Measurements of SAXS signal during TATB detonation using Synchrotron radiation K.A. Ten 1, V.M. Titov 1, E.R. Pruuel 1, I.L. Zhogin 2, L.A. Luk’yanchikov

Measurements of SAXS signal during TATB

detonation using Synchrotron radiation

K.A. Ten1, V.M. Titov1, E.R. Pruuel1, I.L. Zhogin2, L.A. Luk’yanchikov1, B.P. Tolochko2 , Yu.A. Aminov3,

V.P. Filin3 , B.G. Loboyko3, A.K. Muzyrya3, E.B. Smirnov3

1Lavrentiev Institute of Hydrodynamics, Novosibirsk, Russia2Institute of Solid State Chemistry and Mechanochemistry, Novosibirsk, Russia

3RF-NC VNIITF, Snezhinsk, Russia

XIV International Detonation Symposium, April 11-16, 2010, Coeur d`Alene, Idaho

The problem of carbon condensation at detonation of oxygen-deficient high explosives is still open to question. It is important both for understanding the

physics aspect of the phenomenon and for evaluation of the amount of energy released at exothermic coagulation of carbon clusters.

According to literature data on comparison of computational and experimental data on acceleration of very thin metal plates by products of detonation of oxygen-deficient

high explosives, such process is described with a better accuracy under an assumption of carbon condensation behind the chemical reaction zone, or as is

the convention in the detonation theory, behind the Chapman-Jouget plane, which separates the reaction zone from the gas-dynamic flow of the explosion products

[1,2].For the time being, sizes of condensed carbon nano-particles at explosion of high

explosives can be experimentally registered only through diffraction methods using synchrotron radiation (SR) [3].

1. J. A. Viecelli, F. H. Ree. Carbon particle phase transformation kinetics in detonation waves.//Journal of Applied Physics, Vol 88, Num 2, 2000, p 683—690.

2. K.F.Grebenkin, M.V.Taranik, A.L.Zherebtsov. Slow energy release in detonation products of HMX-based explosives: computer modeling and experimental effects.// Zababakhin scientific talks, International Conference, Snezhinsk, Russia, 10-14 September, 2007, p. 76

3. V.M.Titov, B.P.Tolochko, K.A.Ten, L.A.Lukyanchikov, E.R.Pruuel. Where and when are nanodiamonds formed under

explosion ? //Diamond & Related Materials. V.16, Issue 12, 2007. P. 2009-2013.

Introduction.


Acquisition of experimental information on the time history of condensed carbon nano-particles at detonation of oxygen-deficient high explosives.

Problem

Methods

Dynamical recording of small-angle X-ray scattering (SAXS) of synchrotron radiation from the VEPP-3 accelerator. Application of highly-periodic synchrotron radiation (SR) from the accelerator complex VEPP-3 to measuring SAXS with exhibition for 1 ns allows tracing development of the signal in the course of detonation of high explosives.

Cylindrical samples of 15 mm (TNT and TNT/RDX) and 20 mm (TABT (1,3,5-triamino-2,4,6-trinitrobenzol, standard 11903-538-90) and PCT (TABT-based plasticized compound, standard 75 11903-539-90)) in diameter were under study.

Samples


wigglerSR

VEPP-3

Explosionchamber

Transmitted beamdetector

detonationfront

Electron bunches

detonation products

SAXS detector

explosive

beryllium windows

Pulse period – 250 ns, frame time - 1 ns

4Setup of explosion experiment at VEPP-3


Acceleration complex Acceleration complex VEPPVEPP-3 - -3 - VEPPVEPP-4 -4 is the is the basis of the detonation experimentsbasis of the detonation experiments

4.

Detector KEDR

ROKK-1M


View of an explosion lens with a primary charge near it.

Experimental assemblies

General view of an experimental assembly.


Small-angle X-ray scattering (SAXS) measurements at detonation of HE

2 2

0 2

[(sin ) (cos ) cos(2 )]i T

R

rdriqrnqE

)exp()(4

1)(

0kkq4

2Sin

kSin

)()()(1

),(3

qRCosqRqRSinq

nRqE

2 is the scattering angle,


SAXS signal versus the scattering particle diameter in TNT. The calculations were performed subject to the VEPP-3 spectrum and spectral sensitivity of the DIMEX

detector. The angle is given in the numbers of the detector channels.


