Do it with electrons !

II

TEM - transmission electron microscopy

Typical accel. volt. = 100-400 kV (some instruments - 1-3 MV) Spread broad probe across specimen - form image from transmitted electrons Diffraction data can be obtained from image area Many image types possible (BF, DF, HR, ...) - use aperture to select signal sources Main limitation on resolution aberrations in main imaging lens Basis for magnification - strength of post- specimen lenses

TEM - transmission electron microscopy

Instrument components Electron gun (described previously) Condenser system (lenses & apertures for controlling illumination on specimen) Specimen chamber assembly Objective lens system (imageforming lens - limits resolution; aperture - controls imaging conditions) Projector lens system (magnifies image or diffraction pattern onto final screen)

TEM - transmission electron microscopy

Instrument components Electron gun (described previously) Condenser system (lenses & apertures for controlling illumination on specimen) Specimen chamber assembly Objective lens system (imageforming lens - limits resolution; aperture - controls imaging conditions) Projector lens system (magnifies image or diffraction pattern onto final screen)

TEM - transmission electron microscopy

Examples

Matrix - '-Ni2AlTi Precipitates - twinned L12 type '-Ni3Al

TEM - transmission electron microscopy

Examples

Precipitation in an Al-Cu alloy

TEM - transmission electron microscopy

Examples

dislocations in superalloy

SiO2 precipitate particle in Si

TEM - transmission electron microscopy

Examples

lamellar Cr2N precipitates in stainless steel

electron diffraction pattern

TEM - transmission electron microscopy

Specimen preparation Types replicas films slices powders, fragments foils

as is, if thin enough ultramicrotomy crush and/or disperse on carbon film

Foils 3 mm diam. disk very thin (<0.1 - 1 micron - depends on material, voltage)

TEM - transmission electron microscopy

Specimen preparation Foils 3 mm diam. disk very thin (<0.1 - 1 micron - depends on material, voltage) mechanical thinning (grind) chemical thinning (etch) ion milling (sputter)

examine region around perforation

TEM - transmission electron microscopy

Diffraction Use Bragg's law - = 2d sin But much smaller (0.0251 at 200kV) if d = 2.5, = 0.288

TEM - transmission electron microscopy

Diffraction 2 sin 2 = R/L = 2d sin d (2 ) R/L = /d

specimen

Rd = L L is "camera length" L is "camera constant" image plane

TEM - transmission electron microscopy

Diffraction

Get pattern of spots around transmitted beam from one grain (crystal)

TEM - transmission electron microscopy

Diffraction Symmetry of diffraction pattern reflects symmetry of crystal around beam direction Example: 6-fold in hexagonal, 3-fold in cubic

[111] in cubic

[001] in hexagonal

Why does 3-fold diffraction pattern look hexagonal?

TEM - transmission electron microscopy

Diffraction Note: all diffraction patterns are centrosymmetric, even if crystal structure is not centrosymmetric (Friedel's law) Some 0-level patterns thus exhibit higher rotational symmetry than structure has
P cubic reciprocal lattice layers along [111] direction

l = +1 level

0-level

l = -1 level

TEM - transmission electron microscopy

Diffraction

Cr23 C6 - F cubic a = 10.659

Ni2AlTi - P cubic a = 2.92

TEM - transmission electron microscopy

Diffraction - Ewald construction Remember crystallite size? when size is small, x-ray reflection is broad To show this using Ewald construction, reciprocal lattice points must have a size

TEM - transmission electron microscopy

Diffraction - Ewald construction Many TEM specimens are thin in one direction - thus, reciprocal lattice points elongated in one direction to rods - "relrods" Also, very small, 1/ very large

Only zero level in position to reflect

Ewald sphere

TEM - transmission electron microscopy

Indexing electron diffraction patterns Measure R-values for at least 3 reflections

TEM - transmission electron microscopy

Indexing electron diffraction patterns

TEM - transmission electron microscopy

Indexing electron diffraction patterns

Index other reflections by vector sums, differences Next find zone axis from cross product of any two (hkl)s (202) x (220) > [444] > [111]

TEM - transmission electron microscopy

Indexing electron diffraction patterns

Find crystal system, lattice parameters, index pattern, find zone axis ACTF!!! Note symmetry - if cubic, what direction has this symmetry (mm2)? Reciprocal lattice unit cell for cubic lattice is a cube

TEM - transmission electron microscopy

Why index? Detect epitaxy Orientation relationships at grain boundaries Orientation relationships between matrix & precipitates Determine directions of rapid growth Other reasons

TEM - transmission electron microscopy

Polycrystalline regions

polycrystalline BaTiO3 spotty Debye rings

TEM - transmission electron microscopy

Indexing electron diffraction patterns - polycrystalline regions Same as X-rays smallest ring - lowest - largest d

Hafnium ( )

TEM - transmission electron microscopy

Indexing electron diffraction patterns - comments Helps to have some idea what phases present d-values not as precise as those from X-ray data Systematic absences for lattice centering and other translational symmetry same as for X-rays Intensity information difficult to interpret

TEM - transmission electron microscopy

Sources of contrast

Diffraction contrast - some grains diffract more strongly than others; defects may affect diffraction Mass-thickness contrast - absorption/ scattering. Thicker areas or mat'ls w/ higher Z are dark

TEM - transmission electron microscopy

Bright field imaging Only main beam is used. Aperture in back focal plane blocks diffracted beams Image contrast mainly due to subtraction of intensity from the main beam by diffraction

TEM - transmission electron microscopy

Bright field imaging Only main beam is used. Aperture in back focal plane blocks diffracted beams Image contrast mainly due to subtraction of intensity from the main beam by diffraction

TEM - transmission electron microscopy

Bright field imaging Only main beam is used. Aperture in back focal plane blocks diffracted beams Image contrast mainly due to subtraction of intensity from the main beam by diffraction

TEM - transmission electron microscopy

Bright field imaging Only main beam is used. Aperture in back focal plane blocks diffracted beams Image contrast mainly due to subtraction of intensity from the main beam by diffraction

TEM - transmission electron microscopy

What else is in the image? Many artifacts surface films local contamination differential thinning others

Also get changes in image because of annealing due to heating by beam

TEM - transmission electron microscopy

Dark field imaging Instead of main beam, use a diffracted beam Move aperture to diffracted beam or tilt incident beam

TEM - transmission electron microscopy

Dark field imaging Instead of main beam, use a diffracted beam Move aperture to diffracted beam or tilt incident beam

strain field contrast

TEM - transmission electron microscopy

Dark field imaging Instead of main beam, use a diffracted beam Move aperture to diffracted beam or tilt incident beam

TEM - transmission electron microscopy

Lattice imaging Use many diffracted beams Slightly off-focus Need very thin specimen region Need precise specimen alignment

See channels through foil Channels may be light or dark in image Usually do image simulation to determine features of structure

TEM - transmission electron microscopy

Examples

M23 X6 (figure at top left). L21 type '-Ni2AlTi (figure at top center). L12 type twinned 'Ni3Al (figure at bottom center). L10 type twinned NiAl martensite (figure at bottom right).