UNIVERSITY OF RAJSHAHI

Group Work on Microstructure Laboratory

Submitted by Group Three

Group Member Name:
• Sudad Bin Azim (2310478119)
• Sazzad Hossain Parvez (2311178121)
• Sayed Ahmmed Shanto (2311078122)
• Iftekarul Islam Mahim (2310178125)
• Sukhomoy Das (2310478126)

Department: Materials Science & Engineering

1. What is Microstructure?

Ans: Microstructure refers to the small-scale structure of a material, typically observed at

magnifications higher than what the naked eye can see (using microscopes). It includes the
arrangement of grains, phases, defects, and other features that influence a material's
properties, such as strength, ductility, hardness, and corrosion resistance.

Figure 1: Microstructure

Components of Microstructure:

1. Grains & Grain Boundaries

• Grains are crystals of the material, and their size (fine or coarse) affects mechanical
properties.
• Grain boundaries are the interfaces between grains, influencing strength and
diffusion.
2. Phases

• Different phases (e.g., ferrite, austenite in steel) can coexist, affecting behavior (e.g.,
hardness, toughness).
3. Defects

• Includes dislocations, voids, and inclusions that impact material performance.

4. Precipitates & Secondary Phases

• Small particles (e.g., carbides in steel) that strengthen the material (precipitation
hardening).
2. Why Need to Study the Microstructure of a sample?
Ans: Studying microstructure is essential because it directly determines a
material's properties, performance, and suitability for specific applications. Here’s why it
matters:

1. To Understand Material Properties (Microstructure influences)

• Mechanical Properties: Strength, hardness, ductility, and toughness.

o Example: Fine-grained metals are stronger than coarse-grained ones (Hall-
Petch effect).
• Thermal Properties: Heat resistance, conductivity, and expansion.
• Electrical/Magnetic Behavior: Grain boundaries and phases affect conductivity (e.g.,
silicon in semiconductors).
• Corrosion Resistance: Phase distribution can make materials prone to or resistant to
rust (e.g., stainless steel vs. carbon steel).
2. Quality Control & Failure Analysis

• Detect Defects: Voids, cracks, or inclusions that weaken materials.

• Root Cause of Failures: Analyze broken components (e.g., fatigue cracks in aircraft
parts).
• Verify Manufacturing Processes: Ensure heat treatment, welding, or casting produced
the desired structure.
3. Optimize Manufacturing Processes

• Heat Treatment: Adjust cooling rates to create specific phases (e.g., quenching steel
to form martensite for hardness).
• Alloy Development: Design new materials (e.g., high-strength aluminum alloys for
aerospace).
• Additive Manufacturing: Control laser settings to avoid porosity or weak grain
structures.
4. Predict Performance in Service

• Creep Resistance: High-temperature applications (e.g., turbine blades) rely on stable

microstructures.
• Wear Resistance: Hard carbides in tool steels extend lifespan.
• Environmental Durability: Coatings or grain structures can prevent degradation in
harsh conditions.
5. Research & Innovation

• Nanomaterials: Study grain boundaries at atomic scales for breakthroughs.

• Composite Materials: Optimize fiber-matrix interfaces for strength.
• Biomaterials: Ensure biocompatibility (e.g., titanium implants with controlled
porosity).
6. Key Techniques for Microstructure Analysis

• Optical Microscopy: Quick grain size/shape assessment.

• SEM/TEM: High-resolution imaging and composition analysis.
• XRD/EBSD: Crystal structure and orientation mapping.
7. Real-World Example

• Automotive Steel: A dual-phase microstructure (martensite + ferrite) balances

strength and formability for crash safety.
• Electronics: Silicon wafer microstructure affects chip performance.

In short, microstructure is the link between how a material is made, how it behaves, and how
it can be improved. Whether for failure investigation, material design, or process optimization,
studying microstructure is fundamental to engineering and science.

3. What is microscope? How does it work?

Ans: A microscope is a scientific instrument used to magnify and resolve small objects or
details that are invisible to the naked eye. It enables the observation of structures at
microscopic (µm) or even nanoscopic (nm) scales, essential in fields like biology, materials
science, medicine, and nanotechnology.

