Nondestructive Testing

Nondestructive Testing is a wide group of analysis techniques used in science and technology
industry to evaluate the properties of material, component or systems without causing damage or
breaking.
The terms:
Non-destructive Examination (NDE)
Non-destructive Inspection (NDI)
Non-destructive Evaluation (NDE)
are also commonly used to describe this technology.
BASIC ELEMENTS OF NDT METHOD
• SOURCE
• MODIFICATION
• DETECTION
• INDICATION
• INTERPRETATION

ADVANTAGES OF NDT
• The equipments are easy to handle
• Defects can be detected without damaging the components
• Methods are quick and accurate
• Components can be sorted out on the basis of electrical, magnetic or chemical properties
• Test results and other information can be conveniently recorded on paper films, cassettes
and floppies
• It increases the safety and reliability of the product during operation

DIFFERENCE BETWEEN DESTRUCTIVE AND NON DESTRUCTIVE TEST

NON DESTRUCTIVE TEST DESTRUCTIVE TEST
Used for finding out defects of materials Used for finding out the properties of the
material
Load is not applied on the material Load is applied on the material

No load applications, so no chance for material Due to load application, material gets damaged
damage
No requirement of special equipments Special equipments are required

Non expensive Expensive

Less skill Skill is required
e.g: dye penetrate test, ultrasonic, radiography, e.g: tensile test, compression test, hardness test,
etc etc
METHODS OF NDT
• Visual Inspection (VI)
• Liquid Penetrant Testing LPT)
• Magnetic Particle Testing (MPT)
• Ultrasonic Testing (UT)
• Eddy Current Testing (ECT)
• Radiography Testing (RT)

Visual Inspection
• VI is one of the most common and most powerful means of NDT. Visual
testing requires adequate illumination of the test surface and proper
eye-sight of the tester.
• Visual testing can be classified as direct visual testing, remote visual
testing.
• Often the equipment needed is portable light, mirror on stem,
illuminated magnifier etc.

 For internal inspection, light lens systems such as borescopes allow

remote surfaces to be examined. More sophisticated devices of this
nature using fibre optics permit the introduction of the device into very
small access holes and channels. Most of these systems provide for the
attachment of a camera to permit permanent recording.
 Portable video inspection unit with zoom allows inspection of large tanks
and vessels, railroad tank cars, sewer lines.
 Robotic crawlers permit observation in hazardous or tight areas, such as
air ducts, reactors, pipelines.
 Liquid Penetrant Testing
PT can be employed for the detection of open-to-surface discontinuities in any industrial product
which is made from a non-porous material.
Almost any material that has a relatively smooth, non-porous surface on which discontinuities or
defects are open to the surface.

A liquid with high surface

wetting characteristics is
applied to the surface of
the part and allowed
time to seep into surface
breaking defects.
• The excess liquid is
removed from the surface
of the part.
• A developer (powder) is
applied to pull the trapped
penetrant out the defect
and spread it on the
surface where it can be
seen.
• Visual inspection is the
final step in the process.
The penetrant used is
often loaded with a
fluorescent dye and the
inspection is done under
UV light to increase test
sensitivity.
Advantages :
(1) Relatively low cost.
(2) Highly portable NDT method.
(3) Highly sensitive to fine, tight discontinuities.
(4) Fairly simple method.
(5) Can be used on a variety of materials.
(6) All open to surface discontinuities are detected in one operation, regardless of orientation.
Limitations :
(1) Test surface must be free of all contaminants (dirt, oil, grease, paint, rust, etc.).
(2) Detects surface discontinuities only.
(3) Cannot be used on porous specimens and is difficult to use on very rough surfaces.
(4) Removal of all penetrant materials, following the test, is often required.
(5) There is no easy method to produce permanent record.
 Magnetic Particle Testing

MT is used for the testing of materials which can be easily magnetized. This method is capable of
detecting open to surface and just below the surface flaws.
The test specimen is magnetized with a
strong magnetic field created by a
magnet or special equipment. Finely
milled iron particles coated with a dye
pigment are then applied to the
specimen. These particles are attracted
to magnetic flux leakage fields and will
cluster to form an indication directly
over the discontinuity. This indication
can be visually detected under proper
lighting conditions.

