Materials Sciences Lab

JULY 8, 2024
 A material is defined as a (most often a solid, but other condensed phases
can be included) that is intended to be used for certain applications.
Materials can generally be further divided into two classes: crystalline and
non-crystalline. The traditional examples of materials are metals,
ceramics, composites, and polymers.

The classifications of fabrication techniques are shown in Figure (1)

The classifications of fabrication techniques include various ceramic forming

methods shown in Figure (2)

1
1- according to the type of continuous phase (matrix) material Metal-
matrix composite (MMC) A composite material that has a metal or metal

2
alloy as the matrix phase Ceramic-matrix composite (CMC) A composite
for which the matrix phase is the ceramic material Polymer-matrix
composite (PMC) A composite for which the matrix phase is a polymer
resin

2- According to the discontinuous phase (reinforcement) material

 Fibrous (long or short) Composites
 Particulate Composites
 Laminate Composites

Select materials and distinguish between them.

 To understand the outline of the manufacturing process.
 To know the methods of manufacturing each material, studying its
various properties, and being able to use it in daily life applications.

1. Determination of composition (weight percent) for a powder of

Material.
2. Weight of powder material by the sensitive balance.
3. Mix the powder of the material with the ball mill machine.
4. Press mixtures in the hydraulic piston.
5. Sintering or heat treatment of compressed materials

1- Compare the physical and mechanical properties of the materials

(metal, ceramic, and polymer) for 10 different?

2- What is the most electrically conductive material and why?

3
The heat treatment process is a series of operations involving the heating and cooling
of metals in the solid state. Its purpose is to change a mechanical property or
combination of mechanical properties so that the metal will be more useful,
serviceable, and safe for a definite purpose. By heat treating, a metal can be made
harder, stronger, and more resistant to impact; heat treatment can also make a metal
softer and more ductile. The only disadvantage is that no one heat-treating operation

can produce all of these characteristics. Some properties are often improved at the
expense of others. In being hardened, for example, a metal may become brittle.

4
o Annealing
o Normalizing
o Quenching or Hardening
o Tempering

Annealing is the process of softening materials or bringing about required changes

in properties, such as machinability, mechanical or electrical properties, or
dimensional stability. The annealing process consists of heating the metal to above
or near the critical temperature (the temperature at which crystalline phase change
occurs) and then Soaking it for 1 to 2 hours and letting the material slowly cool to
room temperature in an oven, others are cooled by burying them in ashes, lime, or
other insulating material.

It is a type of heat treatment applicable to ferrous metals only. Heating metal

material 40 to 50 °C above the critical temperature, holding it for about 15 minutes,
and then removing it from the furnace for air cooling slowly the purpose of
normalizing is to remove the internal stresses induced by welding, casting, forging,
forming, or machining. Normalizing is used in some plate mills, in the production
of large forgings such as railroad wheels and axles, and some bar products.

5
 The hardening treatment is for heating the metal to a set temperature above the
critical temperature and then cooling it rapidly (quenching) by plunging it into an
oil, water, brine, or polymer bath. Hardening increases the hardness and strength of
the metal but makes it less ductile and more brittle it becomes. To remove some of
the brittleness, you should temper the steel after hardening.

After the hardening treatment is applied, metal is often harder than needed and is too
brittle. Also, severe internal stresses are set up during the rapid cooling from the
hardening temperature. To relieve the internal stresses and reduce brittleness,
Tempering consists of heating the metal to a specific temperature (below its
hardening temperature), holding it at that temperature for the required length of time,
and then cooling it, usually, instilling air.

 Liquid Quenching

1- Water 2- Brine 3- Oil 4- Caustic Soda

 Dry Quenching

This type of quenching uses materials other than liquids. In most cases, this
method is used only to slow the rate of cooling to prevent warping or cracking.