Types of Microscopes

1. Optical Microscope (Light Microscope)

• Uses visible light and lenses.

• Max magnification: ~1,500x.
• Examples: Brightfield, Darkfield,
Phase-Contrast.
• Uses electron beams for higher
resolution.
• SEM (Scanning Electron Microscope):
Scans surfaces; 3D-like images.
Figure 2: Optical Microscope
 • TEM (Transmission Electron Microscope): Passes electrons through thin samples;
atomic-scale details.
2. Scanning Probe Microscope (e.g., AFM)

• Maps surfaces at atomic resolution using a physical probe.

The working principle of a microscope is given below in details and elaborately:

1. Optical Microscope (Basic Principle)

• Illumination: Light (from a lamp or LED) passes through a condenser to focus on the
sample.
• Magnification: Light interacts with the sample, and lenses (objective + eyepiece)
enlarge the image.
• Resolution: Limited by light wavelength (~200 nm). Staining or phase contrast
enhances visibility.
2. Electron Microscope (SEM/TEM)

• Electron Beam: Electrons (instead of light) are emitted from a tungsten filament or
field-emission gun.
• Lenses: Electromagnetic lenses focus the beam.
• Detection:
o SEM: Electrons scatter off the sample’s surface;
detectors create a 3D image.
o TEM: Electrons pass through ultrathin samples;
interference patterns reveal atomic structures.
• Resolution: ~0.1 nm (TEM) to ~1 nm (SEM), far exceeding
optical microscopes. Figure 3: Electron Microscope

3. Advanced Techniques

• Fluorescence Microscopy: Uses fluorescent dyes to tag specific structures (e.g., cell
organelles).
• Confocal Microscopy: Laser scans samples layer-by-layer for 3D reconstruction.
Key Components

• Objective Lens: Primary magnifier (4x to 100x in optical microscopes).

• Stage: Holds the sample.
• Diaphragm: Controls light intensity.
• Detector/Camera: Captures images (e.g., CCD in SEM).
4. What is dark field and bright field microscopy? Explain in detail.
Ans: (A) Bright Field Microscopy
Definition: Bright field microscopy is an optical imaging technique where the specimen is
illuminated with direct light, and contrast is generated due to differences in light absorption
or reflection.
Working Principle:
1. Illumination: A light source (usually a halogen lamp)
passes through a condenser, focusing light onto the
sample.
2. Light Interaction:
o In transmitted light mode, dense regions
(e.g., grain boundaries, precipitates) absorb
or scatter light, appearing dark.
o In reflected light mode, polished surfaces
reflect light, while rough or etched regions
appear darker.
3. Image Formation: The objective lens collects the transmitted/reflected light, forming
an image where structural details contrast against a bright background.
Applications:
• Metallography (grain structure analysis)
• Biological samples (stained tissues, cells)
• Quality control in material science
Advantages:
• Simple setup and widely used.
• Good for observing stained or etched samples.
Limitations:
• Low contrast for transparent/unstained specimens.
• Requires sample preparation (etching, polishing).
(B) Dark Field Microscopy
Definition: Dark field microscopy uses oblique
illumination so that only scattered light from the
specimen enters the objective, producing bright
features against a dark background.
Working Principle:
1. Illumination: A hollow cone of light is
directed at the sample at an oblique angle.
2. Light Scattering: Figure 4: Dark Field Microscopy

o Flat, smooth surfaces reflect light away

from the objective → appear dark.
o Irregularities (e.g., nanoparticles, cracks) scatter light into the objective →
appear bright.
3. Image Formation: Only scattered light contributes to the image, enhancing contrast
for fine details.
Applications:
• Observing nanoparticles and colloids.
• Detecting surface defects (scratches, cracks).
• Studying live, unstained biological specimens (e.g., bacteria, cells).
Advantages:
• High contrast for transparent/reflective samples.
• No staining required.
• Can reveal sub-wavelength features.
Limitations:
• Lower resolution compared to bright field.
• Requires precise optical alignment.

5. (i) What is transmitted light? (ii) What is reflected light?