Advantages :
(1) It does not need very stringent pre-cleaning operation.
(2) Best method for the detection of fine, shallow surface cracks in ferromagnetic material.
(3) Fast and relatively simple NDT method.
(4) Generally inexpensive.
(5) Will work through thin coating.
(6) Few limitations regarding the size/shape of test specimens.
(7) Highly portable NDT method.
(8) It is quicker
Limitations :
(1) Material must be ferromagnetic.
(2) Orientation and strength of magnetic field is critical.
(3) Detects surface and near-to-surface discontinuities only.
(4) Large currents sometimes required.
(5) “Burning” of test parts a possibility.
(6) Parts must often be demagnetized, which may be difficult

EDDY CURRENT TESTING(ECT)

 The main applications of the eddy current technique are for the detection of surface or
subsurface flaws, conductivity measurement and coating thickness measurement.
 Eddy current testing use the principal of “electromagnetism” as the basis for conducting
examinations and applicable to electrically conductive materials only.
 APPLICATION OF ECT
• Crack Detection
• Corrosion Monitoring
• Material Thickness Measurements
• Coating Thickness Measurements
• Conductivity Measurements
A coil carrying high frequency
alternating current induces eddy
current in the test specimen. Eddy
currents flowing in the material
generates their own “secondary”
magnetic field which opposes the
coil’s “primary” magnetic field.
Information about the strength of
the eddy current within the
specimen is determined by
monitoring changes in voltage
and/or current that occurs in the
coil.

ADVANTAGES OF ECT
(1) Sensitive to small cracks and other defects
(2) Detect surface and near surface defects
(3) Inspection gives immediate results
(4) Equipment is very portable
(5) Method can be used for much more than flaw detection
(6) Inspects complex shapes and sizes of conductive materials
Limitations:
(1) Require good theoretical knowledge
(2) Extremely sensitive to surface variations and therefore requires a good surface.
(3) It is applicable to conductor materials only.
(4) Can be used on non-magnetic and magnetic material but is not reliable on carbon steel for
the detection of subsurface flaws.
(5) Its depth of penetration is limited.
(6) Crack tightness and orientation of eddy current flow to a crack or linear discontinuity will
affect detectability.

Ultrasonic Testing
 Ultrasonic testing uses high frequency sound energy to conduct examinations and make
measurements.
 Ultrasonic examinations can be conducted on a wide variety of material forms including
castings, forgings, welds, and composites.
A considerable amount of information about the part being examined can be collected, such
as the presence of discontinuities, part or coating thickness; and acoustical properties can
often be correlated to certain properties of the material.
•A typical UT system consists of
several functional units, such as the
pulser/receiver, piezoelectric
transducer, and display devices.
• A pulser/receiver is an electronic
device that can produce high
voltage electrical pulses.
• Driven by the pulser, the
transducer generates high
frequency ultrasonic energy.
• The sound energy is introduced
and propagates through the
materials in the form of waves.
• When there is a discontinuity
(such as a crack) in the wave path,
part of the energy will be reflected
back from the flaw surface.
• The reflected wave signal is
transformed into an electrical signal
by the piezo electrical transducer
and is displayed on a screen which
provides the inspector information
about the size and the location of
features that reflect the sound.
Test Techniques – Normal and
Angle Beam
•In normal beam testing, the sound
beam is introduced into the test
article at 90 degree to the surface.
•In angle beam testing, the sound
beam is introduced into the test
article at some angle other than 90.

Advantages:
(1) It has high sensitivity which permits detection of minute defects.
(2) It has high penetrating power (of the order of 6 to 7 metres in steel) which allows
examination of extremely thick sections.
(3) It has a high accuracy of measurement of flaw position and size.
(4) It gives Instant test results and portable
(5) It needs access to only one surface of the specimen.
Limitations:
(1) Unfavourable geometry of the test specimen causes problems during inspection.
(2) Inspection of materials having undesirable internal structure is difficult.
(3) It requires the use of a couplant.
(4) The probe must be properly coupled during scanning.
(5) Defect orientation affects defect detectability.
(6) Equipment is quite expensive.
(7) Highly skilled manpower is required.
(8) Reference standards and calibration required.
(9) Rough surfaces can be a problem and surface preparation is necessary.
RADIOGRAPHY
Radiography Testing (RT), or industrial radiography is NDT method of inspecting materials for hidden
flaws by using the ability of short wavelength electromagnetic radiation (high energy photons) to
penetrate various materials.