1. Air 2. Solids: used for cooling include cast iron chips, lime, sand ashe

Study effect of heat treatment on special properties of unalloyed and alloy steels can
be changed

6
Heat treatment is accomplished in three major stages.
Stage 1- Heating the metal slowly to ensure a uniform temperature.
Stage 2- holding the metal at a given temperature for a given time.
Stage 3- Cooling the metal to room temperature.

1- Define Heat Treatment and its advantage and disadvantage.

2- What purposes of annealing?
3- What effects of hardening?
4- Different between Annealing and Normalizing?
5- What purposes of Normalizing?
6- Different between Hardening and Tempering?
7- Different between Annealing and Hardening?
8- What is the reason for using different damping media for heat treatment
processes?

7
Proper preparation of metallographic specimens to determine microstructure and
content requires that a rigid step-by-step process be followed. In sequence, the steps
include sectioning, mounting, course grinding, fine grinding, polishing, etching and
microscopic examination. Specimens must be kept clean and preparation procedure
carefully followed in order to reveal accurate microstructures.

To learn and to gain experience in the preparation of metallographic specimens.

Preparation of metallographic examination is consist of the following steps:

Procedure:
1- Selection of Metallographic Specimens:
Specimens should be chosen from locations most likely to reveal the maximum
variations within the material under study. For example, specimens could be taken
from a casting in the zones where in maximum segregation might be expected to
occur as well as specimens from sections where segregation could be at a minimum.
In the examination of strip or wire, test specimens could be taken from each end of
the coils.
2- Size of Metallographic Specimens:
For convenience, specimens to be grinned and polished for metallographic
examination are generally not more than about 12 to 25 mm (0.5 to 1.0 in.) square,
8
or approximately 12 to 25 mm in diameter if the material is cylindrical. The height
of the specimen should be no greater than generally not more than about 12 to 25
mm (0.5 to 1.0 in.) square, or approximately 12 to 25 mm in diameter if the material
is cylindrical. The height of the specimen should be no greater than
3- Cutting of Metallographic Specimens:
In cutting the metallographic specimen from the main body of the material, care
must be exercised to minimize altering the structure of the metal. Three common
types of sectioning are as follows:

9
4- Cleanliness of Metallographic Specimens:
Cleanliness during specimen preparation is essential. All greases, oils, coolants and
residue from cutoff blades on the specimen should be removed by some suitable
organic solvent.
5- Mounting of Metallographic Specimens
There are many instances where it will be advantageous to mount the specimen prior
for grinding and polishing. Mounting of the specimen is usually performed on small,
fragile, or oddly shaped specimens, fractures, or in instances where the specimen
edges are to be examined. Specimens can be mounted by different ways:

 Mechanical Mounting: The specimens should be tightly bound together to

prevent absorption and subsequent exudation of polishing materials or
etchants as shown in fig4.

10
 Cold Mounting: Where a liquid mixture of two or more polymers solidifies
at room temperature after being poured into a mold containing the specimen
as shown in fig.6

11
6- Grinding of Metallographic Specimens
Grinding removes the damages on the surface produced by sectioning. Grinding
also produced damages which must be minimized so that subsequent grinding with
finer abrasives. Grinding can be done in a number of ways, ranging from rubbing
the specimen on a stationary piece of abrasive paper to the use of automatic devices.
The choice of method depends on the number and type of specimens to be done,
financial considerations and requirements such as flatness and uniformity. Abrasive
paper (covered with silicon carbide grits). Commonly, a series of abrasive paper is
used, from coarse to fine one. The initial grit size depends on the surface roughness
and depth of damage from sectioning. There are several grades of paper, with 180,
240, 400, and 1200, grains of silicon carbide (mosh hardness 9.5) per square inch,
180 grade is the grade to begin the grinding operation.

