Beruflich Dokumente
Kultur Dokumente
26
4 4 Interactions Interactions Electrons Electrons Matter Matter - -
Electron Electron Contrast Contrast SEM SEM
5 5 Electron Diffraction Electron Diffraction - -
Electron Contrast Electron Contrast TEM TEM
6 SEM 6 SEM Channeling Contrast Channeling Contrast and and
Electron Diffraction Techniques Electron Diffraction Techniques
Interactions Interactions Electrons Electrons Matter Matter
K
L
M
electron beam
stroke out
of secondary electron
nucleus
elastically deflected
electron
=> BSE
=> SE
K
L
M
27
Electron Electron Penetration Penetration Depth Depth
ca. 1-10nm
SE1
SE2
BSE
X rays
penetration depth
(dependent on E ) R
0
ca. 0,5R
electron beam
Auger-e
-
specimen current
specimen
AE
SE BSE
N(E)
50 eV
(convention)
E
0
2 keV
E
Electron Electron Penetration Penetration Depth Depth
foil on Cu grid
HV:
1kV 3.5kV 20kV
polymer
copper
diameter of the interaction volume: approx. 2m
polymer
copper
polymer
copper
28
Secondary Secondary Electrons Electrons (SE) (SE) Detector Detector
Secondary Secondary Electrons Electrons (SE) (SE) Detector Detector
Everhart Thornley Detector
specimen
light guide photo multiplier
(successive acceleration
+multiplication at dynodes)
collector
+300V
scintillator photo cathode
behind quartz window
electrical
signal
29
Contrast Contrast Formation: Formation:
Topography Topography & & Edges Edges
primary electron beam (PE)
SE
PE
I
x
Human Human Hair Hair
30
Secondary Secondary Electrons Electrons Gain Gain
: leaving electrons/
incident electrons
: SE gain
: BSE coefficient
negative charging
conductive specimens!
E
0
Back Back- -Scattered Scattered Electrons Electrons (BSE) (BSE) Detector Detector
BSE
SE
electron beam
+
amplifier
Al coating
gold
nsilicon
-
p silicon
+
SE-Detektor
BSE-semiconductor
detector
elastic scattering
inelastic collision BSE at
detector
generation of
electron/hole pairs
p/n transition inhibits
recombination
31
BSE BSE Detector Detector
SE Detector
Material Material Contrast Contrast
light elements (lowZ) dark
heavy elements(high Z) - bright
Al-Si alloy (with Si precipitates)
SE image
BSE image (same position)
32
Contrast Contrast information information: :
Material Material
and and
Topography Topography
BSE detector B A
5 5 Electron Diffraction Electron Diffraction - -
Electron Contrast Electron Contrast TEM TEM
33
Electron Electron Diffraction Diffraction - - Bragg Bragg s s law law
x x
d
primary electron
beam diffracted intensity
lattice planes
2x =2d sin =N
transmitted intensity
E
0
=100kV: =0.0037nm, Cu (111) planes =>=0,5
Debye Debye- -Scherrer Scherrer Diagrams of Diagrams of Polycrystals Polycrystals
500nm
selected area diffraction TEM micrograph (TlCl standard)
electron beam
specimen
diffractionrings
(DS diagrams)
34
Electron Electron Diffraction Diffraction
in in the the TEM TEM
vacuum system
filament (cathode)
Wehnelt cap
anode
condenser lens
condenser aperture
specimen
objective lens
obejctive aperture
selector aperture
intermediate lens
projective lens
fluorescent phophorous screen
camera
diffracted intensities
200 kV
diffraction spots
Bragg diffraction
at lattice planes
2
x
y
z
The The Reciprocal Reciprocal
Lattice Lattice
reciprocal lattice
camera length L
real lattice
2d sin =N (Bragg)
2d N
R
2
2 =tan R/L (geometry)
R/2L
: very small!