 Advantages
◦ Permanent record
◦ No calibration on the job site
◦ Excellent for detecting internal discontinuities
◦ Beam direction unaffected by part geometry
 Disadvantages
◦ Radiation hazard
◦ Depth of discontinuity not indicated
◦ Orientation of linear discontinuities is important
◦ Relatively expensive
◦ Limited depth penetration
◦ Access to both sides required
ULTRASONIC TESTING RADIOGRAPHY TESTING

Less flaw detection capabilities More flaw detection capabilities

Compared to radiography less operational More operational safety is required as the

safety is required radiations are harmful

Probe is used Probe is not used

Better accuracy and reliability Very fast method of testing

Operated manually Less or no manual work

Used for detection of internal defect, For detection of internal defects, porosity,
measurement of conductivity and crack depth casting, lack of fusion in welding, cracks,
measurement of geometry variation and
thickness of components
An impact test measures how much energy is absorbed when an object
fractures or breaks under a high speed collision.
This is often called a material’s toughness.
It has the unit joules per metre cubed (J m-3)

Types of Notch-Toughness Tests

1. Depending on loading
(pendulum stroke or drop-weight loading)
2.Depending on the type of notched specimen
( Charpy V-notch, Charpy U-notch, or Izod)
Charpy Impact Testing
Charpy impact testing has been used for many years to test the impact
toughness of various metals. Since Charpy impact testing is both cheap and fast,
its use was extended to composites. A Charpy impact test machine is shown in
the following picture.
Specimen Preparation
The specimen that fits into the Charpy impact tester is rectangular with a notch
cut in one side. The notch allows for a predetermined crack initiation location.
Many composite Charpy impact tests are performed without the notch cut into
the specimen. In these cases it should be noted in the experimental procedure if
the notch is not present. A typical Charpy impact specimen is shown in the
following figure.

Charpy impact specimen

Test Setup and Procedure

The Charpy impact test method works by placing a notched specimen (with the
notch facing away from the point of contact) into a large machine with a
pendulum of a known weight. The pendulum is raised to a known height and
allowed to fall. As the pendulum swings, it impacts and breaks the specimen,
rising to a measured height. A figure displaying the process is shown below.

The difference in the initial and final heights is directly proportional to the
amount of energy lost due to fracturing the specimen. The total energy of
fracture is determined by
G = mg( hi – hf)

Fig has wrong

Where G is the total energy, m is the mass, g is gravitational acceleration, h i is

the original height, and hf is the final height.
Difference:
 The Charpy test involves three-point loading, where the test piece is
supported at both ends as a simple beam.
 Izod specimen is set up as a cantilever beam with the falling pendulum
striking the specimen above the notch
Drop Weight Impact Testing
Drop weight impact testing is another type of low velocity testing, and it is the
most common test for composite materials. Drop weight impact tests are done
to test the impact behavior on composite plates, which most closely resemble
impact damage in the field. When using a drop weight impact tester, two
categories of damage can occur. The first is clearly visibleimpact damage
(CVID), which can easily be seen by the naked eye. The second type of damage
is barely visible impact damage (BVID), which can eldom be seen by the naked
eye. Evaluation of both types of damage can be enhanced through the use of
post-impact testing.
In drop weight impact testing, a mass is raised to a known height and released,
impacting the specimen. The choice can be made between either an
instrumented or non-instrumented test machine. A figure displaying how an
instrumented impact machine works is shown below.

In Figure 6.7, x(t) is the coordinate system, H is the initial drop height, W is the
impact weight, and vo is the impact velocity. The tup is a hemispherical
impactor that measures the strain during impact [10].