 Surfaces cut by abrasive cutoff saw start with 120 to 240 grits.
 Surfaces cut by EMD or diamond saw start with 320 to 400 grits.
7- Polishing of Metallographic Specimens:
Polishing is done by manually spinning the sample onto the cloth that has been
charged with a soft abrasive and a suitable liquid as shown in Fig.(7), Diamonds,
suspended aluminum oxide particles (suspended in water), and magnesium oxide
(MgO) are the most commonly used abrasives for polishing. Paper or cloth is affixed
to the surface of a wheel that is rotating at a relatively low speed in a horizontal
plane; the sample is placed against the working surface of the wheel and slowly
rotated in a direction opposite to the direction of the wheel. Polishing cloths should
contain abrasives and should not contain foreign materials grains Coarse - 30 to 3-
micron abrasives. Fine - usually <1 micron , Coarse polishing - 150-600 rpm ~ 6-
micron diamond .Final polishing - 1-micron diamond then 0.3 and 0.05-micron
alumina

12
After a while, a well-polished sample should have a mirror-like surface that is free
from scratches

Automated Methods: many styles of automated specimen preparation

machinery are available as shown in fig.8. Major advantages of automated
grinding and polishing procedures are the consistent quality of specimen
preparation and the substantial decrease in time. Therefore, automated techniques
are recommended over manual techniques. Most of the devices for automated
grinding and polishing move the specimen around a rotating wheel covered with
abrasive so that the specimen follows an epicycloids path.

8- Etching of Metallographic Specimens:

The metallographic etching is one of several processes that take place to develop the
microstructure not normally visible in the as polished condition. during sample
preparation for the metallographic examination, a properly prepared specimen will
reveal properties such as microstructural details, grain size, shape, size, and
distribution of the phases and inclusions that are present, while other aspects such as

13
mechanical deformation and thermal treatments may also be able to be determined.
Proper selection of etchant and etching time is the most important. The
microstructure obtained is decided by etchant and etching time the main etching
processes used in sample preparation are:

Chemical Etching: This typically involves immersing the sample in a chemical

solution

Electrolytic Etching: Uses lower voltages and current densities. Most electrolytic
etching processes use direct current electrolysis. The process uses the specimen as
the anode, with the cathode being a highly insoluble, but conductive material.
Typical examples are platinum, graphite, and stainless steel

Thermal etching: Thermal etching is the process of oxidizing a sample in a furnace.

This induces the oxidation of surface features at different rates, to reveal various
features.

9- After etching process the specimen should be washed with water then with alcohol
to remove any chemical solution may be remind on the specimen surface to avoid
pitting corrosion, then the specimen must be dried with warm air to prepare the
specimen for microscopic examination.

1- What are the solutions used in the process of etching alloys?

2-The difference between the Grinding and Polishing Sample Preparation System?

3- What are the materials used for polishing operations?

4- What are the materials used for grinding operations?

5- What are means the numbers on the grinding papers?

14
The optical microscope is composed of several mechanical and optical parts as:

One of the most important tools used to study living things. “Micro” means very
small “Scope” means to look at .The microscope is an essential tool in the study of
life science. It allows you to see things that are too small to be seen with the unaided
eye. Types of Microscopes

1- The light microscope (compound microscope).

2- The fluorescent microscope.

3- The Electron microscope.

4- The dissecting microscope.

The light microscope: the common light microscope use in the laboratory for
diagnosis and study structures the microscopic organisms, the light microscope is
called a compound microscope because it contains two types of lenses that function
to magnify an object. The lens closest to the eye is called the ocular, while the lens
closest to the object is called the objective.

15
Basic Microscope Parts:

Base: Bottom part of the microscope often shaped like a horseshoe.

Light Source: Located beneath the Stage and Diaphragm. Sends light towards the
hole in the stage.

Diaphragm: Changes the amount of light reaching the objective lenses. Located
under the Stage.

Stage: Place where the object you are looking at is placed (Specimen).

Stage Clips: Holds down the slide on the stage.

Arm: Supports the body tube. Used to carry the microscope.

Eyepiece: The lens you look through that magnifies the specimen.

Body Tube: The hollow tube through which light passes. It holds the lenses apart.

Course Focus: Raises or lowers the Body Tube to focus

Fine Focus: Raises and lowers the Body Tube and used to bring objects into focus.
The nosepiece is: the round part that holds the objective lenses apart.

