The using of synchrotron radiation timeresolved Xray diffraction experiment for kinetic investigatio

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The using of synchrotron radiation time-resolved
X-ray diffraction experiment for kinetic
investigation of SHS with millisecond time
resolution.

• B.P.Tolochko, M.R.Sharafutdinov, V.M.Titov,
  V.V.Zhulanov, A.S.Rogachev

Institute of Solid State Chemistry and
Mechanochemistry, Novosibirsk Budker Institute of
Nuclear Physics, Novosibirs Lavrentev Institute
of Hydrodynamic, Novosibirs Institute of
Structural Macrokinetics and Materials Science,
Chernogolovka
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Introduction

• The synchrotron radiation is a powerful
  instrument for study of SHS. At the last decade
  progress in this area was determined by progress
  in development of new specialized generator of
  synchrotron radiations - wigglers and undulators,
  installed at 3-th generation storage rings .
• So brilliance of SR is 1023 (photons/sec/mm2/mra
  d2 in 0.1 bandwidth) now and will reach 1035
  (photons/sec/mm2/mrad2 in 0.1 bandwidth) in the
  nearest future.

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The Synchrotron Radiation Spectrums

• Insertion devices produces light that is about
  one billion times more brilliant than
  conventional X-ray sources.

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What is Synchrotron Radiation?Synchrotron
radiation is emitted from an electron traveling
at almost the speed of light when its path is
bent by a magnetic field. As it was first
observed in a synchrotron in 1947, it was named
"synchrotron radiation".
Synchrotron radiation producedat an undulator
Synchrotron radiation producedat a bending
magnet
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Synchrotron radiation generation
SR
wiggler

• Storige ring

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Siberian synchrotron radiation center in the
Institute of nuclear physics SB RAS
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• The Generation of Synchrotron RadiationSynchrotr
  on radiation is produced at a bending magnet or
  at an insertion device. The insertion device is
  comprised of rows of magnets with alternating
  polarity and is installed in a straight section
  of the electron orbit. Corresponding to the weak
  and strong magnetic field, there are two types of
  insertion devices an undulator and a wiggler.
• Bending MagnetStored electrons run on a circular
  orbit and emit synchrotron radiation with a
  continuous spectrum when they encounter the
  bending magnet.
• UndulatorThe electron beam wiggles with a small
  deviation angle. As a result, ultra-bright and
  quasi-monochromatic light is obtained by the
  interference effect.
• WigglerThe electron beam wiggles with a large
  deviation angle. As a result, bright and
  spectrally continuous light with short
  wavelengths is obtained.

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• General Features of Synchrotron Radiation
• Ultra-bright
• Highly directional
• Broad continua (BM/W) or narrow bands (U)
• Linearly or circularly polarized
• Pulsed with controlled intervals
• High temporal and spatial stabilityBM Bending
  MagnetW WigglerU Undulator

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• Utilization of the Features of the SR Beam1)
  With the use of a microbeam, diffractometry of
  very small samples and microscopy with high
  spatial resolution are carried out.2)
  Time-resolved experiments are conducted on
  various time scales using a high speed shutter or
  a SR pulsed time structure.3) Energy tunability
  is effectively applied, for example, to atomic
  structure analysis using anomalous
  dispersion.4) By making use of highly
  collimated SR, various types of imaging
  techniques are developed with high spatial
  resolution.5) A linearly/spherically polarized
  beam is used especially for studies on the
  magnetic properties of materials.6) The
  availability of high energy X-ray beams enables
  high-Q experiments, Compton scattering, the
  excitation of high-Z atoms and the nuclear
  excitation of isotopes with high transition
  energy.7) With the use of coherence of X-rays,
  coherent X-ray optics, X-ray interferometry and
  X-ray photon correlation spectroscopy are made.

Professor V.V.Boldyrev in 1978 Synchrotron
radiation is an ideal instrument for Solid state
chemistry !
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History of Subject
Professor V.V.Boldyrev (April 2008)
Institute of Solid State Chemistry and
Mechanochemistry,

• V.V.Boldyrev motivation
• Kinetics of solid state fast reaction
• Intermediate states
• - Structure changes in local areas
• Mechanochemistry elementary act
• Relaxation of crystal structure