beam|| zone axis
d R = L
diffraction constant
R =const./d
g
35
The The Reciprocal Reciprocal Lattice Lattice
R: phosphorous screen
g: reciprocal lattice
000
420
R
2
R
1
Evaluation of Evaluation of Diffraction Diffraction Pattern Pattern
R
2
/R
1
36
Diffraction Diffraction
Pattern Pattern
for for different different
Zone Zone Axis Axis
[101] [111]
[211] [100]
[110] [111]
fcc
bcc
Kinematical Kinematical Theory Theory
x
y
r k
0
k
change of wave direction at the atoms =>amplitude/phase differences
primary beam ()
secondary waves()
( )
=
n
n n
i f A exp
resultant amplitude:
37
The The Ewald Ewald Sphere Sphere
primary beam
lattice planes
s
k
o
>>g
plane of the
diffraction pattern
k
k
0
g
2
The The Ewald Ewald Sphere Sphere
two-beam case
(Bragg case)
symmetrical case
(Laue case)
38
Amplitude Phase Diagrams Amplitude Phase Diagrams
Origin Origin of of Wedge Wedge Fringes Fringes 1 1
diffracted intensity 0 max 0 max .....
transmitted intensity I
0
min I
0
min ......
image bright dark bright dark ......
39
Origin Origin of of Wedge Wedge Fringes Fringes 2 2
diffracted transmitted
edge
boundary
Stacking Stacking Faults Faults
stackingfaultsin Al-20Si
from: Hornbogen/Skrotzki: Werkstoffmikroskopie, Springer 1993
40
Bend Bend Contours Contours
Al +Ge particles
from: Hornbogen/Skrotzki: Werkstoffmikroskopie, Springer 1993
+
-
Dislocations Dislocations
b
g
image
primary beam
Burgers vector
diffracted beam
planar dislocation arrangement
(Ti alloy LCB, /2=600MPa)
500nm
41
Dislocations Dislocations: : Pile Pile- -Up Up at at Grain Grain Boundary Boundary
grain
boundary
Dislocations Dislocations
High High- -Resolution Resolution
TEM TEM
Si single crystal
(image taken at magnific. 30000000)
42
Convergent Convergent
Electron Electron
Diffraction Diffraction
Kikuchi Kikuchi
Pattern Pattern
convergent electron beam
specimen
Kossel cone
bright line (dark line)
Fe alloy
[110]
[111]
[211]
6 6 SEM SEM Channeling Contrast Channeling Contrast and and
Electron Diffraction Techniques Electron Diffraction Techniques
43
Influence Influence of of the the Tilt Tilt Angle on Angle on the the
BSE BSE contrast contrast
Channeling Channeling Contrast Contrast
electron beam electron beam
crystalline lattice
44
Imaging Imaging of of Dislocation Dislocation Structures Structures
PSB in deformed single-crystalline Cu
(R. Richter, TU Dresden)
Electron Electron Channeling Channeling Pattern Pattern
Si single crystal Si single crystal
rocking beam
incident e
-
beam
scanning
latticeplanes
latticeplanes
45
Bragg Bragg s s law law
x x
d
primary electron
beam diffracted intensity
lattice planes
2x =2d sin =N
The The EBSD EBSD Technique Technique
( (electron electron back back- -scattered scattered diffraction diffraction) )
striping (streifender)
incident electron beam
46
Bragg Bragg Diffraction Diffraction of of Electrons Electrons
x x
phosphorous screen:
intersection with cone =>parallel lines
Kossel cones
characteristic
X-rays
Bremsstrahlung
E
0
EDS EDS spectrum spectrum
( (energy energy dispersive dispersive X X- -ray ray spectroscopy spectroscopy) )
I
E
example: brass (Messing)
[keV]
EDS EDS detector detector
Cu-rod in vacuum
N (l)
2
specimen
take-off angle
PE
UTW(ultradnnes Polymerfenster)
Si(Li)
53
EDS EDS detector detector
X-Ray quantum
Au contact
Si(Li) crystal
Al layer
FET-
preamplifier
(field effect trasnitsor)
