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Advanced applications of FIB-TEM in Geosciences

Richard WirthHelmholtz Centre Potsdam

GFZ German Research Centre for Geosciences

FIB/TEM ApplicationsFIB systems operated at GFZ Potsdam

FEI FIB 200 TEM

FEI Quanta 3Dimage courtesy Anja Schreiber, GFZ, Potsdam

FIB/TEM Applications

• Applications in Geosciences– Nano-Inclusions in minerals (diamond)– Microstructure, Porosity– 3D imaging

• Applications in Geobiology– Monorhaphis Chuni– Precambrian acritarchs

• DAC experiments– Machining diamonds – Recovering samples from DAC experiments and TEM investigation

• Sample preparation– Synchrotron IR– Synchrotron XRF STXM (Scanning transmission X-ray microscopy) – NanoSIMS– FEG-microprobe

Application of FIB/TEM

Nano-diamonds in melt inclusions in OPX and CPX in Hawaiian Lava

SE image TEM foil, TEM bright field image

Opx

Wirth, R.; Rocholl, A. (2003): Nanocrystalline diamond from the Earth's mantle underneath Hawaii. Earth and Planetary Science Letters, 211, 3-4, 357-369

Application of FIB/TEM

Nano-diamonds in melt inclusions in OPX and CPX in Hawaiian Lava

Aggregates of nanocrystalline diamond (d)Dark field image of an aggregateof nanocrystalline diamond

Dark field STEM image

Wirth, R.; Rocholl, A. (2003): Nanocrystalline diamond from the Earth's mantle underneath Hawaii.

Earth and Planetary Science Letters, 211, 3-4, 357-369

Diamond

Olivine

Application of FIB/TEMNano-inclusions in diamond

HAADF image

Diamond

Olivine

Nano-inclusions in diamond

A.M., Logvinova, R., Wirth, E.N., Federova, N.V., Sobolev., 2008, EUR. J. Mineral., 20, 317-331

Nano-inclusions in diamond are composed of:

•Carbonates (Ca, Mg, Fe, Ba, Sr) •Silicates (phlogopite, high silica mica)•Halides (NaCl, KCl)•Phosphate (F-Apatite)•Ti-phase (Ilmenite, rutile)•Sulphide (Fe-Cu-Ni)•Quench phase (Si, Ba, Sr, F)•Fluid

Inclusions represent High density fluid (HDF) enriched in Cl, K, P, Ba, Si, Sr + water + carbonate,the medium diamond has grown from.Klein BenDavid, Wirth, Navon, 2006, Amer. Min., 91, 353-365

New insights in diamond genesis

FIB/TEM ApplicationsMicrostructure of opal

Apatite

Thorium Silicate

Apatit

Thorium Silicateat

Apatite

Tuning the colour of opal by the arrangement of the basic SiO2 objects

Green opal

4

6

3

Pt

Natural “metamaterial”. Metamaterials are designed and used for special optic devices.In metamaterials the properties largely depend on the structure rather than on the material itself.

FIB/TEM ApplicationsPorosity

Apatite

Thorium Silicate

Apatit

Apatite

4

6

3

15 µm

Pt

500 nm

Original porosity is not changed by FIB sputtering!!

Ultracataclastic core samples recovered from 3194 m and 3294 m depth of the main bore hole of the

San Andreas Fault Observatory at Depth.

Janssen, C.; Wirth, R.; Rybacki, E.; Naumann, R.; Kemnitz, H.; Wenk, H.-R.; Dresen, G. (2010): Amorphous material in SAFOD core samples (San Andreas Fault): Evidence for crush-origin pseudotachylytes?. Geophysical Research Letters, 37, L01303

pores

FIB/SEM Dual Beam Cross-Sectioning

Symplectite Microstructure 3D imagingRainer Abart, University Vienna, Austria

3D reconstruction from successive slices, 100 slices at 100 nm intervals, each slize is imaged using BSE signal on an FEI Quanta 3D FEG-SEM-FIB

montmerw fo

Ca3MgSi2O8 Mg2SiO4at 900°C, 1.2 GPa

FIB/TEM ApplicationsGeobiology

Deep sea sponge monorhaphis chuni

Cross section through the fibre Sponge at the sea floor

M. Roux Univ. Reims



In situ etching of a cross section of the fibre with FIB using XeF2

Not etched etched



SE image of fibre cross section

TEM bright field image of FIB cut foil

C - element map (EELS) of

organic material“Natural fibre composite”

Amorphous silica

(Blue algae)


Kempe, A.; Wirth, R.; Altermann, W.; Stark, R. W.; Schopf, J. W.; Heckl, W. M. (2005): Focussed ion beam preparation and in situ nanoscopic study of Precambrian acritarchs. Precambrian Research, 140, 1-2, 36-54.