Ans: Transmitted light
Definition: Transmitted light refers to illumination that passes through a specimen before
being collected by the objective lens to form an image.
Working Principle:
1. Light Path: The light source (typically
below the sample) emits rays that
travel through:
o Condenser (focuses light onto
the sample)
o Specimen (partially
absorbs/scatters light)
o Objective lens (collects
transmitted light) Figure 5: transmitted light & reflected light
o Eyepiece/camera (forms the
final image)
2. Contrast Mechanism:
o Thicker/denser regions absorb more light → appear darker
o Thinner/transparent regions transmit more light → appear brighter
Requirements:
• Samples must be thin enough to allow light transmission (e.g., biological sections, thin
metal foils).
• Often requires staining/etching to enhance contrast.
Applications:
• Biology (viewing stained tissue sections)
• Polarized light microscopy (mineralogy)
• TEM (Transmission Electron Microscopy)
Advantages:
• Reveals internal structures.
• Compatible with various contrast techniques (phase contrast, DIC).
Limitations:
• Unsuitable for opaque materials.
• Requires sample thinning (may alter natural state).
Reflected Light
Definition:
Reflected light (epi-illumination) uses light bounced off a specimen's surface to form an
image.

Figure 6: Properties of light

Working Principle:
1. Light Path:
o Light source (usually coaxial with the objective) directs light downward.
o Beam splitter reflects light onto the sample.
o Surface reflections are captured by the same objective.
2. Contrast Mechanism:
o Smooth/flat surfaces reflect light directly → appear bright
o Rough/etched areas scatter light → appear dark
Requirements:
• Samples must be opaque or highly reflective (e.g., metals, ceramics, integrated
circuits).
• Often requires polishing to minimize diffuse scattering.
Applications:
• Metallography (grain structure analysis)
• Semiconductor inspection
• Forensic analysis (surface defects)
Advantages:
• No sample thinning needed.
• Ideal for studying surface topography.
Limitations:
• Limited to surface features (no internal details).
• Glare from highly reflective surfaces may obscure details.

6. What is Numerical Aperture? How does it work?

Ans: Numerical Aperture (NA) is a dimensionless number that describes the ability of a
microscope objective lens to gather light and resolve fine details of the specimen at a fixed
object distance.

It is given by the formula:

NA=[Link](θ)

Where:

• n = refractive index of the medium between the specimen and the objective lens (e.g.,
air = 1.0, oil = 1.5).
• θ = half-angle of the maximum cone of light that can enter the lens.

How Numerical Aperture Works in a Microscope: Numerical Aperture (NA) determines how
much light the objective lens can collect from the sample and how finely it can resolve details.

NA controls how much light a lens gathers → more light = better image.
NA controls how small a feature it can resolve → higher NA = finer detail.
NA depends on the lens design and the medium between the lens and specimen
Step-by-Step Working Process:

▪ Light Illumination:

o Light shines on the sample (from below in transmitted light or above in

reflected light).

o The sample reflects, transmits, or scatters the light in all directions.

▪ Light Collection by Lens:

o The objective lens collects some of this light.

o The amount and angle of collected light depends on the lens design.

o A high-NA lens can collect light rays coming from wider angles (larger cone).

▪ Image Formation:

o The more light collected (i.e., higher NA), the brighter and more detailed the
image.

o It also improves resolution, which means the lens can distinguish two closely
spaced points.

▪ Refractive Index Effect:

o Using a medium with higher refractive index (like immersion oil) increases NA.

o For example, oil has n≈1.5n ≈ 1.5n≈1.5, which allows more oblique rays to enter
the lens, thus enhancing resolution.

7. What is illumination beam?

Ans: An illuminating beam is the beam of light that strikes the

sample to make it visible under the microscope. It provides the
necessary contrast and illumination for image formation.

How the Illuminating Beam Works in Optical Microscopy:

• Light is emitted from the light source.

• It is focused using condenser lenses onto the specimen.
• Light interacts with the specimen:
• Some parts absorb, reflect, or scatter light.
Figure 7: illumination beam
• The light that emerges (either transmitted or reflected)
enters the objective lens.
• An image is formed and magnified.