Instrumented impact testing

It has been said that impact testing is where tensile testing was 50 years ago.
However, modern impact testers are becoming increasingly sophisticated. In
modern instruments, the load is increased steadily rather than added in
increments. Also any deformation to the sample is observed and recorded.
Instrumented drop weight and pendulum testing is considered to be the best
general impact testing method presently available
 HARDNESS
Hardness is a measure of a material’s resistance to localized plastic
deformation (e.g., a small dent or a scratch). Or
The hardness test measures the resistance to penetration of the surface of a
material by a hard object.
A qualitative and somewhat arbitrary hardness indexing scheme was devised,
termed the Mohs scale, which ranged from 1 on the soft end for talc to 10 for
diamond.
Principles
Force is applied to an indenter in order to determine the resistance of the
material to penetration.
The depth or size of the resulting indentation is measured, which in turn is
related to a hardness number.
if the material is soft, a fairly large or deep indentation will result and the
lower the hardness index number. If the material is hard, a relatively small or
shallow indentation will result.

Hardness tests are performed more frequently than any other mechanical test
for several reasons:
1. Hardness numbers are used primarily as a qualitative basis for comparison
of materials, specifications for manufacturing and heat treatment, quality
control, and correlation with other properties of materials

2.They are simple and inexpensive—ordinarily no special specimen need be

prepared, and the testing apparatus is relatively inexpensive.

3. The test is nondestructive—the specimen is neither fractured nor

excessively deformed; a small indentation is the only deformation.

4. Other mechanical properties often may be estimated from hardness data,

such as tensile strength. For the cast iron, steel and brass, the HB and the
tensile strength are related according to:
Tensile strength (psi) = 500 HB
Tensile strength (MPa)= 3.45 HB
4. The hardness tests is done to verify - a particular processing step -
Example ----annealing, hardenability, cold working, recrystallization,
surface treatments, and tempering.
5. For a known composition, the hardness associated with a particular
structure will vary.
An alloy with a carbon content of 0.69 (wt. %) and a martensitic structure
would have a hardness value of 65 HRC
while an alloy with a carbon content of 0.25 and a martensitic structure would
have an Rockwell C value of only 47 HRC (ASTM Standard A255, 1986).

classified in one of two ways:

• by the extent of the test force applied or
• the measurement method used.
• Depending on Applied force
• Depending on Applied force
‘‘Macro’’ test-load >1 kg is applied; Brinell testers, Rockwell, Vickers
testers
‘‘micro’’ refers to 1 kg of force is applied. Knoop, Vickers testers
“nanoindentation” testers-loads as light as 0.01 g
 Rockwell Hardness Tests
The Rockwell tests constitute the most common method used to measure
hardness because they are so simple to perform and require no special skills.
Several different scales may be utilized from possible combinations of various
indenters and different loads, which permit the testing of virtually all metal
alloys (as well as some polymers). Indenters include spherical and hardened
steel balls having diameters of and (1.588,3.175,6.350,and 12.70 mm),and a
conical diamond (Brale) indenter, which is used for the hardest materials.
With this system,a hardness number is determined by the difference in depth
of penetration resulting from the application of an initial minor load followed
by a larger major load; utilization of a minor load enhances test accuracy.

On the basis of the magnitude of both major and minor loads, there are two
types of tests: Rockwell and superficial Rockwell.
For Rockwell, the minor load is 10 kg,
whereas major loads are 60, 100, and 150 kg.
Each scale is represented by a letter of the alphabet;
For each scale, hardnesses may range up to 130 .Specimen thickness should be
at least ten times the indentation depth, whereas allowance should be made
for at least three indentation diameters between the center of one indentation
and the specimen edge, or to the center of a second indentation. The modern
apparatus for making Rockwell hardness measurements is automated and very
simple to use; hardness is read directly, and each measurement requires only a
few seconds.