Budker Institute of Nuclear Physics
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Synchrotron radiation experimental hall at vepp-4
Indian Russian SR beamline VEPP-4 BARC/BINP
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Synchrotron radiation experimental hall at vepp-3
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Synchrotron radiation experimental hall at VEPP-3
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X-ray position sansativ detector OD-3M
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????? ????????? ??-3.
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??????????  35 ??????? ??????. ???? ??????
???????????  9 ??????? ??????.
OD-3-350 ?? ?????? ?? BL24XU-B (Hyogo prefecture
beamline, NIRO) SPring-8, Japan
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Position sensitive X-ray detector DIMEX with time
resolution 100 ns (prototype)
DIMEX is the Detector for IMaging of
E?plosions Goal perform dynamic imaging
synchronously with SR flashes from individual
bunches Design - GEM with drift gap and
microstrip signal PCB - gas mixture Xe/20CO2
at 7 bar - readout and DAQ based on PSIs IC
APC128 provided 32 x 100 ns frame-by-frame
measurements
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Introduction
WAXS
Density distribution at detonation front of TNT.
Time resolution 13 ns.
SAXS
Absorbsion, XAFS
Nano diamonds
realized
Test regime
future
Phase diagram of carbon
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Mechanochemical process realization
Nano diamond
v 0.1-12 km/s T 100 5000 C P 0.1 8 Mbar
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X-ray imaging of explosive during detonation
SAXS
Synchrotron radiation
T5000 C, P300 kbar
Detonation front
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Precursors preparation
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Phase transition of adamantan under shock wave
Under shock wave treatment the adamantan crystal
shape not change. It was found phase transition
adamantane ? diamond under shock wave
compression. Conclusion is made on base of this
experiment about breakup of the bond ?-?, rather
then ?-? in structure of adamantane. Conclusion
is made about high diffusions of hydrogens in
adamantane structure, carboxilates, tnt.
Diamond powder inside adamantan crystals
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Silver carboxilates shock wave compression
SAXS signal behavior from AgSt during detonation.
Silver nanoparticles cover by amorphous carbon
after shock wave treatment.
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Experimental setup of explosion experiment at
VEPP-3
products of detonation
detonation front
SAXS detector
VEPP-3
wiggler
electrons bunches
SR
transmitted beam detector
explosive
wires detectors
explosion chamber
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Synchrotron radiation experimental station for
explosion investigation
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Detonation front structure measurements with
using SR

Experimental setup on SR beam. Beam width H18
mm, thickness 0,4 mm. Exposure time 1 ns. DIMEX
detector strip width h0,1 mm.
Relatively density at detonation front of
explosives TNT/RDX 50/50, diameter 7 mm, 10 mm
and 12,5 mm.
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Las Alamos (LANL, protons) and Novosibirsk (BINP,
synchrotron radiation) experimental of density
measurements at detonation front

Las Alamos. Proton experiment. Comparison of the
density on axis from the MESA calculation density
(red line) estimated from a single frame in green
points for PBX9502.
BINP. SR experiment Experimental date received in
explosion experiment of TNT.
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Density measurement of explosion products after
detonation front with using synchrotron radiation
Synchrotron radiation

