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1.

AIM: To study the microstructure of Nickel Oxide and

calculation of activation energy.

2.MATERIALS & EQUIPMENT: Pure nickel(Ni), emery


papers and silica colloidal solution for polishing the
sample, Electric furnace calibrated in the range of 1000 0 C
to 12000 C, Optical microscope, Resin to mount the
sample, Gold sputtering Equipment, Scanning Electron
microscope.
3.PROCEDURE OF EXPERIMENT:
a)
We took three nickel samples which are very pure and
then polished both sides thoroughly with the help of
emery papers ,maintaining the order upto P3000 grade (6
micron size).During the polishing ,we obseved the surface
of the nickel in an optical microscope to understand the
proper direction of the scratch.
b)after appropriate polishing,we kept the samples inside
the electrical furnace at 12000 C,exactly for 9 hours under
normal atmospheric pressure 100kPa and also in presence
of air.
c) after 9 hours heat treatment inside the furnace,the
samples were cooled
d)after cooling,each sample were cutted carefully into two
parts from the middle and mounted in resin.
e)Now this cutted samples were polished again by using
emery papers with the same procedure as we did
initially ,maintaining the order upto the P3000 grade.after
polishing in emery paper,thse were cloth polished by using
silica coloidal solution.
f)Now,after all these polishing of these samples,they were
wrapped in thin Aluminium foil and then we did gold
sputtering on each sample as NiO is insulator.

g)Microstructures of these samples were observed by


using Scanning Electron Microscope(SEM) in Back
Scattered Electron(BSE) mode.
THEORITICAL POINT OF VIEW: The whole point of this
experiment was to study the kinetics behaviour of a
nickel-nickel oxide system(or in general metal metal oxide
system).In another point of view ,it is really very important
to understand the actual oxidation behaviour of nickel as it
is one of the most fundamental supralloy,used at high
temperature.So,it is important to know the thickness of
the oxidation layer on nickel surface.The thickness of the
oxidation layer increases with temperature and the
obvious reason is diffusion as X=(Dt)^0.5 where X is the
thickness of the oxidation layer thickness,D is coefficient
of diffusivity and t is time and D exponentially increases
with temperature.Here this increase of oxidation thickness
layer is mainly due to the diffusion of nickel cations(Ni++)
on the outward nickel surface.the oxide layer shows
duplex morphology ,where external columnar grains
formed on the outward diffusion of nickel and an equiaxed
oxide grains formed on inner oxide layer part.So from this
duplex morphology,it can be said that there is also inward
oxygen flow occurs though the growth of oxide layer is
mainly due to outward diffusion of nickel.
The reason for this inward oxygen flow is the formation of
micro-channels and the pores inside the oxidation layer
creates this micro-channels and oxygen can easily diffuse
through this micro-channel path.But duplex morphology
can not be seen at any temperature as the micro-channels
forms
above
8000C.So.duplex
morphology
is
a
temperature dependent morphology and inward diffusion
of oxygen can be controlled by preventing micro-channel
formation.

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