Brinell Hardness Tests

In Brinell tests, as in Rockwell measurements, a hard, spherical indenter is
forced into the surface of the metal to be tested. The diameter of the
hardened steel (or tungsten carbide) indenter is 10.00 mm (0.394 in.).
Standard loads range between 500 and 3000 kg in 500-kg increments; during a
test, the load is maintained constant for a specified time (between 10 and 30
s).Harder materials require greater applied loads. The Brinell hardness number,
HB, is a function of both the magnitude of the load and the diameter of the
resulting indentation.This diameter is measured with a special low-power
microscope, utilizing a scale that is etched on the eyepiece.The measured
diameter is then converted to the appropriate HB number using a chart..
 Where
BHN=Brinell hardness
number(kgf/mm2)
P=applied load in kilogram-force(kgf)
/applied load in kg

D=diameter of indenter(mm)
D=diameter of indentation(mm)

Maximum specimen thickness as well as indentation position (relative to

specimen edges) and minimum indentation spacing requirements are the same
as for Rockwell tests. In addition, a well-defined indentation is required; this
necessitates a smooth flat surface in which the indentation is made.

Knoop and Vickers Microindentation Hardness Tests

Two other hardness-testing techniques are Knoop and Vickers (sometimes also
called diamond pyramid). For each test a very small diamond indenter having
pyramidal geometry is forced into the surface of the specimen. Applied loads
are much smaller than for Rockwell and Brinell, ranging between 1 and 1000
g.The resulting impression is observed under a microscope and measured; this
measurement is then converted into a hardness number. Careful specimen
surface preparation (grinding and polishing) may be necessary to ensure a
well-defined indentation that may be accurately measured. The Knoop and
Vickers hardness numbers are designated by HK and HV, respectively and
hardness scales for both techniques are approximately equivalent. Knoop and
Vickers are referred to as microindentation-testing methods on the basis of
indenter size. Both are well suited for measuring the hardness of small,
selected specimen regions; furthermore, Knoop is used for testing brittle
materials such as ceramics.
KHN and VHN are used to denote Knoop and Vickers hardness numbers,
respectively.
Sample preparation
• Rockwell tests: surface grinding to at least a 400-grit abrasive paper is
recommended.
• Microindentation tests, such as Vickers and Knoop: Rough polishing to a
finish of 3 mm or better is recommended.
• With any test where the indentation diameter must be measured, the
amount of deformation or scratches on the surface must not interfere
with the operator’s ability to determine the diameter.

The ELASTIC Range Means:
- The strain, or elongation over a unit length, will
behave linearly (as in y=mx +b) and thus
predictable.
-The material will return to its original shape
(Point 1) once an applied load is removed.
- The stress within the material is less than what
is required to create a plastic behavior (deform
or stretch significantly without increasing stress).
Strain Hardening
- If the material is loaded again from Point 4,
the curve will follow back to Point 3 with the
same Elastic Modulus (slope).
- The material now has a higher yield strength
of Point 4.
- Raising the yield strength by permanently
straining the material is called Strain Hardening.
Elastic Region (Point 1 –2)
- The material will return to its original
shape after the material is unloaded (like
a rubber band).
- The stress is linearly proportional to
the strain in this region.
σ
σ Eε or E
ε
σ : Stress (psi)
E : Elastic modulus (Young’s Modulus)
(psi)
ɛ: Strain (in/in)
-Point 2 : Yield Strength : a point at
which permanent deformation occurs. (
If it is passed, the material will no longer
return to its original length.)
Plastic Region (Point 2 –3)
-If the material is loaded beyond the yield
strength,the material will not return to its
original shape after unloading.
-It will have some permanent
deformation.
- If the material is unloaded at Point 3,
the curve will proceed from Point 3 to
Point 4. The slope will be the as the slope
between Point 1 and 2.
- The distance between Point 1 and 4
indicates the amount of permanent
deformation.
Tensile Strength (Point 3)
- The largest value of stress on the
diagram is called Tensile Strength(TS) or
Ultimate Tensile Strength (UTS)
- It is the maximum stress which the
material can support without breaking.
Fracture (Point 5)
- If the material is stretched beyond
Point 3, the stress decreases as necking
and non-uniform deformation occur.
- Fracture will finally occur at Point 5.
 Thermal Analysis
• Thermal analysis is a branch of materials science where the properties of
materials are studied as they change with temperature.
•When matter is heated, it undergoes certain physical and chemical changes.
• Physical changes include phase changes such as melting, vaporization,
crystallization, transitions between crystal structures, changes in microstructure
in metal alloys and polymers, volume changes (expansion and contraction), and
changes in mechanical behavior.
• Chemical changes include reactions to form new products, oxidation,
corrosion, decomposition, dehydration, chemisorption, and the like.
• These physical and chemical changes take place over a wide temperature
range.
Basic Principles of Thermal Analysis
Thermogravimetric Analysis (TGA)
• Principle: TGA measures the amount and the rate of weight change of a
material with respect to temperature or time in controlled environments.
• Instrumentation
A TGA consists of three major parts a furnace,
1. A microgram balance,
2. An auto sampler and
3. A thermocouple.
A computer generally controls the furnace and the data (weight vs. sample
temperature) is collected and processed by computer.
• Several modern analytical microbalances are commercially available - torsion
balances, spring balances, and electro balances. TGA balances are available
for sample masses from 1 to 1000 mg, with the usual sample weighing between
5 and 20 mg.

