Recent Advances in High-Pressure Techniques at the
LVP Facilities at GSECARS (APS)
Y. Wang, N. Nishiyama*, T. Sanehira, M. Rivers, S. Sutton
The University of Chicago
GeoSoilEnviroCARS Sector at the Advanced Photon Source
* Now at Geodynamics Research Center, Ehime University, Japan
(Supported by US National Science Foundation and US Dept. of Energy)
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Outline
•
Ultrasonics at high P and T
– Acoustic velocities and P-V-T equations of state
•
Crystallography at High P and T
– CAESAR diffraction for structural refinements
•
Melt Properties
– Viscosities
– Melting curve determination using X-ray transparent anvils
•
Rheology at high P and T
– Flow law determination
– Lattice preferred orientation and slip systems
•
New developments – towards megabar
– Modified cubic anvil apparatus
– DDIA-30
•
Conclusions
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Elasticity and equations of state
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
P-V-VP-VS-T-L Measurements to 25 GPa and 1600 K (B. Li et al., 2006)
(b) Cell assembly
1st stage anvils
transducer
2nd stage anvils
X-rays
(a) Set up
CaSiO3 Perovskite at 12 GPa
Anvil
Sample
0.004
5.8 GPa
P-Wave
P-wave
Buffer
Rod
0.002
Au markers
200
111
400
CaSiO3 Perovskite
14 GPa, 850C
(* from cell parts)
Amplitude
(c) X-ray diffraction
0.000
-0.002
1.44e-5
1.46e-5
1.48e-5
1.50e-5
NaCl (222)
1.54e-5
1.56e-5
1.58e-5
S-wave
Buffer Rod
*
0
NaCl (422)
211
*
310
*
S-Wave
0.001
(d) Acoustic
signals
0.000
-0.001
400
600
800
1000
Channels
Sample
0.002
Amplitude
*
15.0 GPa
Anvil
0.003
220
NaCl (220)
110
0.004
200
100
1.52e-5
Time, sec
NaCl (200)
Intensity
300
1200
1400
1600
2.14e-5
2.16e-5
2.18e-5
2.20e-5
2.22e-5
2.24e-5
2.26e-5
2.28e-5
2.30e-5
(e) X-ray image
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Unquenchable High-Pressure Clinoenstatite
Kung et al., 2005
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Kung et al., GRL, 2005
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
CAESAR diffraction and
Symmetry of CaSiO perovskite
high P-T crystallography
3
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Conventional Step-Scan with Upstream Single-Energy Discrimination
Detector
Beam
Beam
collimator Sample
collimator
in media
Energy
discriminator
2θ
Detector w/
E discrimination
(SSD)
Polychromatic
radiation
New Step-Scan with Downstream Multi-Energy Discrimination
Beam
collimation
2θ
Polychromatic
radiation
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Combined Angle- and Energy-dispersive Structural Analysis and Refinement
(CAESAR)
2θ
SSD
Collimator
Incident beam
Wang et al., JAC, 2004.
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
i
1st stage anvil
w
w
d
D
SD
High P-T CAESAR diffraction on CaSiO3 perovskite
1400
EDS
7 degr. EDS
1200
Int.
1000
800
600
400
200
ADS
0
0
1000
2000
3000
4000
Channels
1000
80 keV ADS
800
Int.
600
400
200
0
3
Work conducted at BL04B1, SPring-8
4
5
6
7
two theta, degr.
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
8
9
Reitveld refinements
at 13 Pa, 1320 K
Pm3m
13.0 GPa, 1320K, Cmcm
a = 7.1365(7) Ǻ, b = 7.0981(15) Ǻ, c = 7.1163(7) Ǻ,
V = 360.479(63) Ǻ3
Species
x
y
z
Uiso
Ca(1)
0
-0.010(4)
¼
0.012(5)
Ca(2)
0
0.498(6)
¼
0.021(6)
Si(3)
¼
¼
0
0.009(2)
O(4)
0.261(6)
0
0
0.000(6)
O(5)
0
0.237(15)
-0.003(6)
0.028(12)
O(6)
0.270(7)
0.259(12)
¼
0.025(9)
Texture index: 1.7987 (2nd order spherical harmonic)
Cmcm
Cmcm
Uchida et al., in prep.
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Best Fit: Cmcm
211c 220c
4000
210c
3500
200c
3000
111c
2500
110c
2000
100c
1500
1000
500
0
3
4
5
6
7
8
9
Uchida et al., in prep.
