ELECTRON MICROSCOPY FOR MULTI-SCALE POROUS MATERIALS PART II - TEM PRINCIPLES
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1 ELECTRON MICROSCOPY FOR MULTI-SCALE POROUS MATERIALS PART II - TEM PRINCIPLES Marseille Winter School on Multi-Scale Porous Materials (Jan ) A. BARONNET
2 Principles of Transmission Electron Microscopy (TEM) The TEM machine - How it is made of and how it works - Attached techniques Imaging and diffraction Capabilities of the (Fast) Fourier Transform (FFT) in TEM Sample preparation techniques Some applications of high-resolution TEM on clay and clay-related materials -Structural characterization at atomic scale (T and O sheets, polytypes, mixed-layer silicates, non-planar serpentines) Other crystals with reduced dimensionnality: CSH, tunnel Mn oxides, Adding the chemical characterization to complete data ( Jérémie Berthonneau)
3 The electron microscope upside down a "light" microscope in which electrons replace photons vacuum torr Haute tension Kv
4 MET 200 kv (CRMCN)
5 Electron travels through the TEM
6 In a TEM, you may switch immediately from the direct space (image) to the reciprocal space (diffraction) crystal incident beam my god! the eternal dream of my life! objective lens back focal plane diffraction pattern image plane
7 1.25 MV HRTEM RUCA (Anvers) Bigger and bigger? Better and better? Image-corrected 300 kev HRTEM Aix-Marseille Université Desperate guy (red face)) trying to image antigorite
8 Electron sources and acceleration voltage Classical tungsten filament A LaB 6 tip cold and warm cathode field emission tip coherent beam acceleration voltage 300keV Best against beam damages not so coherent beam good for beam-sensitive minerals
9 Incident e Backscattered e (SEM/EBSD) Auger e X-rays(EDS) Cathodaluminescence Secondary e (SEM) Inelastically Scattered e (EELS) Elastically Scattered e (ED) Unscattered e (transmitted beam)
10 Sample volumes analyzed with Electron microprobe/ TEM EDS (ATEM) 5 µm Quantitative data for oxygen and above Z 16 X-ray energy 0-20keV V analyzed = 10 mm 3 V analyzed = 10-6 mm 3 ATEM is a satellite tool absolutely needed for mineralogical studies dealing with micro to nano size of crystals
11 An ideal sample to enter the TEM should be: : Transparent for standard acceleration ( kv) => 0 < thickness < 500 nm for oxides (silicates) HRTEM --> 5-10 nm Manipulable (support inscribed in diam. 3 mm) Conductive or rendered conductive by metallization => amorphous C-coating Representative of the bulk of the materials => structures, microstructures, defects, chemical compositions, be saved (preparation and observation)
12 The thin-sample preparation techniques which materials do you want to look at? organic, mineral, hard, soft, coherent, porous, granular, fibrous, composite,, hydroxylated, hydrated,... What do you want to see in this material? shape, size, crystallinity, chemical composition, defects, texture, ultrastructure,...