9. What is pit?
Ans: A pit is a small surface cavity or defect visible in microstructure analysis, often resulting
from corrosion, etching, or poor sample preparation. It can affect material performance and
is important in failure analysis.

Figure 8: pit

10. What are imperfections?

Ans: Imperfections are atomic-scale or structural irregularities in materials that influence

strength, ductility, conductivity, corrosion resistance, and many other properties. They can be
point, line, surface, or volume defects. Imperfections in materials are defects in the atomic
arrangement that naturally occur during solidification, processing, or due to thermal
vibrations. These imperfections significantly influence a material's strength, conductivity, and
overall performance.

Figure 9:imperfections
11. What is grinding? Why did you do that?

Ans: Grinding is a precision machining process where abrasive wheels or belts are used to
remove material from a workpiece. It is typically employed for achieving tight tolerances,
superior surface finishes, and unique shapes. The grinding process generates friction between
the abrasive surface and the material being worked on, breaking down particles to create the
desired surface texture. Grinding is used in a variety of industries, including automotive,
aerospace, and medical equipment manufacturing.

Figure 10: Grinding

Prepose of Grinding: Grinding is used in microstructure study primarily as a preparatory step

to produce a smooth, flat, and defect-free surface on a metallurgical or material sample before
microscopic examination. This is crucial because:

• Grinding removes surface irregularities and roughness from the sample, providing a
flat surface that allows clear and accurate observation of the microstructure under
optical or electron microscopes.

• It helps to avoid artifacts caused by cutting or mechanical damage, ensuring that the
microstructural features such as grains, phases, and defects are not obscured or
distorted.

• Proper grinding reduces the thickness of any damaged surface layer, which is
necessary before polishing and etching to reveal the true microstructure.
 • It enables precise quantitative analysis of grain size, phase distribution, and defects by
producing a surface suitable for high-resolution imaging and image analysis techniques
like planimetry or linear intercept methods.

• Grinding also helps in studying the effects of processes like grinding itself on
microstructure, such as the formation of metamorphic layers or phase transformations
induced by grinding heat and stress.

12. What is polishing? Why did you do that?

Ans: Polishing is a mechanical surface-finishing process that uses fine abrasives and soft
cloths to produce a smooth, mirror-like surface on a specimen. In microstructure preparation,
it is the final step before etching, aimed at removing scratches and deformation left by
grinding to reveal the true microstructure under a microscope.

Stages of Polishing are given below:

Stage Abrasive Type Particle Size Purpose

Rough Polishing Diamond paste ~6 µm Removes deep grinding scratches

Intermediate Alumina/Silica ~1–3 µm Smoothens surface further

Final Polishing Colloidal silica ~0.05 µm Achieves mirror finish

Prepose of polishing: There are several regions for which we polish the sample before putting
it into the microscopic observation. The reasons are followed:

• Improved Image Clarity: A polished surface

minimizes light scattering and distortion,
resulting in sharper, more accurate images of
the microstructure.
• Reduced Artifacts: Polishing removes surface
imperfections and deformations that can
obscure or misrepresent the true
microstructure.
• Enhanced Contrast: A smooth surface allows
for better differentiation between different
microstructural features, making them easier
Figure 11: polishing
to distinguish.
• Accurate Microstructure Analysis: Clearer images are vital for accurate analysis of
grain size, phase distribution, and other microstructural characteristics.
 • Enables Microscopy: Polishing is a prerequisite for many microscopic techniques, such
as optical microscopy and electron microscopy, where a smooth, reflective surface is
necessary for proper imaging.

13. What is etching? Why did you do that?

Ans: Etching Is a chemical or electrolytic process used after metallographic grinding and
polishing procedures. It enhances the contrast on surfaces in order to visualize the
microstructure or macrostructure. Etching in metallography exerts a controlled influence on
the surface profile or optical properties at grain boundaries, phases, or grain surfaces, thus
enabling microscopic inspection and additional use of optical filters in the microscope.
Preparation before the etching process must be adapted to the investigation target.