• The furnace surrounds the sample and sample holder. It must be capable of
being programmed for a linear heating rate. Modern instruments can be
heated and cooled rapidly. These instruments that heat at rates of up to
10000C/min are available.
• The auto sampler helps to load the samples on to the microbalance.
• It is particularly important to measure the temperature of the sample rather
than that of the furnace. This is difficult because the temperature is measured
with a thermocouple that is near but not in the sample The thermocouple sits
right above the sample. Care should be taken at all times that the thermocouple
is not in touch with the sample which is in a platinum pan.

Experimental Conditions
• Heating Rate
• Purge gas

Heating Rate
• Samples are heated at a rate of 10 or 20°C/min in most cases.
• Lowering the heating rates is known to improve the resolution of overlapping
weight losses.
• Advances in the technology have made it possible for variable heating rates
(High Resolution TGA) to improve resolution by automatically reducing the
heating rate during periods of weight loss
Purge gas
• Nitrogen is the most common gas used to purge samples in TGA due to its
inert nature.
• Whereas, helium provides the best baseline.
• Air is known to improve resolution because of a difference in the oxidative
stability of components in the sample.
• Vacuum may be used where the sample contains volatile components, which
helps improve separation from the onset of decomposition since the volatiles
come off at lower temperatures in vacuum.
• e.g. oil in a rubber tire product.
 Differencial Scanning Calorimetry
(DSC)

DSC is a thermo-analytical technique in which the difference in the amount of

heat required to increase the temperature of a sample and reference is measured
as a function of temperature.
DSC analysis determines
• Tg Glass Transition Temperature
– Temperature (°C) at which amorphous polymers or an amorphous part of a
crystalline polymer go from a hard brittle state to a soft rubbery state
• Tm Melting point
– Temperature (°C) at which a crystalline polymer melts
• Δ Hm Energy Absorbed (joules/gram)
– Amount of energy a sample absorbs when melting
• Tc Crystallization Point
– Temperature at which a polymer crystallizes upon heating or cooling
• Δ Hc Energy Released (joules/gram)
– Amount of energy a sample releases when crystallizing
Differential Thermal Analysis (DTA)
Definition: DTA is a technique in which the temperature between sample &
thermally inert reference substance is continuously recorded as a function of
temperature /time.
If any reaction (physical or chemical change) takes place temperature
difference (ΔT) will occur b/w sample & reference material .

• Some changes result in heat being absorbed by the sample. These types of
changes are called endothermic. Examples of endothermic changes include
phase changes such as melting (fusion), vaporization, sublimation, and some
transitions between two different crystal structures for a material. Chemical
reactions can be endothermic, including dehydration, decomposition,
oxidation–reduction, and solid–state reactions.

