A SEMINAR ON THE TOPIC

TEM SAMPLE PREPARATION

PREETISH D’SILVA
MT13F05
 CONTENTS
1. Requirements of a TEM Specimen
2. Types of TEM Specimen
3. Flow chart of Sample Preparation for
different material geometries
4. Preparation of Self Supporting Disk
5. Specimen on Grids or Washers
6. Cross Section Specimen
7. Focused Ion Beam (FIB)
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 REQUIREMENTS OF A TEM
SPECIMEN
• Should be electron transparent thin(<1µm)
• representative of the material you want to
study
• specimen to be uniformly thin,
• stable under the electron beam

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 Types of TEM Specimen
• Self Supporting specimen- Whole specimen consists of one
material ( Eg: Composites, metals )
• Specimens on a support grid or thin washer (made of usually
Cu, also Au, Ni, Be, C, Pt, etc.)
– Usually the specimen or grid will be 3 mm in diameter

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 Flow chart of Sample Preparation for
different material geometries

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 PREPARATION OF SELF
SUPPORTING DISK

Preparation of Self supporting Disk involves

four stages
I. Initial thinning to make a slice of material
between 100 and 200 µm thick.
II. Cut the 3-mm disk from the slice.
III. Prethin the central region from one or both
faces of the disk to a few micrometers.
IV. Final thinning of the disks
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 I. Forming a Thin Slice from the Bulk
Sample (<200µm)
a. Ductile Materials (Metals)
– Aim is to avoid mechanical damage to sample as defects
are to be studied.
– Used of a chemical wire/string saw, a wafering saw, spark
erosion or by rolling.
b. Brittle Materials (Composites)
– Here there are two cases: (i) where you must not introduce
mechanical (ii) where you don’t mind introducing
mechanical damage or the material won’t damage
– Use of a Razor blade for cleaving , Ultramichrotome or
diamond wafering saw for slicing.

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 II. Cutting 3-mm Disk (Coring)

• Ductile Material :
– Mechanical Punch
• Brittle Material :
– Spark Erosion,
– Ultrasonic Drilling
– Grinding Drill.

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a. mechanical punch b. abrasive-slurry disc cutter
c. ultrasonic cutter d. spark-erosion cutter
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 III. Prethinning the Disk (Dimpling)

• Aim is to thin the center of the disk to produce

regions with 10µm thickness.
• Mechanical Dimpler uses a small radius tool to
grind and polish the disk to a fixed radius of
curvature in the center.
• Dimpling is done by gradually decreasing the
‘grit’ size and conclude with the finest available.
• Precision dimpling with microprocessor control
can sometimes produce electron-transparent
specimens which are <1 µm thick.
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 Dimpling (contd….)
• Dimpling can also be performed chemically.
• In the case of Si this is achieved by allowing a jet of
HF and HNO3 to impinge on the Si disk.
• The HNO3 oxidizes the Si and the HF removes the
SiO2.
• Similar approaches use Br and methanol for thinning
GaAs.
• This dimpling method uses dangerous chemicals, but
it is very efficient.
• It can even be carried to final perforation with care
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Surface dimpling using a chemical solution, e.g., to remove Si from one side of a disk. The light
pipe permits visual detection of perforation using the mirror.
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 IV. FINAL THINNING OF THE DISKS
A. ELECTROPOLISHING
 used for conducting samples such as metals and alloys.
 it can produce foils with no mechanical damage but it can
change the surface chemistry of the specimen.
• Basic principle: There is a certain applied voltage at
which the current due to anodic dissolution of the
specimen creates a polished surface rather than etching
or pitting.
• By keeping the volume of the reservoir constant, the jet
falls under constant pressure. The voltage is applied
between the tip of the pipette and the specimen.
• A twin-jet apparatus can be used to pump a jet of
electrolyte onto both sides of the dimpled disk.
• A laser beam or light sensor detects transparency of disk.
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(A) Electropolishing curve showing the increase in current between the anode and the cathode
as the applied voltage is increased. Polishing occurs on the plateau, etching at low voltages, and
pitting at high voltages. (B) The ideal conditions for obtaining a polished surface require the
formation of a viscous film between the electrolyte and the specimen surface.
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(A) Jet electropolishing by allowing a single jet of gravity fed electrolyte to thin a disk supported
on a positively charged gauze. The disk has to be rotated periodically. (B) Schematic of a twin-jet
electropolishing apparatus. The positively charged specimen is held in a Teflon holder between
the jets. A light pipe (not shown) detects perforation and terminates the polishing.
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 IV. FINAL THINNING OF THE DISKS
B. ION MILLING
• Ion milling involves bombarding the delicate thin
TEM specimen with energetic ions or neutral atoms
and sputtering material from the film until it is thin
enough to be studied in the TEM .
• The variables to control include the voltage,
temperature of the specimen, the nature of the ion and
the geometry.
• An accelerating voltage of 4–6 keV is usually used.
• we minimize the ion beam penetration by inclining
the incident ion beam to the surface of the specimen
at <5˚ to avoid preferential thinning and minimize
ion implantation. Dept of Metallurgical & Materials
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(A) Schematic diagram of an ion-beam thinning device: Ar gas bleeds into an ionization chamber
where a potential up to 6 keV creates a beam of Ar ions that impinge on a rotating specimen.
Although not shown, the whole apparatus is under vacuum. The specimen may be cooled to
liquid-N2 temperatures and perforation is detected by the penetration of ions through the
specimen. (B) Typical ion mill.
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 B. ION MILLING (contd…)

