Vous êtes sur la page 1sur 40

Department of Materials Engineering

Ashraf Ali
NED University of Engineering and Technology, Karachi

Macro Examination
Macro-etching is the procedure
in which a specimen is etched
and evaluated macro
structurally at low
magnifications. It is a frequently
used technique for evaluating
products such as billets, bars,
blooms, and forgings.

Macro-etched Copper Ingot.

For example steels react differently to etching reagents

because of variations in chemical composition, method of
manufacturing, heat treatment and many other variables.
Macro-etching reveal important information e.g., grain

Macro Examination
Macro-etching is the procedure
in which a specimen is etched
and evaluated macro
structurally at low
magnifications. It is a frequently
used technique for evaluating
products such as billets, bars,
blooms, and forgings.

Macro-etched Copper Ingot.

For example steels react differently to etching reagents

because of variations in chemical composition, method of
manufacturing, heat treatment and many other variables.
Macro-etching reveal important information e.g., grain

macro etched copper disc

Macro Examination
Macro-etching of Steel Ingot

(a) macro segregation

(b) macro segregation and (c) shrinkage defects

shrinkage defects

Macro Examination
Macro-Examinations are also performed on a
polished and etched cross-section of a welded
During the examination, a number of features
can be determined including weld run
sequence, important for weld procedure
qualifications tests.
Slag, porosity, lack of weld penetration, lack of
sidewall fusion and poor weld profile are
among the features observed in such
It is normal to look for such defects either by
standard visual examination or at magnifications
of up to 50X.
It is also routine to photograph the section to
provide a permanent record. This is known as a

Micro Examination
This is performed on samples either cut to
size or mounted in a resin mold.
The samples are polished to a fine finish,
normally one micron diamond paste, and
usually etched in an appropriate chemical
solution prior to examination on a
metallurgical microscope.
Micro-examination is performed for a
number of purposes, the most obvious of
which is to assess the structure of the

Weld Duplex Stainless Steel

Weld Microstructure



Base Metal
Fig. 30 Microstructure of 7-Mo PLUS duplex stainless steel (Fe-<0.03%C-<2%Mn-27.5%Cr4.85%Ni-1.75%Mo-0.25%N) welded with Nitronic 50, etched with Beraha's BI reagent, and
viewed with brightfield illumination. Ferrite is colored, and austenite is unaffected. The
magnification bar is 200 m long.

Micro Examination
It is also common to examine for metallurgical anomalies such as third
phase precipitates, excessive grain growth, etc.
Many routine tests such as phase counting or grain size determinations
are performed in conjunction with micro-examinations.

Micro Examination
Revealing -ferrite in
Martensitic Stainless Steel

Cast Iron

Cast Iron

Weld Examination
Metallographic weld evaluations can
take many forms.
In its most simple form, a weld deposit
can be visually examined for large scale
defects such as porosity or lack of
fusion defects.
On a micro scale, the examination can
take the form of phase balance
assessments from weld cap to weld root
or a check for non-metallic or third
phase precipitates.
Examination of weld growth patterns is
also used to determine reasons for poor
mechanical test results.
For example, an extensive central
columnar grain pattern can cause a
plane of weakness giving poor charpy

Drawing showing the various regions of the HAZ

in a single-pass weld and the possible defects.

Case Depth
Case hardening may be defined as a process for
hardening a ferrous materials in such a manner
that the surface layer (known as the case), is
substantially harder than the remaining materials
(known as the core).
This process is controlled through carburizing,
nitriding, carbonitriding, cyaniding, induction and
flame hardening.
The chemical composition, mechanical properties,
or both, are effected by these practices.
Methods for determining case depth are either
chemical, mechanical or visual and should be
selected on the basis of specific requirements.

Decarburisation Measurement
This method is designed to detect
changes in the microstructure,
hardness, or carbon content at the
surface of the steel sections due to
The depth is determined as the depth
where a uniform microstructure,
hardness, or carbon content, typical of
the interior of the specimen is
This method will detect surface losses
in carbon content due to heating at
elevated temperatures, as in hot
working or heat treatment.