Low Power Objective: Magnifies the specimen at a lower power

High Power Objective: magnifies the specimen at a higher power the nosepiece
hold the objective lenses apart. The microscope has several objective lenses. Each
lens has a different magnification power.

It is used for the study of detailed gross internal structure.

16
 Using the Microscope in 10 Steps

1. To carry the microscope, grasp the arm with one hand. Hold the Base with your
other hand.

2. Adjust the diaphragm while looking through the eyepiece

4. Place the slide on the stage.

5. Center the specimen over the small opening on the stage.

6. Secure the slide with the stage clips.

7. While looking at the stage from the side, turn the course focus knob to lower the
body tube until the low power objective almost touches the slide.

8. While looking through the eyepiece, carefully move the course focus knob until
the specimen comes into view.

9. To switch to the high power objective lens, look at the microscope from the side.

10. Move the nosepiece until the high power objective lens “clicks” into place. If
the lens hits the slide, the slide and/or lens might break. Turn the fine focus knob
until the specimen comes into focus.

1- What are the advantage and disadvantage of optical microscope?

17
Differential scanning calorimetry (DSC):
Calorimetry - The study of heat transfer during physical and chemical process.
Calorimeter - A device for measuring the heat transferred.

• Differential scanning calorimetry (DSC): is a technique for measuring the energy

necessary to establish a nearly zero temperature difference between a substance and
an inert reference material, as the two specimens are subjected to identical
temperature regimes in an environment heated or cooled at a controlled rate.

DSC curves:

DSC experiment is a curve of heat flux versus temperature or versus time. There are
two different conventions: exothermic reactions in the sample shown with a positive
or negative peak, depending on the kind of technology used in the experiment. This
curve can be used to calculate enthalpies of transitions. This is done by integrating
the peak corresponding to a given transition. It can be shown that the enthalpy of
transition can be expressed using the following equation:

18
This technique is used to study what happens to polymers/samples upon heating. It
is used to study thermal transitions of a polymer/sample (the changes that take place
on heating) – For example:

• The melting of a crystalline polymer

• The glass transition

• The crystallization

• The sample and reference are maintained at the same temperature, even during a
thermal event in the sample

• The energy required to maintain zero temperature difference between the sample
and the reference is measured

• During a thermal event in the sample, the system will transfer heat to or from the
sample pan to maintain the same temperature in reference and sample pans

19
1- What can DSC measures?
2- Why heaters don’t heat at the same rate?
3- What are Factors affecting DSC curve?

20
Fourier Transform Infrared (FTIR) spectroscopy is the preferred method
of infrared spectroscopy. IR radiation is transmitted through a sample in infrared
spectroscopy. The sample absorbs some of the infrared energy, and some of it is
transferred (passed through). The resulting spectrum gives the sample a molecular
fingerprint by displaying the molecule’s absorption and transmission. No two unique
molecule configurations produce the same infrared spectrum, just like fingerprints.
As a result, infrared spectroscopy is useful for a variety of analyses. FTIR (Fourier
Transform Infrared Spectrometer) spectrometers are commonly used in organic
synthesis, polymer science, petrochemical engineering, the pharmaceutical sector,
and food analysis. Furthermore, as FTIR spectrometers can be hyphenated to
chromatography, they can be used to explore the mechanism of chemical reactions
and the detection of unstable compounds.

21
This analytical test method, sometimes referred to as FTIR analysis or FTIR
spectroscopy, is used to distinguish between organic, polymeric, and, occasionally,
inorganic materials. Infrared light is used in the product composition analysis
procedure employing FTIR technology to scan test samples and track chemical
characteristics.