Fossil Acritarch cell walls from 650 my old Chichkan Formation, Kazakhstan

Ancient cell wall

Precambrian Acritarch cell walls

TEM bright field image of cell walls

C -elemental map (EELS) of cell walls


Kempe, A.; Wirth, R.; Altermann, W.; Stark, R. W.; Schopf, J. W.; Heckl, W. M. (2005): Focussed ion beam preparation and in situ nanoscopic study of Precambrian acritarchs. Precambrian Research, 140, 1-2, 36-54.

FIB/TEM ApplicationsMicromachining of diamond for DAC application

diamond

Wirth, R. (2004): A novel technology for advanced application of micro- and nanoanalysis in geosciences and applied mineralogy. European Journal of Mineralogy, 16, 6, 863-876

FIB/TEM ApplicationsMicromachining of diamond for DAC application

Synchrotron radiation

diamond

X-ray fluorescence

FIB milled section

FIB/TEM ApplicationsSample recovery from DAC experiments

sample

Rhenium gasket

0.2 mmsample

gasket


sample

Rhenium gasket

0.2 mmsample

gasketsample


sample

Rhenium gasket

0.2 mm

FIB/TEM ApplicationsTEM investigation of the foil

sample

Rhenium gasket

0.2 mm

Amorphous carbonate

diamond

Pt

Experiment: Sergio Speziale, GFZ Potsdam

Reacting Fe - MgO - CaCO3 at Lower Mantle conditions

FIB/TEM ApplicationsSample preparation : synchrotron IR spectroscopy

Zinco-Staurolite from Samos

Synchrotron IR-Measurement

FIB cut foil

30 x 20 x 5 micron

FIB/TEM ApplicationsSample preparation: Nano SIMS

diamond

carbonate

TEM foil on grid, optical micrograph

TEM foil TEM bright field image

FIB/TEM ApplicationsSample preparation: Nano SIMS

diamond

Y. Sano, D. Pinti, Center for Advanced Marine Res., Ocean Research Institute, Tokyo, Japan

FIB/TEM ApplicationsTEM and Nano SIMS

diamond

L. F. Dobrzhinetskayaa,, Ri. Wirth, J.Yang, I. D. Hutcheon, P. K. Weber, and H.W. Green II (2009)High-pressure highly reduced nitrides and oxides from chromitite of a Tibetan ophiolite. Proceedings of the National Academy of Sciences of the United States of America (PNAS), 106, 46, 19233-19238.

Coesite bearing chromitite from Luobasa, Tibet

TiN

High-pressure highly reduced nitrides and oxides from chromitite of a Tibetan ophiolite

TEM HAADF image

FIB/TEM ApplicationsSample preparation: STXM, EXAFS

diamond

Scanning transmission X-Ray microscopy STXM of the foil imaged at 500 eV

Daniel Fliegel, Richard Wirth, Antonio Simonetti, Anja Schreiber3, Harald Furnes and Karlis Muehlenbachs (2010)

Tubular textures in pillow lavas from a Caledonian West-Norwegian Ophiolite a: combined TEM, LA-ICP-MS and STXM study . G3 in press.

STXM image at the C-K edge

XANES spectra at the C-K edge

Bernard, S.; Horsfield, B.; Schulz, H.-M.; Schreiber, A.; Wirth, R.; Vu, T. T.; Perssen, F.; Kitzer, S.; Volk, H.; Sherwood, N.; Fuentes, D. (2010): Multi-scale detection of organic and inorganic signatures provides insights into gas shale properties and evolution.. Chemie der Erde - Geochemistry,70, Suppl. 3, 119-133.

FIB/TEM ApplicationsSample preparation: STXM, XANES

XANES images

FIB/TEM ApplicationsTEM element mapping after using the foil for STXM and XANES

Bernard, S.; Horsfield, B.; Schulz, H.-M.; Schreiber, A.; Wirth, R.; Vu, T. T.; Perssen, F.; Kitzer, S.; Volk, H.; Sherwood, N.; Fuentes, D. (2010): Multi-scale detection of organic and inorganic signatures provides insights into gas shale properties and evolution.. Chemie der Erde - Geochemistry,70, Suppl. 3, 119-133.

FIB/TEM Applicationssample preparation: Brillouin Spectroscopy

Flat and parallel surfaces required

S. Speziale1, H. Marquardt1, R. Wirth1, A. Schreiber1, K. Marquardt1, G. Neusser2, H.J. Reichmann1

(2010), AGU Fall Meeting, San Francisco

FIB/TEM Applicationssample preparation: FEG microprobe analysis

Interaction sample - electron beam (thin sample)

Incident electron beam

X-ray photonsX-ray photons

Excited volume

Sample surface

TEM foil (150 nm thick)

FEG microprobe analysis with thin TEM foils at reduced acceleration voltage (< 10 keV) improves the spatial resolution of the analysis << 100 nm!

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