Post on 15-Apr-2022
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Themes:Metals thermal EOS and melting: Pt Simple diatomics‐molecular dissociation: H2, D2, N2, O2 Minerals: MgO Noble metals‐thermal conductivity: Ar
Challenges:Materials characterization under extreme conditions of high P‐T ‐strain rate New materials synthesis under extremes including non‐equilibrium conditions
Time-domain experiments in diamond anvil cells
Alexander Goncharov
Geophysical Laboratory, Carnegie Institution of Washington
New pulsed laser and X‐ray techniques: Pulsed laser heating Ultrafast laser pump‐probe techniques Combined Xray synchrotron‐pulsed laser experiments Laser driven shock compression in the DAC
NSLS-II
Delay Time (ns)0 200 400 600 800
Rea
ctio
n Pr
oduc
t (ar
b. u
nits
)
0
20
40
60
80
100 Induction Reaction
Probe
D. A. DaltonV. V. StruzhkinM. SomayazuluR. J. Hemley
S. R. McWilliamsM. Mahmood
M. R. ArmstrongJ. C. Crowhurst
V. PrakapenkaI. KantorM. Rivers
LLNL
GSECARS, APS, ANL
Howard University
Acknowledgements
NSFDOE BES (EFree)DOE NNSA (CDAC)DCOAROCIW
Geophysical Laboratory
Support
Carnegie Washington DC campus
Scientific challenges: bridge the gap between static and dynamic experiments in P‐T‐strain rate conditions reached & probed
Pressure (GPa)
10 100 1000
Tem
pera
ture
(K)
100
1000
10000Hugoniot
DAC limit
Theory
Proposed shock in DAC (sketch)
Melt lineMelt line
Hugoniotprecompressed
Jupiter isentrope
Reverberating shock
Dissociation
Orientationallydisordered
solid
Orientationallyordered solids
Fluid?
Molecular fluid
Atomic fluid?
Hydrogen
Proposed pulsed heating (sketch)
QuantumMonte Carlo
Phase diagram of hydrogen
Gap
Extreme P‐T conditions are relevant for:‐warm dense matter‐new materials synthesis‐fast chemical reactivity‐materials strength‐melting curves‐ planetary interior
Here we propose to combine static and dynamic experiments in the DAC by performing• pulsed laser heating• laser driven shock in the DAC
Melting phenomena and properties of fluids at high P‐T condition
New techniques are needed to enable accurate measurements of melting phenomenaimproved laser heating techniques:
Time‐resolved X‐ray & optical techniques : diffuse peak in XRD XAS spectroscopy elastic, optical, and vibrational properties
Shock & static experiments disagree by 1000’s K
Dramatic decline of melting line?!Diagnostics of melting is scarce
Problems with static methods• Instabilities (e.g., diffusion)• chemical reaction• indirect criteria and lack of positive observations
Guillaume et al., 2011
Wavelength (nm)580 600 620 640 660 680
Inte
nsity
(arb
. uni
ts)
0
20
40
60
80
100Planck Fit, T=10570±190 KMeasurements
Pulsed versus continuous laser heating in the DAC
Continuous Heating
Radial distance (10-6m)0 10 20
Axia
l Dis
tanc
e (1
0-6 m
)
-4
-2
0
2
4 400 600 800 1000 1200 1400 1600
Axia
l Dis
tanc
e (1
0-6 m
)
Pulsed Heating
Radial Distance (10-6m)0 10 20
-4
-2
0
2
4 500 1000 1500 2000 2500 3000 3500 4000
Time (10-6s)
0.0 2.0 4.0 6.0 8.0 10.0
Tem
pera
ture
(K)
0
500
1000
1500
Continuous heating after turning on power
0.00 0.05 0.10
Pow
er (W
)
0
5
10
15
20
Power ramp
Time (10-6s)0.0 0.1 0.2
Tem
pera
ture
(K)
0
1000
2000
3000
4000
Pulsed heating
0.00 0.02 0.04
Pow
er (W
)
0
400
800
Temperature histories (FE calculations)
Finite element calculations, mapsPulsed laser heating: experiment
Measurements are very challenging (small volume, strong thermal radiation)Uniform in space and time heating in the DAC require longer pulses
Time‐domain experiments in laser heated DAC:thermal radiation & chemical reactivity suppression
Pulsed heating (ns and s): we discriminate spatially and temporally (by measuring ~5‐10 s after the arrival of the heating pulse).