voltage step: mV/ns
500-700 V
generation of
electron/hole pairs
Si inactive layer
(Totschicht)
LED
main amplifier/ADC
multi chanel analyzer
X-ray energy
t
Pulse Pulse Pile Pile Up Up
X-ray energy
t
peak too high due to
pulse pile up
within DT ->reject
100s =DT (dead time)
54
Pulse Pulse Pile Pile Up Up
input (cps)
output
no signal anymore:
pulse pile up
Sum SumPeaks Peaks
2 Al K X-rays simultaneous
55
Escape Escape Peak Peak
Cu K quantum generates Si K quantum
Regions Regions of of Interest Interest Line Line Scan Scan
energy
example: brass (Messing)
intensity
energy
Background (noise/Bremssstrahlung))
improvement by narrow energy window
intensity
56
Regions Regions of of Interest Interest Line Line Scan Scan
NiCrMo-Schicht
Stahl
NiCrMo scale
steel
Element Element Mapping Mapping
Al Ti
100m
57
Monte Carlo Simulation Monte Carlo Simulation
characteristicTa X-rays
WDS WDS crystal crystal spectrometer spectrometer
( (wavelength wavelength dispersive dispersive X X- -ray ray spectroscopy spectroscopy) )
x x
d
r
r =2r
Krist.
crystal (J ohannson)
on Rowland circle
proportional counter
Gas Gas Flow FlowProportional Proportional Counter Counter
Ar outlet Ar inlet
high voltage
(+1 to +3kV)
signal
(to pre amplifier)
isolator
FPC window
X-rays are absorbed by Ar atoms =>ejectionof photo electrons
(up to 50000 counts/s amplificationup to 2000)
thin wire (W)
x-ray photon
59
Comparison Comparison EDS/WDS EDS/WDS
EDS
WDS
characteristic X-rays
emission line
natural width
Quantitative X Quantitative X- -Ray Analysis Ray Analysis
=> => background background subtraction subtraction
continuous Bremsstrahlung absorption (<2keV)
background modelingor background filtering
2 4
6
8
energy [keV]
60
Quantitative X Quantitative X- -Ray Analysis Ray Analysis
=> => Geometry Geometry of of the the Detector Detector
working distance W (10mm), intersection distance d (10mm),
elevation angle E (35), azimuth angle A (45), Scale S (50mm)
surface tilt M (0) => TAKE OFF=35
TEM different !!
Quantitative X Quantitative X- -Ray Analysis Ray Analysis
=> ZAF => ZAF Corrections Corrections
atomic number effect (Z)
Fe+Cr
electron beam (PE)
FeCr alloy
Cr
BSE yield
(different to pure
substances)
TEM:
thin foil!!
61
Quantitative X Quantitative X- -Ray Analysis Ray Analysis
=> ZAF => ZAF Corrections Corrections
absorption (A) and fluorescence effects(F)
Fe+Cr
electron beam (PE)
FeCrNi alloy
Cr
Fe
Fe
Fe
absorption
Fluorescence
8 Case Studies & Discussion
62
Biological Biological Specimens Specimens
fly detail of the wing surface - vacuum dried
(alterantive: environmental SEM)
Phase Phase Characterization Characterization
Ti nitride in NiCr alloy (deep etched/EDS)
63
Phase Phase Characterization Characterization
Ti sulfidein CMSX-6 (polishedand Au sputtered)
Phase Phase Characterization Characterization
phase in SRR99 (electropolished - perchloricand aceticacid)
64
Phase Phase Characterization Characterization/Analysis /Analysis
( ( phase phase in in Ni Ni- -base base superalloy superalloy CMSX CMSX- -6) 6)
200nm
EDS 1
EDS 3
EDS 2
Fracture Fracture Surfaces Surfaces
striations
dimples
65
Damage Damage Analysis Analysis
broken implant (=>metal fatigue)
3D Images of 3D Images of Fracture Fracture Surfaces Surfaces
about 5tilt
66
Damage Damage Analysis Analysis
corrosion corrosion EDS EDS analysis analysis