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Practical exercise -7
Topic: Preparation of micro specimen for microanalysis.
The purpose of the work:
to study the preparation of microslices for microanalysis.
Theoretical information
A cylinder with a diameter of 10-12 mm and a height of 8-10 mm or a cube
with an edge of 10-15 mm is cut from the zagotovka on a cutting tool for micro-
grinding. Then the surface of the sample is smoothed by rubbing with a special ego
or wheel with small teeth and is rolled on a fast rotating disk surrounded by a soft
material.
The cleaned and flattened sample is first washed in water, then in alcohol or
gasoline and dried.
is treated with a chemical reagent ( 4% solution of NNO2 in ethyl alcohol ).
After treatment with reagents, the sample
is washed again with water, then
alcohol or gasoline, and dried using filter paper. After that, the sample is ready for
inspection.
1 . Microslice inspection process.
Defects in the surface cleanliness of the microsand break the rays falling on the
surface of the part, redirect them to other sides and reduce the useful efficiency of
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the ray. Since the resulting image is visible through the reflected light falling on the
surface of the detail, it also has a negative effect on the quality of the image.
2 . Two-disc microgrinding device.
One side of the disc has a 1 on the other side, and a 0 on the other. First it
spins on the 1 side, then on the 0 side.
Examining the external appearance and structure of any materials, i.e. solids,
including metals, with the help of an ordinary eye or a lens (loupe)
is called
determining its macrostructure
. Usually, lenses or magnifiers magnify the actual
size of objects up to about 30 times. In order to determine the macrostructure of the
material, the surface of the samples prepared from it is polished and cleaned, such a
sample is called
a macroslide .
When determining the macrostructure in the
experiment, samples with a thickness of 10 to 20 mm are prepared from carbon steels
that have not been found, that is, rolls. When steels are macroanalyzed, it is often
determined whether there are liquefaction phenomena in them, the presence of voids:
sulfur, phosphorus, manganese and gas bubbles, air voids, cracks or not . It should
be said that the degree and character of liquation depends not only on the amount of
carbon
and waste rock , but also on the conditions of depositing the metal,
crystallization of the ingot, and pressure treatment.
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Sulfur liquefaction in steels is determined by the Bauman method. Liquation of
phosphorus in steel is determined by treating steel with the following reagent: 85 g
of copper chloride (SuSl
2
) and 53 g of ammonium chloride (NN
4
S1) are dissolved
in 1000 cm
3 of water.
Determination of sulfur liquation.
1. The surface of the smoothed sample is cleaned by wiping with cotton soaked
in alcohol.
is kept in 5% sulfate solution for 6 minutes , then it is removed from the solution
and dried between filter paper. When the dried photo paper
is glued to the prepared
macroslide sample with the emulsion side, it is pressed with ash. In this case, the air
between the photo paper and the macroslide will escape. After 2-3 minutes, the photo
paper is copied from the sample.
3. The copied photo paper is washed with water, then in a 25% solution of
sodium hyposulfite in water for 3-4 min. held and washed again in water and then
dried. The brown areas on the photo paper show areas of sulfur accumulation (sulfide
deposits) in the sample.
It is known that sulfur is found in steel in the form of chemical compounds MnS
and FeS with manganese and iron .
4. These compounds react with sulfuric acid and release hydrogen sulfide N
2
S.
If sulfur is liquified (entered) in the macroslide (sample), then the hydrogen sulfide
(N
2
S) released as a result of the experiment with silver bromide (AgVg) on the
photo paper reacts and silver sulfide (Ag
2
S ) produces.
This will appear as the brown part on the
photo paper
Determination of phosphorus liquation.
1.
The surface of the smoothed sample is cleaned by wiping with cotton soaked
in alcohol.
2.
The sample is placed in the above-mentioned reagent (a mixture of copper
chloride and ammonium chloride) and held for 1-2 minutes. The iron contained in
the sample dissolves in the reagent and squeezes the copper. The extruded copper
adheres to the sample surface.
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3.
The copper on the surface of the sample is washed in a stream of water and
wiped with a damp cloth.
4.
The sample is dried. Dark spots (parts) that appear on the sample will be areas
enriched with phosphorus, because the more phosphorus in iron, the better and faster
it dissolves.
5.
Draw the traces formed on the sample and
characterize the phosphorus
liquation.
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