Decarburisation in Fe-0.8C Plain carbon


Coating /
Plating Evaluation
A coating or plating application is used primarily for
protection of the substrate.
The thickness is an important factor in the
performance of the coating or plating.
A portion of the specimen is cut, mounted
transversely, a prepared in accordance with
acceptable or suitable techniques.
The thickness of the cross section is measured with
an optical microscope.
When the coating or plating is thinner than .00020",
the measurement should be taken with the aid of
the scanning electron microscope.
Cross-sectioned metallographic examinations of
substrates with platings, surface evaluations,
thickness measurements, weight per volume

Electric arc metal spray coating, showing grey

oxides and round, unmelted particles

Surface Evaluation
Surface inspection includes the
detection of surface flaws and he
measurement of surface defects
and roughness. One method
includes the use of a laser light.
When the scattered light is reflected
off the surface of a sample, it can
be analyzed and measure. Another
method is the use of a motorized
stylus (profilometer). The stylus is
placed on the surface and the
texture of the material is measured
in micro-inches or millimeters

Fig.17: Burr on a solder spot of a heat exchanger,

pre-etched with sodium hydroxide, colour etched
with potassium permanganate.

Fig. 8: Melted grain boundaries due to overheating in

heading. Nickel base alloy Etchant: modifi ed Kallings

Department of Materials Engineering

NED University of Engineering and Technology, Karachi

Quantitative Metallography
The properties of materials
depends upon size, spacing
and amount of phases in
the sample.
Quantitative metallography
is a group of material
characterisation techniques
in which amount and size of
microconstitunts in the
sample measured.

Phase Proportions

316 austenitic stainless steel, containing sigma phase

(formed probably from delta ferrite after low-time, hightemperature exposure) colored by Murakamis reagent
at 80C, 500x, BF

Phase Proportions
One of the most common measurements,
determination of the amount of phases present,
can be done using three different methods:
(a) Areal analysis, developed by Delesse in 1848, says that the
area percent of a phase on a 2-D plane is equal to its volumetric
percent, that is, AA = VV. However, measuring the area of second
phases is very tedious unless they are quite coarse.
(b) Lineal analysis, developed by Rosiwal in 1898,
says that the lineal fraction of test lines in a phase on the 2-D plane
is equal to its volumetric percentage, that is, LL = VV. This is easier
to determine but still rather tedious.
(c) Point Count Analysis developed by several metallographers
state that the percentage of points on a test grid lying in the phase of
interest was equal to the volumetric percentage, that is, PP = VV.

Phase Proportions
Point Count Analysis, of
the three methods, is the
most efficient technique;
that is, it produces the
best precision for the
least effort when done


The point counting

technique is described
fully in ASTM E 562 (also
ISO 9042).
Image analysers use essentially the same procedure; that is, the amount
of a phase (usually called the area fraction or volume fraction even if it
actually is a point fraction) is determined by the number of picture
elements or pixels in the phase of interest divided by the total number of
pixels; i.e., PP, expressed usually as a percentage.

Point Counting Example

The microstructure shows the beta phase in Muntz metal (Cu40% Zn) preferentially colored by Klemms reagent while the
alpha matrix is unaffected - ideal conditions for point counting.
Since there is less than
, we will count the number
of times the points fall in the
colored grains.
The amount of is simply
100 - % .
we superimposed a 64point test grid (8 rows of 8
points) over the structure
and we have 17 hits.

The point fraction (volume fraction) is 17/64 = 0.266 or 26.6%.

Point Counting Method

The point counting grid would be placed randomly over
the structure a number of times so that the point fraction
is determined for a number of fields.
The necessary number of fields to yield a 10% relative
accuracy varies inversely with the volume fraction (the
lower the volume fraction, the greater the number of
fields, i.e., the greater the total number of applied grid
Counting 5000 points generally give 2-5% accuracy.