Common Etchants & Materials

Material Type Common Etchant Composition Example

Steels Nital 2–5% nitric acid in ethanol

Stainless Steel Vilella’s reagent Picric acid + HCl + ethanol

Aluminum Alloys Keller’s reagent HF + HCl + HNO₃ + water

Copper Alloys Ferric chloride sol. FeCl₃ + HCl + water

Prepose of etching: There are some crucial purposes of etching. They are mentioned and
described and given bellow:

• To reveal grain boundaries and phases: Etching makes the crystalline structure visible
by preferentially attacking grain boundaries or
different phases, enabling identification of grain
size, shape, and distribution.
• To improve optical contrast: It enhances the
contrast on the polished surface so that
microstructural features can be clearly observed
with optical or electron microscopes.
• To differentiate phases and constituents:
Different phases (e.g., ferrite, pearlite,
martensite) or inclusions respond differently to
etchants, allowing their identification and study. Figure 12: Etching
 • To detect defects and discontinuities: Etching can expose cracks, segregation zones,
and heat-affected areas important for failure analysis and quality control.
• To support quantitative analysis: Revealed microstructures enable measurement of
grain size, phase fractions, and morphology critical for understanding material
properties.

14. What is grain and grain Size?

Ans: Grain refers to an individual crystalline region within a polycrystalline metal, such as
steel. Each grain is a single crystal with atoms arranged in a specific, repeating lattice structure
(For example: body-centered cubic or face-centered cubic), but the orientation of the crystal
lattice differs from grain to grain. Grains are separated by grain boundaries, which are
interfaces where the crystal orientation changes. The grain structure forms as the metal
solidifies from the molten state and is influenced by processing methods like casting, forging,
and heat treatment.

Figure 13: Grain

Figure 14: Grain size

Grain size is the measure of the dimensions of these individual grains within the metal. It can
be described by the average diameter or by the number of grains per unit area or volume.
Grain size is a critical factor because it strongly influences the metal’s mechanical properties.
Smaller grains typically increase strength and toughness (due to grain boundary
strengthening), while larger grains can enhance ductility. Grain size can be controlled by
processing parameters such as cooling rate, heat treatment, and deformation.

15. What is single crystal?

Ans: Single crystals are materials in which the entire

sample has a continuous and unbroken crystal lattice to
the edges of the sample with no grain boundaries. The
lack of defects associated with grain boundaries can
impart unique properties to single crystals, particularly
mechanical, optical and electrical properties, which can
also be anisotropic, depending on the type of crystal
structure. In addition to making them valuable in
certain gems, these properties are also used industrially
for technical applications, particularly in the fields of
optics and electronics. Figure 15: Crystalline

16. What is polycrystalline?

Ans: A polycrystalline material is a solid composed of many small crystals or grains, each with
its own orientation. These grains are tightly packed together, and the boundaries between
them are called grain boundaries.

When a material solidifies from the molten state, it usually doesn't form one large crystal.
Instead, nucleation occurs at multiple points, and small
crystals begin to grow. As they expand, they eventually
meet and fuse, forming a polycrystalline structure.

Each grain within the material is a single crystal, but the

overall solid lacks long-range order across the entire
sample because the grains are randomly oriented. This
is what distinguishes polycrystalline materials from
single crystals (which have a continuous lattice
throughout) and amorphous solids (which lack any
long-range order). Figure 16: Polycrystalline
17. Write down the Seven Crystal Systems?

Ans: The seven crystal systems are the fundamental ways in which atoms are arranged in
three-dimensional space within a crystalline solid. Each system is defined by the relative
lengths of its unit cell edges (a, b, c) and the angles (α, β, γ) between them. These systems
form the backbone of crystallography and help classify all known crystal structures.