• Other changes result in heat being given off by the sample. Such changes are
termed exothermic. Exothermic changes include phase changes such as
freezing (crystallization), some transitions between different crystal structures
and chemical reactions; decomposition, oxidation–reduction, and
chemisorptioncan be exothermic.
Instrumentation
Sample holder
Sample & reference crucibles are generally metallic (Al, Pt) or ceramic
(silica) and may or may not have a lid. Best results are obtained when the area
of contact between the sample and the pan or crucible is maximized. Samples
are generally in the 1–10 mg range for analytical applications.
 Furnace
The sample and reference should be matched thermally and
arranged symmetrically with the furnace so that they are both
heated or cooled in an identical manner.
The metal block surrounding the wells acts as a heat sink.
The temperature of the heat sink is slowly increased using an
internal heater.
Sensors & Recording system
A pair of matched thermocouples is used.
One pair is in contact with the sample or the sample container, the other pair
is in contact with the reference.
The output of the differential thermocouple, Ts - Tr or ΔT, is amplified and
sent to the data acquisition system.
This allows the difference in temperature between the sample and the
reference to be recorded as a function of either the sample temperature, the
reference temperature or time.

Operating temperatures for DTA instruments are generally room temperature to

about 16000C, although one manufacturer makes a DTA capable of operating
from - 1500C to 24000C.
• To reach the very low subambient temperatures, a liquid nitrogen cooling
accessory is needed.
• Some low temperatures (but not -1500C) may be reached with electrical
cooling devices or with forced air-cooling.
• When a physical change takes place in the sample, heat is absorbed or
generated.
• For example, when a metal carbonate decomposes, CO2 is evolved. This is an
endothermic reaction; heat is absorbed and the sample temperature decreases.
The sample is now at a lower temperature than the reference. The temperature
difference between the sample and reference generates a net signal, which is
recorded.
Applications of DTA
DTA is based on changes of heat flow into the sample
Using DTA, we can detect the decomposition or volatilization of the
sample, just as we can with TGA.
physical changes that do not involve weight changes can be detected by
DTA. Such changes include crystallization, melting, changes in solid crystal
phases.
The main use of DTA is to detect thermal processes and characterize them as
exothermic or endothermic, reversible or irreversible, but only
qualitatively.
• DTA thermal curves can be used to determine the order of a reaction
(kinetics), and can provide the information required to construct phase
diagrams for materials.
• DTA is widely used in the pharmaceuticals and food industries.
• DTA may be used in cement chemistry, mineralogical research and in
environmental studies.

Scanning electron microscope (SEM) is a microscope that uses electrons rather

than light to form an image.

Advantages of Using SEM over OM

Magnification Depth of Field Resolution

OM 4x –1000x Small depth of field Low resolution
15.5μm – 0.19μm ~ 0.2μm
SEM 10x – 3000000x Large depth of field High resolution
4mm – 0.4μm 1-10nm

The SEM has a large depth of field, which allows a large amount of the sample
to be in focus at one time and produces an image that is a good representation
of the three-dimensional sample. The SEM also produces images of high
resolution, which means that closely features can be examined at a high
magnification.