• The principal variables for the sputtering yield during

bombardment are
– The ion: mass, energy, charge, and angle of incidence.
– The ‘target’: mass density, atomic mass, crystallinity,
crystal structure, and orientation.
• Ar is used because it is inert, heavy, and not naturally
present in most samples.
• Special applications may use reactive ions like iodine, or
add oxygen, etc in semiconductor processing.
• Cooling the specimen is recommended for almost all
materials.
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Figure: Variation in penetration depth and thinning rate with the angle of incidence.
High-incidence angles promote implantation, which is undesirable. The rate of
thinning reaches a maximum at 20° incidence, after which the beam penetrates rather
than sputters the sample surface. Initial thinning should start at 20–30° reducing to
<10° as perforation approaches.

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 B. ION MILLING (contd…)

• Ion milling is the most versatile thinning process, being

used for ceramics, composites, polyphase semiconductors
and alloys, and many cross section specimens.
• In addition, fibers and powders, which constitute a wide
range of important materials, can also be thinned by ion
milling.
• To do this, you have to first embed the particles or fibers in
epoxy and transfer the mixture into a 3-mm brass tube for
strength.
• The next step is to saw the tube/epoxy mixture into 3-mm
disks and finally dimple and ion mill to electron
transparency.
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Figure: Sequence of steps for thinning particles and fibers by first embedding them in
epoxy and forcing the epoxy into a 3-mm (outside) diameter brass tube prior to curing
the epoxy. The tube and epoxy are then sectioned into disks with a diamond saw,
dimpled, and ion milled to transparency.

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 SPECIMENS ON GRIDS/WASHERS
• Electron-transparent portions of the specimen
or particles are created and then are supported
on a thin film on a grid or washer.
• We can deposit these small particles on
amorphous or crystalline films. The classic
example is the amorphous carbon film.
• The thin supporting film should have a uniform
thickness.
• The particles may stick to the film or may have
to be clamped between two grids.
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 A. Electropolishing-The Window Method
for Metals and Alloys
• First cut a thin sheet of metal into a square 10 mm on the side, then seal the
edges with a polymer lacquer to prevent preferential attack.
• The ‘window’ of exposed metal is immersed in electrolyte surrounded by a
cathode and a voltage is applied.
• The solution may or may not be stirred. The correct voltage will ensure that
a viscous layer of electrolyte builds up at the surface of the specimen which
results in uniform controlled thinning without pitting or corrosion.
• After some time, the sheet is removed, cleaned, and turned through 180° and
replaced in the bath as shown schematically.
• After several rotations the sheet will finally thin in the center.
• After perforation, remove the sheet and cut off slivers of material from
around the perforation using a scalpel under an inert solvent such as ethanol.
• Catch the floating slivers on oyster grids, dry them and they are ready for
viewing.
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Window polishing. (A) A sheet of the metal 100mm2 is lacquered around the edges and made
the anode of an electrolytic cell. (B) Progress during thinning: the initial perforation usually
occurs at the top of the sheet; lacquer is used to cover the initial perforation and the sheet is
rotated 180°and thinning continues to ensure that final thinning occurs near the center of the
sheet; if the final edge is smooth rather than jagged it is probably too thick.
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 B. Ultramicrotomy

• A microtome is used to cut very thin tome (piece cut off). For the
TEM the slices may be <100 nm thick and the instrument is known as
an ultramicrotome.
• The principal advantages of the technique are that it leaves the
chemistry unchanged and can be used to create uniform thin films of
multiphase material.
• The main disadvantage, of course, is that it fractures and/or deforms
the samples and therefore is most useful in cases where the defect
structure is of secondary (zero) importance.
• The ultramicrotome operates by moving the specimen past a knife
blade.
• The blade can be glass (cheap) for soft materials but will be diamond
for harder ones.
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Ultramicrotomy. (A) The sample is first embedded in epoxy or some other medium or
the whole sample is clamped and moved across a knife edge. (B) The thin flakes float
off onto water or an appropriate inert medium, from where they are collected on
grids.

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 C. Grinding and Crushing

• Many brittle materials such as ceramics and minerals are most

easily prepared by crushing in a clean pestle and mortar
preferably in an inert liquid.
• The liquid containing the particles can then be ultrasonically
stirred and allowed to settle.
• A drop of this liquid, if placed on a holey carbon film on a
grid, will evaporate in a dry environment, leaving a
distribution of the particles on the support film.