0 10 20 30 40 50

0,0

0,2

0,4

0,6

0,8

Channels

SA

XS

C d = 2 nm D d = 4 nm E d = 10 nm F d = 20 nm G d = 200 nm

VEPP-3, TNT, d=20 mm


Dependence of the form-factor on the size of the scattering spheres.



Computed angular dependence of SAXS on the TNT charge thickness. The calculations were performed subject to the VEPP-3 spectrum and spectral sensitivity of

the DIMEX detector. The angle is given in the numbers of the detector channels.

.

0 10 20 30 40 50

0,0

0,2

0,4

0,6

0,8

1,0S

AX

S

Channels

L=1cm B C 1.5 cm D E 2.0 cm F G

D=5 nm

Contrast influence


The yellow arrow denotes the incident SR beam; the violet cone designates the

X-ray scattering on carbon nano-particles.

Detonation products

Sample of HE

SR

detector DIMEX

SAXS



014,02 max

0006,02 min

rad

Rad,

Dmax = π/qmin = λ/(4θmin) = ~ 75 nm.

Dmin = π /q max = λ/(4θmax) ≈ 2,0 nm,

SAXS distributions at detector tuning. D is for SR beam closure by blade K3, B is for SAXS from the sham, C is for position of the borderline of the SR beam (passed radiation). The angle is given in the numbers of the detector channels.


180 190 200 210 220 230 240 250 260-500

0

500

1000

1500

2000

2500

3000

3500

4000

SA

XS

Channels

B C D


The angular dependencies of SAXS signal at detonation of a ТATB sample. Different colors show frames recorded with an interval of 0.5 μsec. Frame Q

corresponds to the detonation front. The angle is given in the numbers of the detector channels.

.

Small-angle X-ray scattering (SAXS) measurements at detonation of HE.

150160170180190200210220

0

500

1000

1500

2000

2500

3000

D E F G H I J K L M N O P Q R

SA

XS

ChannelsFrames


The angular dependencies of SAXS signal at detonation of ТNT.



Determination of nano-particle sizes by the Guinier formula

).3/exp()0()( 22gRqIqI

3/))(ln( 220 gRqLnIqI

Sinq

4

θ = h 10-4 -1 0 1 2 3 4

2,0

2,5

3,0

3,5

4,0

4,5

5,0

5,5

ln(I

q)

q2 ,(1/nm)2

Type_538 t = 0,5 mkS

C Linear Fit of Data12_C

SAXS distribution behind the detonation front in TATB with an interval of 0.5 μsec. The red line (by the Guinier

formula) corresponds to the particle size D - 2.5 nm.


Nano-particle size versus time at trotyl/hexogen (50/50)

detonation.



Nano-particle size versus time at TABT detonation.

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5 4,0 4,5

1,5

2,0

2,5

3,0

3,5

Siz

e,

nm

Time, mkS

Type_538 C 802 D 798 E 799 F Average


Measurement of small angle X-ray scattering (SAXS) on nano-particles

Dependence of integral SAXS signal on time at detonation of trotyl/hexogen (50/50), TNT, and TABT


The measured SAXS distributions show that nano-particles of d~2.5 nm are registered immediately after the detonation front. Then the particle size is increasing weakly and reaches d 4-5 nm by the moment t=3 μs, in TNT/RDX. In TNT and TATB charges, the growth of particles is slower: by the same time, their size is d2.5 nm for TATB and d4 nm for TNT. Thus no traces of nano-diamonds were registered at detonation of TABT samples of 20 mm in diameter. Even if there are such nano-diamonds, their size does not exceed 1 nm. The arising graphite-like particles are of d 2.6 nm .

Conclusions



Thank you for your attention!

Благодарю за внимание!




Determination of nano-particle sizes from the Guinier formula

Nano-particle size versus time at PCT detonation.

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5 4,0 4,51,3

1,4

1,5

1,6

1,7

1,8

1,9

2,0

2,1

2,2

2,3

2,4

2,5

2,6

Time, mkS

Siz

e,

nm

Type_539 C 807 D 809 E 805 F Average


Documents

Measurements of SAXS signal during TATB detonation using Synchrotron radiation K.A. Ten 1, V.M. Titov 1, E.R. Pruuel 1, I.L. Zhogin 2, L.A. Luk’yanchikov