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Structural stability
•
CaSiO3 perovskite:
– Non-cubic distortion persists up to 24 GPa and 2050 K
•
CaSiO3 + 3wt% Al2O3 perovskite:
– Cubic up to 22 GPa and 2000 K
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Melt properties
• Viscosity
• Melting curves
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Viscosity of Melts Under High P-T
σ=ηε·
Terminal velocity:
vt = (2 Δρ r2 g) / (9 η)
Δρ = ρsphere - ρmelt
r = sphere radius.
Diopside: Reid et al., unpublished
Dacite: Tinker et al., Am Min, in press
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Melt viscosity
λ = 2.8 Å diameter of (O2-)
Pure Fe at 2050 K (Rutter et al., PRB’02)
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Use X-ray transparent anvils in mono diffraction
CCD
2θ
Mono X-rays
T-Cup, sintered diamond anvils as X-ray windows
2D monochromatic diffraction (ADD)
Record diffraction signal over entire 360° azimuth angle
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Si: XI – V – L triple junction
wBN
hBN
Phase XI
064
A
(14.3 GPa, 973 K)
C
B
Liquid
066
Phase V
070
(14.6 GPa, 1048 K)
031
220+211
(14.5 GPa, 998 K)
G
011
Intensity 066 (melt) - Intensity 064 (phase XI)
010
In te n sity (a .u .)
200
110
420
phase XI
hBN
wBN
231
Phase XI
064-066
020+110+011
D
Phase V
070-066
F
2
4
6
8
2theta (degrees)
10
Kubo et al., JPCS, in press
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Melting Curve of Si
L
Temperature (K)
1500
Phases
I
I + II
II
XI
V
L
This study
Voronin et al. (2003)
McMahon et al. (1994)
Jayaraman et al. (1963)
Bundy (1964)
Lees and Williamson (1965)
Brazhkin et al. (1995)
melting curve (Bundy 1964)
1000
V
II
I
500
XI
0
0
5
10
15
Pressure (GPa)
Kubo et al., JPCS, in press
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Rheology of earth materials
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
High P-T deformation on serpentinite
conditions investigated
dε/dt fixed ~ 10-6 to 10-4 s-1
14 deformation cycles
Hilairet et al, Science, in press.
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Serpentine: weakest link at slab-mantle interface
ε = Aσ nexp(-Q/RT)
PM: Peierls mechanism
di: wet diopside；an: anorthite
Hilairet et al, Science, in press.
ε: strain rate
A: constant
σ: ultimate strength
n: stress exponent
• Serpentine:
– impedes stress build-up
– limits downdip
propagation of large
earthquakes
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Comparison between mechanical data of hcp-Fe at ~18 GPa
and deformation map of hcp-Zn
hcp-Fe
Tm at 18 GPa
= 2100 K
(Shen et al., 1998)
μ at 18 GPa
= 174 GPa
(Vocadlo et al., 2003)
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Nishiyama et al., GRL, in press
Slip systems and lattice preferred orientation
in deformed CaIrO3 post-perovskite
[100](010)
Not [001](110)
as in MgGeO3
Miyagi et al., EPSL,in press
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
The megabar LVP
• Megabar pressure generation with second-stage SD
anvils (6/8) and 6/2 configuration on mm sized
samples
• Load capacity: 1000 ton (10 MN)
• Operated with and without synchrotron radiation
• Structural studies under these conditions
• Deformation on large samples at transition zone P-T
conditions
• Acoustic emission on large samples with controlled
deformation
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Modified Cubic-Anvil Apparatus
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
DDIA-30: a hybrid megabar module
2nd stage
anvil
1st stage
anvil
14
Cell
Sintered diamond
“filler”
500 mm
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006
Collimator
Conclusions
• Unique high pressure devices for wide range applications
–
–
–
–
–
T-25: 30 GPa, 2800 K
T-10: 23 GPa, 2000 K, SD anvils
DIA: 12 GPa, 2000 K,
D-DIA: 20 GPa, 1500 K, strain rates down to 10-7 s-1
High-P topmography
• Continuing to develop new devices to take advantage of bright
radiation sources
•
•
– Modified cubic anvil apparatus for double-stage, ultrahigh pressure
generation
– D-DIA 30 for double-stage, ultrahigh pressure generation, deformation
of large samples, acoustic emission
– PE cell for structural studies of liquids
Beamtime contact: wang@cars.uchicago.edu
Post-doc opportunities
GeoSoilEnviroCARS ● The University of Chicago ● Paris, April 27, 2006