Timing for pulsed heat + pulsed Raman operation:
A. F. Goncharov & J. Crowhurst (2005); Goncharov et al., 2008; Goncharov et al., 2010
Temperature Map
Radial Distance (s)
0 5 10
Axia
l Dis
tanc
e (
s)
-2
0
2
400 600 800 1000 1200 1400 1600 1800
Coupler
T map: FE calculations
Time (s)
5 10 15 20
Tem
pera
ture
(K)
500
1000
1500
2000
T coupler T center Laser Pulse
Intensity (arb. units)
Measurement
before after
Time‐Resolved Raman Spectra of Hydrogen with double‐sided microsecond laser heating
Sample: H2, Ir Coupler P = 10‐25 GPa
Time‐domain experiment
Timing
Raman excitation
S. R. McWilliams
Raman spectra
Fluid
Laser heating
Raman shift (cm-1)
3900 4000 4100 4200 4300
Inte
nsity
(rel
ativ
e un
its)
445 K
815 K
1200 K
1500 K
1800 K
300 K
Raman spectraCW excitation 60 GPa
Rapidly collected Raman spectra showmodified intramolecular bonds above40 GPa.Subramanian et al. PNAS, 2011
0.16 0.20 0.24 0.28 0.32 0.36 0.400.0
0.3
0.6
Inte
nsity
, a.u
.
Time, ms
up to 50 kHz
Goncharov, Struzhkin, Prakapenka, Kantor, Rivers, Dalton
X-ray diffraction combined with pulsed laser heating
1‐50 μs, 5‐20 KHz
Time‐resolveddetector: Pilatus
Pulsed fiber laserSpectrograph & Intensified gated CCD detector
Thermal radiation
Sector 13: GSECARSX‐ray
Diffraction
Laser
Pulse generator
Pulsed laser heating in the DAC: s timescales
GL: A. Goncharov, V. Struzhkin, A. Dalton; GSE CARS: V. Prakapenka, M. Rivers, I. Kantor
Time-resolved X-ray diffraction
8 12 16 20
1
2
Inte
nsity
, a.u
.
2-theta, degree
Detection of melting
Pt
Time (s)
T (K
)
0
1000
2000
3000
Uni
t Cel
l Vol
ume
(A3 )
54.5
55.0
55.5
-20 0 20 40 60 80 100 120
Rel
etiv
e In
tens
ity Pulse profile
Unit Cell Volume FE calculated temperatures:
surfacecenter
Pulse profile vsThermal expansion & temperature histories
Tm Pt 38 GPa
Optical Pump‐Probe System for Time Domain Thermoreflectance experiments use a double modulation approach
AlAl AdCQRT )1(
MgO
Aluminum
DAC
Sample cavity
Argon
Pump + Probe
D. Dalton, A. Goncharov, W.‐P. Hsieh, D. Cahill
Fianium LaserWavelength: 1064 nm
Rep Rate: Single Shot to MHzEnergy: 2 μJ, Pulse Width: <10 ps
Peak Power: ~20 kW
DelayStage
PhotonicCrystalFiber
½ WP
Polarizer
1064, 532 nm mirrors
Spectrometer with Gated Detector
(300nm‐780 nm)
BroadbandmirrorsBroadband, chirped
Source for CARS
Narrowband fundamental
DAC10 x
Objective
10 xObjective
KTPDoubling crystal
Long passfilter
532 nmnotchfilter
Short passfilter
532 nmnotchfilter
Heating Laserμs scale pulse
We are developing a new coherent Antistokes Raman and broad band spectroscopy systems
D. A. Dalton, McWilliams
The supercontinuum data was collected in a single shot manner at ~180 nJ/pulse into the fiber
Tungsten lamp (~3000 K) data collected at 103 longer accumulation time.
Broadband Optical Spectroscopy will enable single shot study of optical properties at the extreme environments attainable in the DAC.
Supercontinuum Generation (SG) results in a very bright, white light source.
D. A. Dalton & S. McWilliams
lens
lens
nonlinear fiber
insulator
sample
Transient extreme conditions;diamond anvil cell combined withpulsed laser heating.
Time‐domain optical spectroscopy in the diamond‐anvil cell.
background
Heating pulse
transmittedprobe
600‐760 nm
Oxygen, absorbance with P & T
Ultrafast absorption spectroscopy usingsuper‐continuum optical probe.
heating laser
super‐continuum probe
present probe: 400 to 850 nm
20 picosec.
