Introduction:

The design of this experiment is made to give us the opportunity to

closely investigate featured characteristics about the macrostructure of different
metallic samples using the methods of:

1. Macroetching.

2. Sulfur printing.

Theory and Discussion:

Macrostructure: is the structure that can be seen by the naked eye or

magnification up to10x.

Carrying out macrostructure examinations allows one to:

a. Determining the mythology of manufacturing processes which can

be:

1. Rolling: in which the material is passed through the gap between

two rotating rollers that squeeze the material as it passes between
them. The rolled material emerges with a thickness roughly equal to
the gap between the rollers.
 This manufacturing process can be identified by the shape of the
elongated grains in the rolled plates.

2. Extrusion: produces parallel flow lines that can be revealed by

macrostructure examination.

3. Forging: used to form plates that are either hot or cold.

b. Heat treatments: such as carburizing and case hardening.

c. Determining the grain size.

d. Detecting physical defects.

Objective:
1. Implementing macroscopic methods to differentiate between two
aluminum samples, where one was subjected to a fast cooling rate
while the other was subjected to a slow cooling rate.

2. Study the macrostructure of two steel samples, one that has been
carburized and the other was subjected to welding in which a type of
defects is expected.

:Materials
The material required for this experiment might include selected
weldments, castings, cold formed and forged parts, and various
.chemical reagents

• Silver bromide photographic papers.

• 2-5% solution of H2SO4.
• Photographic fixing solution.

:Apparatus
The apparatus required is an abrasive belt machine for producing a
.smooth surface as well as silicon carbide papers

Etching apparatus includes a hot plate, Pyrex etching bowls or beakers,

.,stainless steel tongs, rubber gloves, fume hood

:Procedure
The normal procedure for macro-examination involves the following
:steps

• Obtain a specimen from the instructor.

• Cut or section the specimen if necessary. Clean all
adhering dirt or grease with a suitable solvent.
• Prepare a flat surface using the abrasive belt machine or
file using emery paper of degrees (120, 180, 240, and 400) in this
order.
• Select and prepare the proper etching solution in the
beaker and if necessary, bring it to the recommended
temperature on the hot plate. Slowly and carefully immerse the
specimen in the solution using stainless steel tongs.
• Etch the specimen for a few minutes. Remove, wash
carefully, and examine the progress of etching. Too short a time
will not allow detail of the structure to completely develop. Too
long an etching time may obliterate the structure. Continue
etching the specimen until the desired results are obtained.
• Remove the specimen from the reagent; wash in running
water. During rising, carefully scrub the specimen surface with a
soft-bristle brush to remove deposits formed on the specimen
 during etching. Rinse the specimen in alcohol to remove last
traces of water and dry on hotplate or in a warm air blast. If the
specimen is to be preserved, coat it with a light coat of clear acrylic
spray.
• Record on the data sheet the details of the procedure
followed, including etchant, time and temperature.

Results and Conclusions:

In this experiment two aluminum specimens and two steel specimens are used.

The first aluminum specimen is obtained by sand casting, the specimen was
cooled in the air, and one could see that the outer grains are bigger than the
internal ones; that is due to the interaction with air and the small time of the
grains forming, the outer grains didn’t have enough time to recrystallize thus
they have wider diameters. When moving inside the specimen one could see
that grains size decreases, that is due to the longer time the inner grains had to
form thus they are smaller and more uniform.

The other one was uniform; it's more likely to be obtained by fast cooling rate
processes such as die casting, and that's why we can't see equi-axed grains.

Figure (1): Comparing the rates of cooling according to (Axed-grains)

The steel sample was studied where we used etching and we looked at the
dark brown spots that indicate the position where the carbonization took place
(case hardened so one could obviously see the luminous bounds of the
specimen due to carbon impurities (carbonizing)).

The Carburized steel

The two aluminum .sample
samples.

1: slow cooled
sample. 2

2: fast cooled
 1
.A defected specimen

Figure (2): Samples we used in the experiment.

In sulfur printing; the sulfur exists in the forms of FeS or MnS, thus when
applying the 10% H2SO4 solution, and with using the AgBr photographic
:paper the chemical reactions happens to be

FeS or MnS + H 2SO 4 

→FeSO 4 or MnSO 4 + H 2S( gas )
Then
H 2S( gas ) + 2AgBr 
→Ag 2S + 2HBr

The Ag2S is in the form of dark brown spots showing the sulfur
.distribution in the steel specimen used
 .Figure (3): Sulfur printing photo graphic paper

Answers to questions in the lab

manual:
Etchant
Material Time needed Temperature
composition

H2O 75%
Steel 1-2 min
25% HNO3

HF 15%

HCl 25%
Aluminum 1-2 min
HNO3 35%

25% H2O

Questions:

1. How did you choose the etchant to reveal the

microstructure?

Based on the consideration the chemical reaction that would happen

and thus the etchant is chosen to react with grain boundaries depending
on the type of the material to be examined using table.1 in the laboratory
manual.

2. What are the reasons for inhomoheneity in grain structure,

chemical composition and mechanical properties?
 Inhomoheneity in Grain structure: such structures result from different
solidification rates, crystal growth, gas evolvement or thermal
processing.

Inhomoheneity in Chemical composition: results from segregation due to

impurities in the metal or from surface treatments such as carburizing.

Inhomoheneity in Mechanical properties: they arise from plastic

deformation in forged or rolled parts.

3. Show the Inhomoheneity in grain structure and chemical

composition on the photographs you printed in the experiment.

The left picture show the Inhomoheneity in grain structure where we can see
the equi-axed grains resulted from slow cooling rates.

The right picture shows the bad distribution of added impurities in a carburizing
process of steel.
Experimental Laboratory in Materials
Science and Engineering

Experiment No.1

Macroscopic Examination

Group Members:

Student Name: Reg. No.