pressure calibration in dac -- challenges for increasing accuracy and precision
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Pressure Calibration in DAC -- Challenges for Increasing Accuracy and Precision. Ho-kwang Mao Carnegie Institution of Washington. Pressure Calibration Workshop January 26-28, 2007. Different Challenges in Different P-T Ranges. 2. 1- 100 GPa 10 MPa – 1 GPa - PowerPoint PPT PresentationTRANSCRIPT
Pressure Calibration in DAC --
Challenges for Increasing Accuracy and Precision
Ho-kwang Mao Carnegie Institution of Washington
Pressure Calibration Workshop January 26-28, 2007
• 1- 100 GPa
• 10 MPa – 1 GPa
• 100- 300 GPa
• High temperatures
Different Challenges in Different P-T Ranges
2
Topics
• Primary calibration (accuracy)
• Secondary calibration (precision)
• Hydrostaticity
• X-ray diffraction (axial and radial)
• Optical spectroscopy (Brillouin, Raman, fluorescence)
• Inelastic x-ray scattering spectroscopy
3
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
4
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
4
Primary calibration requires measurements of two independent functions related to pressure.
Examples:
• F and A – free rotation piston-cylinder
• US and UP – shock Hugoniot
• V and – DACV
2 = K/ K = dP/d P = V
2d.
5
Primary calibration requires measurements of two independent functions related to pressure.
Examples:
• F and A – free rotation piston-cylinder
• US and UP – shock Hugoniot
• V and – DACV
2 = K/ K = dP/d P = V
2d.
5
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
6
Pressure calibration, P/P ±1%
from x-ray diffractionVfrom Brillouin scatteringP- EOS by integration (Primary)
Ruby fluorescence shiftCalibrated by MgO P- EOS(Secondary)
Zha, Mao, Hemley, PNAS (2000)
6
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
10
Secondary Calibration of Six Metals
XRD, ±0.2%,P/P ±1%
Ruby fluorescence shiftCalibrated by MgO P- EOS(Secondary)
Dewaele, Loubeyre, Mezouar, PRB (2004)
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
12
High T Primary Calibration Using V and
Problem: KS = (1 + T) KT
Difference ~10% at 3000 K introduces >1% error
A practical alternative is to combine 300 K primary calibration and high resolution high P-T XRD
13
121
122
123
124
125
126
127
106 110 114 118 122 126 130 134
0
0.006
0.012
0.018
0.024
0.03
300 900 1500 2100
Pressure (GPa)
Vol
ume
(Å3 )
300 K
1400 K
2000 K
Fs20 ppv
Temperature (K)
(VT –
V30
0)/
V30
0
14
Post-perovskite P-V-TW. Mao et al, submitted (2007)
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
15
- BIOCHEMICAL REACTIONS IN HYDROTHERMA FLUIDS
- LIFE IN EXTREME ENVIRONMENTS (>1600 MPa)
[Sharma et al., Science 295, 1514 (2002)]- PRESSURE EFFECTS ON STRUCTURE-FUNCTION RELATIONS
Single-Crystal Diffraction of Cow Pea Mosaic Virus
[Lin et al., Acta Crystal. D61, 737 (2005)]
Biomaterials -- bacteria and virus16
350 MPa
Hydrogen storage in clathrate
Energy, keV
d-spacing, Å
Intensity
25 35 45 55 65
311
5 2.56 4 35.5 4.5 3.5
533
220
222
400
331 42
2
440
531
620
511
333
H2-2H2O S-II clathrate-- A clean and efficient material for hydrogen storage
0.2 GPa
10 kPa77 K 110 140 240
HH-sII
280
H2+H2O
17
W Mao et al, Science (2002)--Synthesis S-II at HP and quenched to low PT;
Lokshin et al, PRL (2004)--Identification of H2 in S-II cages with neutron;
Florusse et al, Science (2004)-- Stabilized to 280K at 1 bar
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
18
High Pressure Experiments Challenge Existing Understanding of Seismic Waves in Deep Earth
The crushing pressures in the lower mantle squeeze atoms and electrons so closely together that they interact differently from under normal conditions, even forcing spinning electrons to pair up in orbits. In theory, seismic-wave behavior at those depths may result from the vice-gripping pressure effect on the electron spin-state of iron in lower-mantle materials. Carnegie’s team performed ultra high-pressure experiments on the most abundant oxide material there, magnesiowüstite (Mg,Fe)O, and found that the changing electron spin states of iron in that mineral drastically affect the elastic properties of magnesiowüstite. The research may explain the complex seismic wave anomalies observed in the lowermost mantle.
