on the
right) detectors are currently installed on
FSD. Two new modules are in preparation.
90º-detector
Sample position
Neutron guide
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IAEA activity Coordinated Research Projects
Active CRP 1575 (2009-2012) Development,
Characterization and Testing of Materials of
Relevance to Nuclear Energy Sector Using Neutron
Beams (SANS, diffraction and neutron
radiography)
Objectives investigation and characterization
of materials relevant to nuclear energy
applications optimization and validation of
experimental and modeling methods creation of a
database of reference data for nuclear materials
research enhancement of the capacity of research
reactors for nuclear materials research ? 8
Research Contracts 9 Research Agreements

1. Argentina
2. Australia
3. Brazil
4. China
5. Czech Republic
6. France
7. Germany
8. Hungary
9. Indonesia
10. Italy
11. Japan
12. Korea
13. The Netherlands
14. Romania
15. Russian Federation
16. Switzerland
17. USA

Expected output Materials characterized,
experimental/modelling methods optimized
Creation of multilateral network in the field of
advanced nuclear materials research Creation of
an experimental reference database for models and
calculations Final project publication
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Ferrite-Martensite Steels Dispersion Hardening
Studied by TOF Neutron Diffraction
Scientific scope of the project
Relation between dispersion-hardening particle
size and microstress value in steel. The
influence of these parameters on strength
characteristics of steels at various temperatures.
Subject of studies
High-strength dual-phase ferrite - martensite
steels (soft ferrite matrix containing islands of
martensite) with dispersion-hardened phases
Fe-12Cr matrix V/Mo/Nb carbides (EP-450),
V/W/Nb nitrides (EP-900), EP-450 ODS (oxide
dispersion strengthened by Y2O3).
Experimental technique
High-resolution TOF neutron diffraction with
high-temperature in situ loading.
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• Five main topics to be addressed
• Utilization Applications of RRs
• Operation Maintenance
• New RR Projects
• Safety of RRs
• Spent Fuel Management, Waste Decommissioning
• Jointly by NA, NE, NS and TC
• Contact D. Ridikas_at_iaea.org

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ISTC project ? 3074.2
Neutron-Diffraction Study of Micro- and
Macrostresses in Structural Ageing Alloys for
Nuclear Power Engineering after Thermal and
Radiation Exposure and Predicting Resistance to
Radiation-Induced Swelling
Participants Institute of Metal Physics,
Yekaterinburg Joint Institute of Nuclear
Research, Dubna Institute of Technical
Physics, Snezhinsk Period of
realization September, 2008 February, 2011 (30
months) Budget 253,229 Euro Foreign
Experts Dr. Rainer Schneider, Berlin Dr.
Carsten Ohms, Petten Dr. Pavol Mikula, Prague
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ISTC project ? 3074.2
First task microstresses in the bulk of the
components from radiation-resistant ageing alloys
in the course of formation, growth and
coagulation of the second-phase disperse
particles. Steels with coherent Ni3Ti
intermetallic precipitates, semi-coherent and
incoherent VC carbides will be studied.
Second task analysis of microstresses around
defect clusters formed in place of displacement
cascades under neutron irradiation.
Third task investigation of residual macro- and
microstresses arising as a result of phase and
structural transformations in steel and alloys,
predominantly in the thermally affected zone of
weld seams of large-diameter pipes.
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Austenitic steel Fe0.748Mn0.179V0.013Cr0.042C0.018
with VC precipitates
Three samples have been studied after quenching
from 1100ºC initial, annealed at 600?? and
700??. Annealing time was 1, 6, and 12 hours.
The lattice parameter dependence for 40?4?18?
steel vs. annealing time at two
temperatures 600?? and 700??.
The strain (?a/a) dependence for 40?4?18? steel
vs. annealing time at two temperatures 600?? and
700??.
Comparison of diffraction patterns for 40?4?18?
steel samples initial and aged at 600?? and
700?? in 12 hours.
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Investigation of the atomic and magnetic
structures of crystals and internal stresses in
bulk materials and components
In the frame of JINR NECSA project Neutron
Scattering Applications
Co-ordinator from JINR Dr. Anatoly M.
Balagurov Co-ordinator from NECSA (South
Africa) Dr. Anrew M. Venter
1. Instruments development 2. Joint experiments
Stresses in biaxially fatigued stainless steel
sample of cruciform geometry Residual stresses
in a stainless steel-Ti(Nb) bimetallic tube
adapter
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Joint experiment in 2009/2010
Residual stresses in biaxially fatigued
stainless steel sample of cruciform geometry
SALSA (ILL, France) POLDI (PSI, Switzerland
Metastable austenitic stainless steel AISI 321
were subjected to the in-plane biaxial
tension-compression fatigue cycling on the
INSTRON planar biaxial loading machine at FIMS
(Bremen). Residual stresses in to the ex-situ
in-plane biaxial low cycle fatigued sample of the
cruciform geometry from AISI 321 were measured
at SALSA (ILL) and POLDI (PSI) instruments.
Spectra from the martensite (left side) and
austenite (right side) in the Krest-2 sample
measured on the SALSA.
(211) martensite
Vg 0.5 mm3 texp 20 to 35 min.
(220) austenite
Biaxially fatigued stainless steel sample of
cruciform geometry at POLDI (SINQ neutron source,
PSI).
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Joint experiments in 2010/2011
Residual stresses in a stainless
steel-titanium/niobium bimetallic tube adapter
POLDI diffractometer at SINQ, PSI (Villigen,
Switzerland)
Stainless steel-titanium bimetallic tube adapters
are being considered for use in superconducting
radiofrequency cavities. Hermetic welding of the
adapter is achieved by explosive bonding method.
The residual stresses into the adapter are of
large practical interest for the improvement
of explosive welding technology and
minimization of the production cost.
A set of samples are prepared for investigation
of residual stresses in bimetallic joining.
Bimetallic tube is placed at the POLDI
diffractometer, SINQ neutron source, PSI.
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User program at the IBR-2M spectrometers
Time-sharing (13 spectrometers)
FLNP (35)
International experts commissions
External fast (10)
I. Diffraction II. Inelastic Scattering III.
Polarized neutrons IV. SANS
External regular (55)
User statistics
Others, 19
FLNP, 25
France, 3
Poland, 5
Germany, 17
Russia, 31
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You are invited for experiments at the IBR-2M
reactor in Dubna a nice place at the Volga
River