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 D. Replication and Extraction

• Replication is used to study fracture surfaces or surface topography in

general.
• Evaporate a carbon film on the surface of interest, then etch away the
underlying surface with an acid so that the carbon film floats off.
• If you coat this film with a heavy metal at an oblique angle, you will
thus produce a sample that shows enhanced mass-thickness contrast;
support the film on a grid for observation.
• Alternatively first replicate the surface by softening a plastic, pressing
it on the surface, and allowing it to harden.
• Pull off the plastic replica, coat it with carbon, then dissolve the plastic
with a suitable solvent, and pick up the carbon replica on a support
grid.
• If the carbon replica is produced directly from a metal surface, it may
be necessary to dissolve some of the metal with acid then float off the
carbon onto distilled water before picking up on a grid.
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(A) Replication of a surface by the two-step
method: spray acetone on the surface to be
replicated before pressing a plastic (usually
cellulose acetate) onto the surface which
softens in contact with the acetone; the
plastic is removed from the surface when it
has hardened and a C, Cr, or Pt film is
evaporated onto the replicated plastic
surface; the plastic is then dissolved with
acetone and the evaporated film retains the
original topography.

(B) alternatively, the direct carbon replica

of a metal surface may be floated off on
distilled water after scratching the carbon
and etching to free the film, which may
subsequently be shadowed obliquely to
enhance the topography.

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(A) Making the extraction replication: particles
embedded in a matrix are revealed by etching
the matrix, which leaves the particles
standing proud of the surface; a thin
amorphous carbon film is evaporated over
the particles, then the rest of the matrix is
etched away leaving the particles adhering to
the carbon film.
(B) Example from a Ƴ/Ƴ‘ alloy showing not only
that the articles are mainly located at the
grain boundaries but also the different
contrast from Ƴ‘ grains and two-phase Ƴ/Ƴ‘
grains.

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 E. Cleaving and the SACT
• Cleaving is used to make thin specimens of graphite, mica,
and other layer materials that are weakly bonded along one
plane.
• The idea is to attach adhesive tape to both sides of the sample
and then pull the two pieces of tape apart. This process is
repeated until the specimen is thin enough for TEM.
• A special variation on cleaving, known as the small-angle
cleaving technique (SACT) is employed presently.
• The idea is to propagate a crack through the sample along a
plane that is not a natural (crystallographic) fracture plane and
then create another crack that is shallowly inclined to the first
fracture surface.
• The technique can be applied to crystalline samples such as Si
coated with thin films or to coated glass Samples that have no
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SACT of a coating on glass. (A) Scratch the sample; (B)cleaving along the scratch;
(C, D) TEM images.
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 F. The 90° Wedge

The 90°-wedge specimen: (A) prethin to create a 2-mm square of the multilayers on a Si
substrate; (B) scribe the Si through the surface layers, turn over, and cleave; inspect to make sure
the cleavage is clean, giving a sharp 90° edge; reject if not; (C, E) mount the 90° corner
over the edge of a hole in a Cu grid; (D, F) then insert in the TEM; note that two different
orientations are available from a single cleavage operation.
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 G. Lithography

Etching of a multilayer sample (A).Etch away most of the sample, leaving a small etched plateau
(B) mask a region <50nm across and etch away the majority of the surrounding plateau. If this
thin region is turned 90° and mounted in a specimen holder (C), the interfaces are now parallel
to the electron beam.
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 H. Preferential Chemical Etching

Lithographic techniques applied to thinning a

multilayer specimen:
(A) the un-thinned sample is shown with a grid
of Si3N4 barrier layers evident. Etching between
the barrier layers, shown in (B), produces an
undercutting down to the implanted layer which
acts as an etch stop, producing a uniform layer
~10 mm thick. Further thinning with a different
solution produces large areas of uniformly thin
material (not shown) supported by the Si3N4 grid
and the remaining un-thinned regions.
(C, D) A commercial Si3N4 thin films support disk;
(D) is the enlarged view.

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 CROSS-SECTION SPECIMENS

Schematic sequence for cross-section specimen preparation: the sample is cut into
thin slices normal to the interfaces which are glued together between spacers which
could be Si, glass, or some other inexpensive material so that they are wider than the
slot in the grid. The ‘club’ sandwich is then itself glued to the grid (over the slot) and
ion milled to perforation.

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 FIB- Focused Ion Beam
• We can think of the FIB essentially as an SEM
with a built-in ion mill.
• The single ion gun produces a well-controlled
beam of Ga ions .
• The ion beam also acts as the electron beam of
the SEM with the secondary electrons being
used to form the ‘SEM’ image of the sample.

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Schematic of a two-beam (electron and ion)
FIB instrument.

Stages in making TEM samples using a FIB instrument. (A) The area of interest has been
marked. (B) A Pt bar is deposited to protect this area from the Ga beam. (C, D) The two trenches
are cut. (E) The bottom and sides of the slice are (final) cut. (F) The TEM specimen is polished in
place before extracting it. Dept of Metallurgical & Materials
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 Figure: Summary flow chart for specimen preparation.
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 Source
• Transmission Electron Microscopy- A
Textbook for Materials Science (4 volumes) -
David B. Williams & C. Barry Carter , 2nd
edition, 2009.
• Transmission Electron Microscopy (TEM) :
sample preparation guide

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 THANK YOU

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