Making EBSD on water ice routine.
Electron backscatter diffraction (EBSD) on ice is a decade old. We have built upon previous work to select and develop methods of sample preparation and analysis that give >90% success rate in obtaining high-quality EBSD maps, for the whole surface area (potentially) of low porosity (<15%) water ice samples, including very fine-grained (<10 μm) and very large (up to 70 mm by 30 mm) samples. We present and explain two new methods of removing frost and providing a damage-free surface for EBSD: pressure cycle sublimation and 'ironing'. In general, the pressure cycle sublimation method is preferred as it is easier, faster and does not generate significant artefacts. We measure the thermal effects of sample preparation, transfer and storage procedures and model the likelihood of these modifying sample microstructures. We show results from laboratory ice samples, with a wide range of microstructures, to illustrate effectiveness and limitations of EBSD on ice and its potential applications. The methods we present can be implemented, with a modest investment, on any scanning electron microscope system with EBSD, a cryostage and a variable pressure capability.
Department of Geology, University of Otago, Dunedin, New Zealand.
D J
DJ
Prior
Department of Geology, University of Otago, Dunedin, New Zealand.
K
K
Lilly
Department of Geology, University of Otago, Dunedin, New Zealand.
M
M
Seidemann
Department of Geology, University of Otago, Dunedin, New Zealand.
M
M
Vaughan
Department of Geology, University of Otago, Dunedin, New Zealand.
L
L
Becroft
Otago Centre for Electron Microscopy, University of Otago, Dunedin, New Zealand.
R
R
Easingwood
Universiteit Utrecht, Department of Earth Sciences, Utrecht, Netherlands.
S
S
Diebold
Thayer School of Engineering, Dartmouth College, Hanover, New Hampshire, U.S.A.
R
R
Obbard
Thayer School of Engineering, Dartmouth College, Hanover, New Hampshire, U.S.A.
C
C
Daghlian
Thayer School of Engineering, Dartmouth College, Hanover, New Hampshire, U.S.A.
I
I
Baker
Department of Earth, Environmental and Planetary Studies, Brown University, Providence, Rhode Island, U.S.A.
T
T
Caswell
Earth Atmosphere and Planetary Sciences Department, MIT, Boston, Massachusetts, U.S.A.
N
N
Golding
Department of Earth and Environmental Science, University of Pennsylvania, Philadelphia, Pennsylvania, U.S.A.
D
D
Goldsby
Earth Atmosphere and Planetary Sciences Department, MIT, Boston, Massachusetts, U.S.A.
W B
WB
Durham
Department of Earth and Planetary Sciences, Macquarie University, NSW, Australia.
S
S
Piazolo
School of Earth, Atmosphere and Environment, Monash University, Melbourne, Victoria, Australia.
C J L
CJ
Wilson
Cryo-SEM; EBSD; Ice