There are several ways to use an FTIR. You can sample liquids, solids in solution,
and pellets. The samples are typically held between KBr or NaCl [Link]
Michelson interferometer consists of a beam splitter, a moving mirror, and a
stationary mirror. The beam splitter divides the light beam into two halves, which
are reflected by the moving and fixed mirrors before being recombined by the beam
splitter. As the moving mirror makes reciprocating movements, the optical path
difference to the fixed mirror changes, causing the phase difference to shift over
time. Interference light is created in the Michelson interferometer by recombining
the light beams. An interferogram records the intensity of the interference light, with
the optical path difference recorded along the horizontal axis. Samples as small as
10 microns can be evaluated using FTIR analysis. The tiny sample size allows for
cost effective identification of particles, residues, films or fibers. FTIR analysis can
also measure levels of oxidation or degrees of cure in some polymers as well as
measuring the level of contaminants or additives

22
1- What are Advantages and Limitations of FTIR?
2- What are Applications of FTIR?
3- Why used KBr or NaCl plates in sample preparation?
4- What is the difference between IR and FTIR?

23
Wear test is carried out to predict the wear performance and to investigate the wear
mechanism. Wear is a process of removal of material from one or both of two solid
surfaces in solid state contact. As the wear is a surface removal phenomenon and
occurs mostly at outer surfaces, it is more appropriate and economical to make
surface modification of existing alloys than using the wear resistant alloys.

 Type of wear

1- Adhesion Wear 2- Abrasion Wear 3- Erosion Wear 4- Fatigue Wear

 Laboratory wear testing method
1- An abrasive wear tester 2- A rolling sliding wear tester 3- A pin-on-disc wear
tester
In this experiment, the test was conducted with the following parameters:

1. Load 2. Speed 3. Distance In the present experiment the parameters such as speed,
time and load are kept constant throughout for all the experiments

PIN-ON-DISC TEST: In a pin-on-disc wear tester, a pin is loaded against a flat

rotating disc specimen such that a circular wear path is described by the machine.
The machine can be used to evaluate wear and friction properties of materials under
pure sliding conditions. Either disc or pin can serve as specimen, while the other as
counterpace. Pin with various geometry can be used. A convenient way is to use ball
of commercially available materials such as bearing steel, tungsten carbide or
alumina (Al2O3) as counterface, so that the name of ball-on-disc is used.

24
Fig. 1: Schematic of a pin-on-disc wear test and the arrangement of samples.

Wear rate:

Wear rates are calculated results reflecting wear mass loss, volume loss or linear
dimension change under unit applied normal force and/or unit sliding distance. Wear
rate can be expressed in many different ways.

Wear resistance: is a term frequently used to describe the anti-wear properties of

a material. However, the scientific meaning of wear resistance is vague, and there is
no specific unit to describe wear resistance. Nevertheless, the inverse of mass loss
or volume loss is sometimes used as the (relative) wear resistance. The ratio of wear
loss for a reference material over that of the investigated material under same testing
conditions can also used as relative wear resistance. In any case, if a numeric value
of wear resistance is given, its meaning should be clearly indicated.

25
1. Cut the sample by size (10 x 20) cm.
2. Weigh the sample before wearing wear with a digital balance.
3. Clean the steel disk with acetone to free it from any debris from the earlier
usage.
4. Remove the existing loads if any on the machine.
5. Fix the specimen in the pin holder using align key.
6. Note down the track radius.
7. Apply a load of 1Kg in the Pan.

26
8. Switch on the power of the control unit and set the timer to 5minutes.
9. Set the wear and frictional force to zero.
10. Start the wear testing machine and set RPM to 500.
11. Weight the first sample after wearing with a digital balance.
12. Note down the readings of wear and frictional force at the end of 5 minutes.
13. Repeat the experiment with 2Kg, 3Kg and 4kgs.
14. Tabulate the results and calculate the co-efficient of friction.
15. Draw a graph of Wear (μm) Vs Load (N).

• Discuses and compare the results, graphs to compare test parameters of different
Parameters?
• What are the main wear characteristics of the given specimen?
• Give your understanding about each effect of experimental parameters?
• What are the types of wear and explained briefly?
• What is the benefit of testing on the human body and what are the most places
where there is wear can be happen?

27