25 GPa
60 GPa
45 GPa
25 GPa
7 GPa
T
T
T
PCF fiber output
Goncharov, McWilliams, Dalton, Geophysical Lab
First Sweep of the Supercontinuum using a streak cameraWavelen
gth (arb. units)
Coherent Anti Stokes Raman Spectroscopy (CARS) will be used for time resolved chemistry in the DAC
ωpump
ωStokes
ωCARS
CARS has better conversion efficiency that RamanCARS can discriminate from fluorescense and thermal backgroundCARS does have non‐resonant background
λ=532 nm
λ= 532 nm‐2 μm
ωprobe
ωpump
ωStokes
ωCARS λ= ~300‐532 nm
CARSRaman Effect
=ωprobe
ωmolecule
Rayleigh Anti‐StokesStokes
ω0 ω0ω0 ‐ ∆ω ω0 + ∆ω
ωmolecule =ωpump ‐ ωStokes
Second harmonic Supercontinuum
Broadband Coherent Anti‐Stokes Raman Spectroscopy (CARS) is planned to perform single shot study of optical properties at the extreme environments attainable in the DAC: first tests at CIW
Dalton, McWilliams, & GoncharovRaman Shift (cm-1)
1000 2000 3000
Inte
nsity
(arb
. uni
ts) CARS, 532 nm
Raman, 457 nm
CARS spectra with supercontinuumFianiumLaser
Wavelength: 1064 nmRep Rate: Single Shot to MHz
Energy: 2 μJ, Pulse Width: <10 psPeak Power: ~20 kW
DelayStage
PhotonicCrystalFiber
½ WP
Polarizer
1064, 532 nm mirrors
Spectrometer with Gated Detector
(300nm‐780 nm)
BroadbandmirrorsBroadband, chirped
Source for CARS
Narrowband fundamental
DAC10 x
Objective
10 xObjective
KTPDoubling crystal
Long passfilter
532 nmnotchfilter
Short passfilter
532 nmnotchfilter
Heating Laserμs scale pulse
CARS spectra with supercontinuum at CIW
Methanol 0.5 GPa
Broadband Coherent Anti‐Stokes Raman Spectroscopy (CARS) is planned to perform single shot study of optical properties at the extreme environments attainable in the DAC: first tests at CIW
Dalton, McWilliams, & Goncharov
CARS spectra with supercontinuumFianiumLaser
Wavelength: 1064 nmRep Rate: Single Shot to MHz
Energy: 2 μJ, Pulse Width: <10 psPeak Power: ~20 kW
DelayStage
PhotonicCrystalFiber
½ WP
Polarizer
1064, 532 nm mirrors
Spectrometer with Gated Detector
(300nm‐780 nm)
BroadbandmirrorsBroadband, chirped
Source for CARS
Narrowband fundamental
DAC10 x
Objective
10 xObjective
KTPDoubling crystal
Long passfilter
532 nmnotchfilter
Short passfilter
532 nmnotchfilter
Heating Laserμs scale pulse
CARS spectra with supercontinuum at CIW
Raman Shift (cm-1)
500 1000 1500 2000 2500 3000
Ram
an In
tens
ity (a
rb. u
nits
)
CARS, 2 s488 nm Raman, 1 s
Nitrogen 22 GPa
Laser driven shock compression in the DAC:samples are dynamically compressed in the DAC
Armstrong and Crowhurst, LLNL
• Precompression in 100 GPa range is possible• Preheating and precooling if needed• Ultrafast experiments can be small scale: Table top system, unlike currently better known technique of laser shocks which involves large laser facilities (such as NIF)
Al
Diamond
Pump
Moving Alsurface
Precompressedsample
Shocked AlShock front
Shockedsample
SchematicUltrafast interferometry diagnostics
Observation of Off‐Hugoniot Shocked States with Ultrafast Time Resolution: Probing High‐pressure, Low‐temperature States
Laser shocks in the DAC can generate and detect 10s GPashock waves (and low pressure acoustic waves) in materials under precompression of 10s GPa
Laser shocks in the DAC can generate and detect 10s GPashock waves (and low pressure acoustic waves) in materials under precompression of 10s GPa
Bonev et al., (2010)
Phase diagram of hydrogen
Armstrong et al ., in press
Example of data for Ar
First shots on deuterium
•Shock and particle velocities of ~12‐13 km/s and ~1 km/s for precompression ranging up to 36 GPa, giving a shock pressure ~10 GPa.
•Possible phase transition over the duration of the probe window
Pha
se s
hift
per 5
ps
Delay (ps)
M. Armstrong. J. Crowhurst, LLNL
Pulsed laser techniques have a great abilities to: ‐ access unavailable previously extreme P‐T conditions‐ overcome problems of containing and probing chemically reactive and mobile materials‐study vibrational, optical, elastic, transport properties under extreme conditions
The full potential of these techniques will be reached with further development of ultrafast (ps to fs) pump‐probe & single –shot techniques coupled to pulsed laser heating and laser shocks in the DAC. ‐perform experiments in a time domain to access the time scale and dynamics of phase transitions & chemical reactions
We are looking forward for developing new combined X‐ray – optical techniques at synchrotron beamlines (e.g., ERL, Petra III, XFEL, NSLS‐II)
Outlook: the field is matureWe are looking for new opportunities which will be
given by new generation synchrotron sources