dimpled specimen

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The extration replica technique

(a) polished surface

(b) etched to expose second phase

(c) carbon coated

(d) re-etched and replica floated off

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Single stage replication:

a-specimen
b-carbon coating
c-final replica
Two stage replication:
d-specimen, e-intermediate thick plastik coating,
f- plastic replica (inverted), g-carbon coating, h-final carbon replica
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Carbide in steel

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Precision cut-off and grinding

Automatic cut-off machine

Accutom 50
Application area:
Automatic cut-off and grinding
Cut-off of samples for TEM-preparation
Grinding of samples for TEM/SEM-sample
preparation
Producer: Struers
Variable wheel speed of 300 rpm - 5000 rpm
Feed speed: 0.005 mm/s -3.000 mm/s
Position accuracy: 5 m
Al2O3 and diamond cut-off wheels
Diamond cup wheels for hard, brittle and
ductile materials (91 m, 40 m)

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Seite 5

Wire saw

A wire saw produces very fine slices from a

material with just small stress to the sample.
This procedure is applied to brittle materials,
but also for cross section preparartions.

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Seite 6

Duo Mill Ion mill

Application area:
ion milling of mechanically prepared specimens
ion milling of electro polished specimens
cooled ion milling of beam sensitive specimens
Producer: GATAN Inc.
Operation voltage: 1000 V - 4000 V
Cathode: Octogun
2 coolable specimen stages (liquid nitrogen)
Vacuum: 2 rotation pumps, 1 oildiffussion
pump

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Seite 7

Precision Ion Polishing System (PIPS)

Application area:
ion milling of mechanically prepared specimens
ion milling of electro polished specimens
Producer: GATAN Inc.
Operation voltage: 2000 V - 5000 V
Vacuum: 1 membrane pump, 1 turbo
molecular pump (oil free)

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thin with the ion etching system

ion source
specimen

ion beam

ion source

the surface of the rotating sample,

with the help of two ion beams removed

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the ablation rate depends on the angle

between ion beam and sample surface

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Seite 9

Mounting specimens in an ion beam mashine

a) Schematic diagram
b) and c) two types of holder which
permit double-sided thinning
In c) the gear teeth engage in a mount
which enables the whole plate to be
rotated while ion beams are directed
at both sides of the disc D

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Seite 10

Electrolytic thinning
TenuPol-5
Application area:
electrolytic thinning of TEM samples
automatic shut-off through infra-red sensor
Producer: Struers
Controlled operation temperature down to
-30C with cooling unit.

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Seite 11

Tenupol 5
Installation of the electropolisher Tenupol
in a fume cabinet

Tenupol specimen holder and installation of a

disc specimen
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Seite 12

Elektropolishing

Schematic diagram illustrating the

action of a jet thinning technique

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Seite 13

Tenupol 5

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Seite 14

Tenupol 5

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Ideal current-potential curve

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current density

typical current density-voltage curve at the thin

electroplating of metals

gas development
polishing
etching
voltage
The best polishing conditions prevail in the range of 2
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Seite 17

Fluid dynamic parameters

Polishing profiles dependendent on the fluid dynamic parameters

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Seite 18

FIB preparation: Lamellar-Transportation I

Transmission Electron Microscope Sample Preparation Using a Focused Ion Beam

in-situ: using a Kleindiek-micromanipulator

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Seite 19

FIB: Focussed Ion Beam

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Seite 20

FIB Preparation of TEM specimens

Mechanical thinning on
about 100 microns and
defining a sample area

Advantages:
targeted preparation
Fast preparation (approx. 2 hours)

Disadvantages:
Material ablation with high
intensity ion beam

No samples for HRTEM because

of the sample thickness (100 nm) and
surface amorphisation
high investment costs
FIB

Material removal with ion

beam of lower intensity, until
a thin lamella remains. These
will be removed and
directly in the TEM can
be investigated

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Seite 21

FIB preparation: Lamellar-Transportation II

Fixing the
TEM lamella to
W-tip by means
FIB-deposition,
then complete
Isolation of Lamella

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Seite 22

FIB preparation of Nanowires

Nachfolgende FIB-Abscheidung

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Seite 23

FIB preparation : gradually after processing

Transportation to
sample holding
system

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Seite 24

TEM specimen

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Seite 25

References

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MoKo Sommersemester 2004, K. Tracht

Seite 26

References

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MoKo Sommersemester 2004, K. Tracht

Seite 27