13 TEM grids and slots mesh grids conducting: Cu, Ni, Mo, Au,... "bivalve" grids 3 mm honeycomb grid "stadium" slot for ion thinning
14 The "drop deposition" technique 3 mm Advantages - the simplest and quickest -for powder characterization -(size, shape, diffraction, composition) Drawbacks -not for water soluble minerals -Particle density adjustment -drift and tilt under the beam (no clean HRTEM) - +-noise from C-film background(holey, lacey C-films- C-film wettability 1 mm Celadonite mica crystals (O. Grauby) synthetic chrysotile charge
15 Ultramicrotoming (continue) advantages unique for powders, fibers, synthesis charges chemically extremely clean ready for the TEM drawbacks not for big and hard materials sample bent and cracked: neither for microstructure nor defect observations Long training for embedding samples and to cut well O. Grauby - CINaM expensive diamond knives mechanical drift under the e-beam: no good HRTEM
16 Focused ion beam (FIB) milling advantages sample below a surface feature ready for TEM normal to the surface soft and hard, porous samples Slicing the nacreous layer of an oyster shell- O. Grauby drawbacks chemically dirty: Ga & Pt implantations smearing of chemical composition strong structural damages
17 3 mm Recent FIB specimen holder
18 The royal road From the rock to the atomic image by TEM diamond saw the rock slice thin-section facility of a geological laboratory uncovered rock slate double face 1µm polish µm-thick Thermofusible resin (Lakeside, crystalbond) glass plate thin section a special thin section sugar piece 300 µm diamond wire saw polishing machines
19 Crossed nicols light microscopy to place the slots thin section -recognize the minerals from their optical properties -crystallographic orientation with 15 accuracy microdrilling around the slot and melt the glue underneath (< 200 C) < 50 µm ready for the PIPS milling detach with a twizzer and wash the glue with alcohol
20 The top for high-resolution electron microscopy (HRTEM) of most minerals Ion - milling systems Precision ion polishing system (PIPS) Ar+ ions, 5 -->2 kev, two guns 7-4 incidence. Polishing time 0.5h to 5 days for 50µm - thick thin section Advantages -large and thin surfaces to look at -wedge-shaped sample: extra-thin zones - gentle heating -high mechanical stability -reasonable damages (amorphisation) Drawbacks -pollution by sputtering: grid, specimen holder -needs to be trained for optimum use
21 1 mm Around the hole: hours of exploration to come + continuous C-coating --> essential for electron conduction to the TEM mass Ready to enter the microscope
22 Preparation of TEM specimens: The sampling problem: to be representative for larger scale to be meaningful "All thinned samples of the Earth crust for TEM enter a thimble while the crust volume is roughly km 3.So, good luck for sampling! David, Veblen, JHU, Baltimore
23 The direct lattice (blue) and the reciprocal lattice (green) A 2-D case
24 Diffraction by crystals Bragg's law 2d (hkl) sin = nl and for high-energy electrons: 2d (hkl) nl 1/λ < >only lattice planes // to the incident beam are diffracting very thin specimen ---> elongation of reciprocal lattice nodes --->relaxation of Bragg's conditions > many reflections at a time
25 intersecting the 3D arrangement of the reciprocal lattice (RL) The SAED pattern = Visualisation of sub planar sections of the reciprocal lattice Tilting the sample in diffraction mode is exploring the RL in 3-D Double tilt, high-resolution, specimen holder ± 15 Procedure of alignment of a single crystal: find a crowdy SAED, put the zero-order Laue zone(zolz) perfectly symetrical around the transmitted beam by centring the first - order Laue zone (FOLZ) when visible! FOLZ ZOLZ
26 Microdiffraction patterns of some states of matter amorphous polycrystalline single crystal + disorder cylindrical lattice Quasi crystal seen along a 2-fold axis B. Devouard
27 The objective lens is the only one that matters In its focal plane, the diffraction pattern of the object In its image plane, the microscope performs a Fourier photosummation The Graal: the charge density projection of the crystal structure A biperiodic image = discrete sum (troncated) of sine variations of fringe contrast along diffraction vectors In the trigonometric form: (y,z)= k l F 0kl cos 2 (ky + lz + 0kl ) = F 000 Amplitude Wavelength Phase + F 010 cos 2 (y ) + F 020 cos 2 (2y+ 020 ) F 001 cos 2 (z+ 001 ) + F 002 cos 2 (2z+ 002 ) F 011 cos 2 (y+z+ 011 ) + F 022 cos 2 (2y+2z+ 022 ) +...
28 Point-to-point resolutions at CINaM: 2.8 Å for 200 kv TEM 1.6Å or 2.1Å for 300kV TEM 0.5Å somewhere in the world Electronic image = recombination of discrete diffracted beams; not a «shadow» image that keep amplitudes and phases of diffracted waves but: dynamical diffraction + phase offsets due mainly to spherical aberration The Scherzer defocus (critical underfocusing) roughly compensate for those phase offsets within the transfer window toward the structure image d r = 0, 65l 3 / 4 Cs 1/ 4
29 Correct phases are essentiel to get a correct structure image Objective Aperture Back focal plane Diffraction vectors Wave shift
30 Very HR numerical scan of the image «nuclear» film circular selection FFT processing (FIJI application) l 02l 04l 06l 5 nm Recorded Diff pattern Quasi-atomic image of the biotite mica seen along <1 0 0> FFT now realistic substitute to the microdiffraction
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