Here’s a quick summary of what each system represents:

Crystal Axes
Angles Figure
System Relationship

Cubic a=b=c α = β = γ = 90°

Tetragonal a=b≠c α = β = γ = 90°

Orthorhombic a≠b≠c α = β = γ = 90°

Hexagonal a=b≠c α = β = 90°, γ = 120°

 Trigonal a=b=c α = β = γ ≠ 90°

Monoclinic a≠b≠c α = γ = 90°, β ≠ 90°

Triclinic a≠b≠c α ≠ β ≠ γ ≠ 90°

18. What is crystal defect?

Ans: A crystal defect is an imperfection or irregularity in the regular arrangement of atoms in

a crystalline solid. In an ideal crystal, atoms are arranged in a perfectly ordered, repeating
pattern. However, in real materials, various types of defects disrupt this perfect structure.

Types of Crystal Defects:

1. Point Defects: point defect refers defects at or around a single lattice point:

• Vacancy: A missing atom from a lattice

site.
• Interstitial: An extra atom placed in the
spaces between regular atoms.
• Substitutional: A foreign atom replaces a
host atom in the lattice.
• Frenkel Defect: An atom moves from its
normal site to an interstitial site, creating a Figure 17: Crystal defects
vacancy and interstitial pair.
• Schottky Defect: Equal numbers of cations and anions are missing, maintaining charge
neutrality.
2. Line Defects (Dislocations): It refers defects involving rows of atoms:

• Edge Dislocation: An extra half-plane of atoms is inserted.

• Screw Dislocation: The crystal layers spiral around a central line.

3. Surface Defects: Refers irregularities at the crystal surface:

• Grain boundaries
• Twin boundaries
• Stacking faults

4. Volume Defects: larger imperfections such as:

• Voids (empty spaces)

• Inclusions (trapped foreign particles)

Importance of Crystal Defects:

• Mechanical properties: Defects can strengthen or weaken materials (e.g., dislocations

enable plastic deformation).

• Electrical properties: Defects affect conductivity in semiconductors.

• Diffusion: Vacancies allow atoms to move through the crystal.

19. What are FCC and BCC crystal system?

Ans: FCC (Face Centred Cubic) and BCC (Body-Centred

Cubic) are two common types of cubic crystal structures,
found in many metals and alloys. They describe how atoms
are arranged in the unit cell of the crystal.

1. FCC (Face-Centred Cubic)

Structure:

• Atoms are located at:

o 8 corners of the cube Figure 18: FCC Crystal System

o 1 atom at the centre of each face (6 faces)

Number of atoms per unit cell:

• Each corner atom is shared by 8-unit cells.

• Each face atom is shared by 2-unit cells.

• Total:4 atoms
Properties:

• High packing density: ~74%

• Ductile and strong

• Slip systems: 12 (easier plastic deformation)

Examples:

• Aluminium (Al)

• Copper (Cu)

• Gold (Au)

• Nickel (Ni)

• Silver (Ag)

2. BCC (Body-Centred Cubic)

Structure:

• Atoms are located at:

o 8 corners of the cube

o 1 atom at the centre of the cube

Number of atoms per unit cell:

• Total: 2 atoms Figure 19: BCC Crystal System

Properties:

• Lower packing density: ~68%

• Harder and less ductile

• Slip systems: 48 (but fewer close-packed directions, so less ductile)

Examples:

• Iron (Fe, at room temperature)

• Chromium (Cr)

• Tungsten (W)

• Molybdenum (Mo)
20. What are the lattice angle and lattice parameter?

Ans: Lattice angle and lattice parameter are terms used in crystallography to describe the
geometry of a crystal lattice—the repeating 3D arrangement of atoms in a crystal. Here's what
they mean:

1. Lattice Parameter (or Lattice Constant):

These are the distances between the unit cell

edges. In a 3D crystal structure, the unit cell is
defined by three edge lengths:

a, b, and c: These are the lattice parameters

(usually in nanometres or angstroms, Å).

They represent the length of the unit cell along

the x, y, and z axes.

Figure 20: Lattice Parameter

2. Lattice Angle:

These are the angles between the edges of

the unit cell:

α (alpha): Angle between b and c

β (beta): Angle between a and c

γ (gamma): Angle between a and b

Example: Figure 21: Lattice Angle

For a cubic crystal system (like in simple cubic, BCC, FCC):

a=b=c

α = β = γ = 90°

For a hexagonal crystal system:

a=b≠c

α = β = 90°, γ = 120°