Microstructure evolution

during creep and

annealing of minerals
and rocks

D. Tatham,
D.J. Prior, E. Mariani, S.J. Covey-
Crump, J. Mecklenburgh, J. Wheeler

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High temperature deformation in the Earth

Ed Garnero

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 How do we gain insight into mechanisms of
deformation in the Earth’s crust and their implications?
SE Torre Saliere NW

1 Km
Fold structure in the Morcle Nappe,
Nappe, Salanfe,
Salanfe, Swiss
Alps
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 Tools for understanding high temperature
deformation of rocks

Electron
backscatter
diffraction
(EBSD)

Naturally deformed systems

“Final microstrucutres”

Experimental
rock
deformation Modelling
“Post mortem
analysis”
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 We track microstructural evolution
through in-situ heating and deformation
experiments in the SEM with
simultaneous EBSD
These may tell us about:
• dynamics and kinematics of grain boundary mobility
• the behaviour of special (twin, CSL) boundaries
• the control of orientation/chemistry on boundary migration
• what mechanisms control static and dynamic recrystallization

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 The SEM in Liverpool

• The CamScan X500

CrystalProbe is specifically
designed for high-
temperature in situ
experiments.
• Tilted column permits
experimentation on horizontal
samples.

• Sample assembly and

detectors separated by
water-cooled heat shield,
reducing contamination of
signal at high experimental
temperatures.

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Static Heating Stage

• Coiled Ta wire resistance

heater.
• Capable of furnace
temperatures in excess of
1200oC.
• Equates to sample surface
temperatures in excess of
1000oC.
• Samples up to 9x9x3mm sit in
a cavity in graphite furnace
core.
• Furnace heating path controlled
by a Oxford Instruments
Intelligent Temperature
Controller.

Seward et al., 2000 Scanning, 24, 232-240.

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Annealing of deformed NaCl

Slide8.avi

Bestmann et al., 2005. J. Struct. Geol. 47, 447-457

8 Piazolo et al. 2006, Tectonophysics 427, 55-71
Annealing of deformed NaCl

Before heating

500 µm
Bestmann et al., 2005. J. Struct. Geol. 47, 447-457
Piazolo et al. 2006, Tectonophysics 427, 55-71
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Annealing of deformed NaCl

after 2.5h heating at 350-410°°C

500 µm
Bestmann et al., 2005. J. Struct. Geol. 47, 447-457
Piazolo et al. 2006, Tectonophysics 427, 55-71
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Annealing of deformed NaCl

after 4.5h heating at 350-410°°C

500 µm
Bestmann et al., 2005. J. Struct. Geol. 47, 447-457
Piazolo et al. 2006, Tectonophysics 427, 55-71
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 GBM at low T GBM at high T

Increasing continuity (time and space) of movement

Decreasing tendency to create ‘poikiloblasts’
Decreasing influence of pre-existing substructure
Increasing face control
Increasing length of straight segment movement

12 Piazolo et al., 2006, Tectonophysics 427, 55-71

Grain growth in annealed copper at 850oC

Slide13.avi

Video is 30x real-time

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Grain growth in annealed copper at 850oC

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 In--situ deformation & heating stage
In

• Stepper motor-driven tensile

Stepper LVDTs
heating/deformation rig in-situ
motor
in SEM. Load
Sample
• Opposing lead screws allow cell
tensile load & strain while
keeping the area of investigation
under the electron beam.
• Paired resistance heaters
capable of furnace
temperatures in excess of
1400oC & sample surface Heaters
temperatures well in excess of Ceramic sample jig
1000oC.
• Samples thermally isolated from Water-cooled plate
deformation assembly by
ceramic jig.
• Controlled via LabVIEW.

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Deformation in copper at ~700oC

Slide16.avi

Video is 300x real-time, 0.8mm total extension

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17
 P,T

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 Pressure
• inhibits brittle failure

• promotes GBM

In the SEM we need higher temperature but...

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Practicalities of working on geologically important materials

Slide20.avi

Mariani and Tatham, unpublished experiments;

20 Bestmann. unpublished experiments
Tracking microstructure evolution

LVDT

fixed piston

displacement rods

moving piston
New SEM stage
passive load (to Prior, January 09)
High T creep rig
(to Mariani, July 09)
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Tracking microstructure evolution

microstructural evolution

stress

rheology
shear strain
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Tracking microstructure evolution

U ndefo rm ed
0 500 10 00 0 500 10 00
sca le / m sca le / m

shear strain = 0.5

T= 973K
P= 300M Pa

With Julian Mecklenburgh,

Manchester
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Oxford Instruments F+ Camera & Fast Acquisition Software

200 µm 100µm

EBSD of calcite (0.7 um step). Raw EBSD data of garnet (1.5 um

step).
20kV, 35nA . 450 pt/s !!!
20kV, 50nA . 280 pt/s.

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Higher Resolution

Carrara marble

Solenhofen limestone

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 Summary

• The Earth is a dynamic system that accommodates its internal stresses by

the deformation of rocks on all scales, from continental, through kilometre, to
grain and sub-grain scales.
• In
nature and existing rock deformation experiments, we often only see the
end result of deformation: so called ‘frozen-in’ microstructures for post-
mortem analysis.
• In
situ experiments in the SEM allow us to actually observe and conduct
quantitative analyses during rock deformation experiments on natural,
synthetic and analogue materials.
• Continual advances in EBSD and SEM technology allows us to collect more
data, faster, and with higher resolution. This permits us to better understand
natural systems and further refine our models of how the Earth
accommodates stress.

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 Thank you
Movies available at:
pcwww.liverpool.ac.uk/~tatham/mtmovies.zip

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