Density distribution.
Experiment setup.
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Reconstruction of 3D density distribution in the
detonation waves of the explosive trinitrotoluol
- hexogen
The use of X-ray radiation for research of
detonation is traditionally. However low
intensity of X-ray tubes limited opportunities of
a method and some of tasks remained unresolved.
In particular, small intensity not allowed to
investigate distribution of density behind front
of detonation because of too big experimental
errors. Use of SR has changed a situation the
dynamic range of measurement of intensity passing
through a sample have increased up to 104 , and
accuracy of definition of density improved up to
1 . Processing of the received images of
axial-symmetric samples has allowed to receive 3D
distribution of density behind front of a
detonation. The comparison of experimental
result with hydrodynamical simulation has shown,
that calculations do not take into account many
parameters and use erroneous constants.
Detonation front
SR irradiated area
Fig.1. X-ray tube image of detonated explosive
Abel equation treatment
Detonation front
Fig. 2. SR image of detonated explosive
Fig.3. Reconstructed 3D density distribution
behind detonation front
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Detonation and shock waves investigation
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Integral intensity of SAXS behavior for trotyl
during explosion
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Influence of free carbon on integral intensity of
SAXS behavior for different explosives
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Small angle X-ray scattering (SAXS) during
explosion
World record !
Small angle X-ray scattering experimental data of
RDX/TNT (50/50) during explosion. Each frame was
received with exposure time 1 ns and periodicity
125 ns. Accumulating regime from frame to
frame was used in this experiment.
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Influence of dispersion condition of detonation
products at nanodiamond nucleation
The SAXS signal time dependence from RDX-TNT
(50/50) with using PMMA tube with thickness no
tube - (1), 1,5 mm - (2), 3 mm - (3), 6 mm - (4).
The experiment setup for changing of dispersion
condition of detonation products. Detonator
(2), Explosive (2), PMMA muff (3), SR beam
(4), SAXS (5).
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The Equation of State for Nanocomposites
The technical realization of the dream
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Shock wave propagation in SiO2
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Shock-wave experiments at synchrotron radiation
beam line
Synchrotron radiation beam
Experiment set up 1- flat wave generator, 2- gun
tube, 3-plunger, 4-detonator, 5-detector, 6-
explosive, 7- sample.
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1-coordinate detector
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Shock wave in SiO2
Shadow imaging of the shock wave. Time
resolution 0.5 µs.
Velocity of shock wave in SiO2 .
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????????? ??????? ???? ? SiO2
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Shock-wave experiments at synchrotron radiation
beam line
Shock-wave adiabat reconstruction of aerogel by
shock-wave experiments at synchrotron radiation
beamline
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One impact SAXS from SiO2
v gt2.8 ??/?
v lt 2.8 ??/?
SAXS during one impact from high speed bullet
SAXS during one impact from low speed bullet
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Phase transition in SiO2 nanocomposite under
shock wave
v gt2.8 ?m/s
v lt 2.8 ?m/s
Dynamic of SAXS of SiO2 nanocomposite under
shock wave when vlt2.8 km/s. The microstructure
returned back.
Dynamic of SAXS of SiO2 nanocomposite under
shock wave when vgt2.8 km/s. The microstructure
was destroyed.
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Bullet velocity influence
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Bullet velocity influence
v gt2.8 ??/?
v lt 2.8 ??/?
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Silver stearate shock wave compression

a)
b)
c)
a) AgSt b) T2300
C, P248 kbar c) diamond
block structure.
Diamond
111 Ag
Diamond
200 Ag
5 nm
Ag nanoparticles capsulated in amorphous carbon
X-ray diffraction patterns of Ag and diamond
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SHS
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Self Propagation High Temperature Synthesis
(SPHTS) of NiAl investigation by X-ray
diffraction with 5 ms time resolution
Schema of experiment with DED5
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Test sample SiC
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Self Propagation High Temperature Synthesis
(SPHTS) of NiAl investigation by X-ray
diffraction with 5 ms time resolution
World record !
t 0 ms
t 10 ms
t 35 ms
NiAl
NiAl
t 20 ms
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Boldyrev V.V., Aleksandrov V.V., Tolochko B.P. et
al. Doklady Akademii Nauk SSSR, 1981, v.259, ?5,
p.1127-1129. Sharafutdinov M.R., Aleksandrov
V.V., Tolochko B.P Rogachev A.S. et al Journal.
Synchrotron Rad. (2003). 10, 384-386.
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Scheme of the experimental setup
Angular range 30 grad. Resolution - 3328
channels Exposition time 100 ?s and less
OD-3 detector
Sample
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The view of the actual experimental station
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• Using of this method for SHS allows to receive
  new, inaccessible earlier information - about
  phase transformation in chemical reaction zone,
  about formation of an intermediate phases, about
  behavior of the reagents crystalline lattice
  before reactions, and about relaxation process
  after reaction.
• At present time was reached following parameters
  of diffraction experiment for SHS locality - 5
  micrometers, time resolution - 1 ms, number of
  the frames - 1000.

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Peak brilliance of XFELs versus third generation
SR light sources. Bluespots show experimental
performance of the FLASH at the DESY.
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Electron bunch time pattern with 10 Hz repetition
rate and up to 3,000 bunches in a 0.6 ms long
bunch train. The separation of electron bunches
within a train is 200 ns for full loading. The
duration of electron bunches is 200 fs and the
non-linear FEL process reduces the duration of
the photon pulses to 100 fs.
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Schematic overview of the electron beam
distribution between accelerator and experimental
hall. The two electron beamlines (black) include
the five undulator systems for SASE FEL and
spontaneous synchrotron radiation, which in turn
feed five photon beamlines (red). The distance
between the separation into two electron
beamlines and the experimental hall is 1300 m.
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• ??????? ?? ????????
• Thank you for attention
• Welcome to Indian-Russian wiggler synchrotron
  radiation beamline at VEPP-4 !