MM3100-Transmission Electron Microscopy-1

Vir Karan MM19B057

February 2022

1 Slow-speed diamond cutter

Primarily used for slicing down bulk metallic samples for use in TEM. Firstly,
the sample is fixed in the slot provided and fastened. Then, the diamond blade is
attached and adjusted and the sample and blade are aligned together. Once the
alignment of the sample to the zero level is done, by further rotation (10 readings
gives a thickness of 100 micron) of 6 readings to account for the thickness of
the blade, around 400 microns of the sample can be prepared for use in TEM.
During the cutting, some water and oil has to be provided to prevent the blade
from corroding and to act as a coolant. After switching the machine on, the
RPM of the blade can be adjusted and the cutting can be done.

2 Disc punching
After obtaining 300-400 micron of the sample after diamond cutting, the sample
has to be gently polished using an abrasive paper to reduce the thickness down
to around 100 microns. Then, this reduced sample is placed in the disc punch
and a disc of around 3 mm diameter is cut out.

3 Ultrasonic disc cutter

Used to prepare brittle samples that cannot be cut down to 3mm discs using
the diamond cutter and disc punching. This machine contains a piezoelectric
device connected to a transducer which provides an ultrasonic wave to one plate
that cuts the sample. A schematic of the machine and its components is shown
in Figure 1. First, the sample is pasted onto a hot plate using glue and then
it is left for some time to allow the temperature of the plate to reduce to room
temperature. Then, the specimen table is placed into the slurry-retaining ring
and then placed onto the magnetic platform. To cut the sample, the cutter has
to be pulled down and some abrasive powder (consisting of Silicon carbide and
Boron carbide) has to be applied, after which the machine can be switched on.
Before turning off the machine, the cutter has to be pulled back up to ensure
that it doesn’t damage the cut sample.

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Figure 1: A schematic showing the Ultrasonic Disc Cutter and its components.

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4 Dimple grinder
Once the 3mm discs have been obtained, the sample is further thinned down
significantly at a point using the dimple grinder. This is done as follows: Using
adhesive, the 3mm diameter disc punched from the ground sample is adhered to
the stub. This adhesive melts at 130°C and cools to set. To adhere the sample
to the stub, it is heated to 130°C and adhesive is applied to the centre. Then,
the sample is placed in the middle of the stub on the adhesive and dried. The
stub is then fixed to the magnetic stage and a microscope is used to check the
sample’s position. If not done properly, the dimple will not form in the centre
of the sample, but rather at the edges, which is inconvenient for subsequent
preparation steps. The grinding tool is then lowered onto the sample after it
has been adjusted to the centre. The dial reading is adjusted with the dial
gauge and the thickness reduction reading is monitored. Ion milling is done for
further preparation once the sample thickness has been reduced sufficiently in
the centre. Throughout the process, the sample has to be handled with care
and cleaned thoroughly.

5 Precision ion polishing system (PIPS)

Prior to using PIPS, beam aligned must be done. First, a screen is placed inside
the system and a vacuum is created. The gun angles are adjusted and the gas
flow of one of the guns is turned off. The screen is rotated, timer is set and the
gun voltage is adjusted to the desired values. Then, the gas flow can be varied
and the beam profile can be noted. The beam’s thickness has to be adjusted so
that it is slightly larger than the central hole in the screen. In case the beam is
off-centred, it can be adjusted using the beam alignment tool. Once this process
is done for one gun, it can be switched off and the same can be repeated for the
other gun. Then, both guns can be switched on and the gas flow is adjusted so
that the beams intersect at the centre of the screen. If this does not happen,
the beams can be further adjusted. Once beam aligned is done, the sample can
be ion-milled. To do so, the sample is placed in the sample holder, and placed
inside the PIPS equipment and vacuum is created. The gun angles, timer and
voltage are adjusted and ion-milling is done. Hole formation is viewed through
the microscope. Once the hole forms, polishing is done by lowering the gun
angle and beam energy.

6 Twin jet polishing machine

Only used for electrically conducting samples like metals and alloys. Samples
obtained after this step are free from mechanical damage. This step works on
the principle of applying a voltage and a current, causing anodic dissolution
which leads to a polished surface of the sample. An electrolyte is filled (which
depends on the material in the sample) and the set-up is placed on top. The
3mm disc specimen is placed in a holder and inserted into the set-up. Once the

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machine is switched-on, parameters such as applied voltage and temperature
are adjusted. Once a critical light act value is reached, the specimen has to be
taken out of the set-up and cleaned to prevent further etching. Then, a sample
free from mechanical damage is ready to be put in the TEM.