SEM is primarily used to study surface topography.SEM is complementary to

spectroscopy
What can be seen
• Grain size
• Orientation of grain and crystal
• Phases
• Chemical attack resulting in the growth of the precipitates
• Where the reaction take place (at boundaries or certain grains)
• Topography of fractured surfaces
• Porosity
At higher magnification
• Crystal structure of minor phases
• Formation of amorphous surface layer
• Interfacial layers etc.
SEM Instrumentation:
Cathode: Electrons can be emitted from a very fine hair V - type cathode made
of tungsten (W) which may be thorium doped for higher electron emission. The
W hair cathode is heated to ~2300º C. Higher electron current can be emitted
from lanthanum hexaboride (LaB6 ) cathode at much lower temperature.
Wehnelt: Wehnelt is a cylindrical cup electrode controlling the electron current
intensity emitted from the electron gun.
Anode: Anode accelerates the electron to a desired energy. The electron
energy can be selected from 1 keV to 30, 40 keV by changing of the floating
potential of the electron gun.
Vacuum: Vacuum is needed to form electron beam for its free passage from its
cathode origin to the sample. The number of collisions between electrons and
residual molecules should be negligible small.
Magnetic lens (Condenser): a magnetic focusing electron lens is located
nearby the anode to focus the electron beam. This lens is called condenser.
The condenser is used to adjust the spot size of the electron beam. The
condenser is the lens with a short focal length.
x- y scanning coils:
The scanning generator powers x and y coils for both the electron beam probe
and electron beam of cathode ray tube (CRT). These two scans are
synchronized. Difference is only that electron beam probe is scanned over a
very small sample surface while the electron beam of cathode ray tube is
scanned over whole CRT screen. These scan areas are responsible for
magnification
Magnetic lens (Objective): there is a magnetic lens that finally focuses the e-
beam on specimen. This last magnetic lens is called objective. The objective
has longer focal length to provide the higher depth of field.
Everhard-Thornley Electron Detector (E-T detector)
The electrons emitted from solids can be detected with an E-T detector. This
detector is sensitive to both backscattered and secondary emitted electrons.
The backscattered electrons are sufficiently energetic to directly excite the
detector. Low energy secondary electrons are drawn towards the detector by a
potential of + 300 V applied to a collector wire - mesh screen at the front the
detector. Once inside the screen the collected electrons are accelerated
towards a scintillator with a potential of +10 kV (12 kV). The accelerated
electrons produce light when incident the scintillator. The light is led through a
light pipe to a photoelectron multiplier tube (PMT) where it is converted to an
electric signal. The electric signal after electrical processing/ amplification
modulates the intensity of the viewing CRT. The processed signal is supplied to
the CRT wehnelt.
 Secondary Electrons (SE)

The interaction of the beam electron with the solid can lead to the
ejection of loosely bound electrons of the conduction band in metals or the
valence band in insulators and semiconductors. This interaction results in the
transfer of only a few electron volts of energy to the band electron and causes a
slight energy loss and path change in the incident electron. Each incident
electron can produce several secondary electrons.

Arbitrairly, such emergent electrons with energies less than 50 eV are

called secondary electrons. 90% of secondary electrons have energies less than
10 eV; most from 2 to 5

Production of SE is very topography related. Due to their low energy,

only SE that are very near the surface (<10nm) can exit the sample and be
examined (small escape depth).

Backscattered Electrons (BSE)

BSE are produced by elastic interactions of beam electrons with nuclei

of atoms in the specimen and they have high energy and large escape depth.

elastic scattering results in little or no change in energy of the scattered

electron, although there is a change in momentum. Since momentum, p=mv,
and m doesn't change, the direction of the velocity vector must change. The
angle of scattering can range from 0-180 degrees. Elastic scattering occurs
between the negative electron and the positive nucleus.

BSE images show characteristics of atomic number contrast, i.e., high

average Z appear brighter than those of low average Z. k

Backscattered electrons Secondary electrons

sensitive to atomic number Sensitive to surface topology
high K.E. K.E. < 50eV;
originated from the lower surface originated from the top surface region
region

Why Need a Vacuum?

When a SEM is used, the electron-optical column and sample chamber must
always be at a vacuum.
1.If the column is in a gas filled environment, electrons will be scattered by gas
molecules which would lead to reduction of the beam intensity and stability.

2.Other gas molecules, which could come from the sample or the microscope
itself, could form compounds and condense on the sample. This would lower
the contrast and obscure detail in the image.

Electron guns

Electron guns are used to produce a fine, controlled beam of electrons which are
then focused at the specimen surface.The electron guns may either be
thermionic gun or field-emission gun
 Thermionic Emission Gun
• A tungsten filament heated by
DC to approximately 2700K or
LaB6 rod heated to around
2000K
• A vacuum of 10-3 Pa (10-4 Pa for
LaB6) is needed to prevent
oxidation of the filament
• Electrons “boil off” from the tip
of the filament
• Electrons are accelerated by an
acceleration voltage of 1-50kV
Field Emission Gun
• The tip of a tungsten needle is
made very sharp (radius < 0.1
m)
• The electric field at the tip is
very strong (> 107 V/cm) due to
the sharp point effect
• Ultra-high vacuum (better than
10-6 Pa) is needed to avoid ion
bombardment to the tip from the
residual gas.
• Electrons are pulled out from
the tip by the strong electric
field
• Electron probe diameter < 1 nm
is possible