Normalized volume of magnesiowüstite, (Mg0.83,Fe0.17)O, as a function of pressure at 300 K.
Jung-Fu Lin, Viktor V. Struzhkin, Steven D. Jacobsen, Michael Y. Hu, Paul Chow, Jennifer Kung, Haozhe Liu, Ho-kwang Mao and Russell J. Hemley; "Spin transition of iron in magnesiowüstite in the Earth's lower mantle" Nature 436, 377-380 (21 July 2005)
Spin transition of iron in magnesiowüstite19
Goals
Primary calibration (accuracy)• 1- 100 GPa P/P = ±1%
• 100- 300 GPa P/P = ±1%
• High temperatures -- at 100 GPa-2500 K P/P = ±1%
Secondary calibration (precision)• 10 MPa – 1 GPa P = ±5 MPa
• 1- 100 GPa P/P = ±0.2%
• 100- 300 GPa P/P = ±0.2%
20
Topics
• Primary calibration (accuracy)
• Secondary calibration (precision)
• Hydrostaticity
• X-ray diffraction (axial and radial)
• Optical spectroscopy (Brillouin, Raman, fluorescence)
• Inelastic x-ray scattering spectroscopy
21
0
1
2
3
0 20 40 60
Argon
t(G
Pa)
P(GPa)
Shear strength of argon
Mao, et al, J. Phys.: Cond. Mat. (2006)
Primary calibration needs to use He medium
Topics
• Primary calibration (accuracy)
• Secondary calibration (precision)
• Hydrostaticity
• X-ray diffraction (axial and radial)
• Optical spectroscopy (Brillouin, Raman, fluorescence)
• Inelastic x-ray scattering spectroscopy
23
Attaining V /V± 1%
• Ultrasonic measurements
• Nuclear resonant inelastic x-ray scattering
• Brillouin Spectroscopy
• Inelastic x-ray scattering spectroscopy
24
Attaining V /V± 1%
• Ultrasonic measurements to 50-300 GPa?
• Nuclear resonant inelastic x-ray scattering
• Brillouin Spectroscopy
• Inelastic x-ray scattering spectroscopy
25
Nuclear resonant inelastic x-ray spectroscopy (NRIXS)
APD
APD HRM M
KBmirrors
x-rays
DAC150nsec
NRIXS signal
SMS signal
nonmagnetic
magnetic
time
Energy
Inte
nsi
ty
Anti-stokes Stokes
Elastic line
XOR, Sector 3, APS, ANLXOR, Sector 3, APS, ANL
g(
) de
nsity
of s
tate
s
Debye Model
“Real” Crystal
2322
)(
Vg
333
213
SpD
222
3
4
)(
SP
KV
PVK
Attaining V /V± 1%
• Ultrasonic measurements
• Nuclear resonant inelastic x-ray scattering
• Brillouin Spectroscopy
• Inelastic x-ray scattering spectroscopy
27
Brillouin Spectroscopy
• Single crystalV accuracy ±1%
• PolycrystallineV accuracy 3-10%
28
Fiquet et al., Science 2001
Antonangeli et al., EPSL 2004
Antonangeli et al, PRL 2005
Single-xtal Co at 39 GPa
Inelastic x-ray scattering spectroscopy (IXSS)Poly-xtal hcp-Fe to over 100 GPa
Determines phonon dispersion
Inelastic x-ray scattering spectroscopy (IXSS)
7.6
7.8
8
8.2
8.4
0 10 20 30 40 50 60 70 80 90
angle between q and DAC compression axis
VP
(km
/sec
)
high resolution
medium resolution
Improve energy resolution from 6 meV to 1 meVto get to V /V± 1%
35XU, SPring-8
30
hcp-Fe at 52 GPa
W. Mao et al, in prep.
High Res. XRD with panoramic DAC
CCD
CCD
ctn Going from 2 = 10º to 2 = 90º, / improves 10x !
UNICAT, 34-ID, APS, ANL
Summary: Achievable Goals
Primary calibration (accuracy)• Hydrostaticity of He? P/P = 0.2-1%?
• Single-xtl Brillouin scattering or single-xtl ixss to 100- 300 GPa V/ V = ±1%
• Polycrystalline XRD to 100- 300 GPa and 100 GPa-2500 K / = ±0.2% P/P = ±1%
Secondary calibration (precision)• High resolution XRD at 10 MPa- 300 GPa
/ = ±0.02% P/P = ±0.2%
• Optical calibration P/P = ±0.2%
32