Areal Analysis Method

Relative Error

No. of Particles
required to
be counted











Grain Size Determination

Fe-0.18C-0.43Mn steel

Grain Size Determination

A material's grain size is important as it affects its
mechanical properties.
e.g., a refined grain structure gives enhanced
toughness properties and alloying elements are
deliberately added during the steel-making process
to assist in grain refinement.
Grain size is determined from a polished and
etched sample using optical microscopy at a
magnification of 100X.


There are three main methods of measuring

the grain size:(a) A comparative method based on charts
defining areas of grains intersecting a planar section
through the microstructure.
(b) Grain size can be measured by the planimetric
method (developed by Zay Jeffries in 1916)
(c) or by the intercept method (developed by Emil
Heyn in 1904).

ASTM E112 shows charts

with outline grain structures
at various dimensions by
which grain sized range
form 1 (very coarse) to 10
(very fine).

ASTM Grain Size Number

The ASTM grain size number, G , is defined as:

n = 2G-1
where n is the number of grains per square inch at 100X.

To convert n to NA (the number of grains per square mm at IX),

multiply n by 15.5.
The four ASTM grain size charts show graded series of grain
structures of different types.

Planimetric Method of Grain Size

(Jeffries Methods)
Grain size can be measured by the planimetric
method (developed by Zay Jeffries in 1916).
In the planimetric method, a count is made of
the number of grains completely within a
circle of known area and half of the number of
grains intersected by the circle to obtain NA.

NA = f (Ninside + Nintercepted)
where f is Jefries multiplier =0.0002M2 to
obtain grains/mm2 (M is magnification).
This method is slow when done manually
because the grains must be marked when
counted to obtain an accurate count.

Count grains within circle only

Grains must be marked to avoid biasing

Intercept Method of Grain Size

(Heyn Methods)
In the intercept method either straight lines or circles are
placed over the structure and a count is made of either the
number of grain boundary intersections, P, or the number
of grains intercepted, N, by the line.
P or N is divided by the true line length, LT, to determine
PL or NL, the number of intersections or interceptions per
unit length (for a single phased structure). The reciprocal
of PL or NL gives the mean lineal intercept length, l,

l = 1/NL = 1/PL
m.l.i. l is a measure of grain size that can be converted
to ASTM no. G according to the formula given in

G = {-6.644 (log10 l) 3.288}

No. of grains=N=5
No. of grain boundaries=P=5

The intercept method is more efficient than the planimetric method yielding acceptable
measurement precision (<10% relative accuracy) in much less time.
ASTM E 112 contains a complete description of these methods.

TABLE 6: Grain Size Equations Relating Measured

Parameters to the Microscopically Determined
ASTM Grain Size, G

ASTM Grain Size Number

Specimens with Non-Equiaxed

Grain Shapes
If the grain shape was altered by
processing so that the grains are no
longer equiaxed in shape, grain size
measurements should be made on
longitudinal (l), transverse (t) and
planar (p) oriented surfaces for
rectangular bar, plate or sheet type
material. For round bars, radial
longitudinal and transverse sections
are used.
The hot rolled microstructure of an
austenitic-ferritic duplex structure, 40
to 50 percent of which is a gray
ferritic phase, while the remainder is
a white austenitic phase.

Grain Size Example

Grain size can be measured using either the planimetric or the intercept
In the planimetric method, ASTM recommends using a test circle with a
diameter of 79.8 mm (5000 sq. mm area) place randomly over the grain
To obtain an accurate count of the
number of grains inside the circle and
the number intercepted by the circle,
we must mark the grains on the
template as we count which makes
this method slow (although this is not
a problem by image analysis).
We must know the magnification of
the image as well.

Grain Size Example: Solution

The image shows the grain structure at 200X of a
low carbon sheet steel after colour etching.
A circle of known size (64.4mm diameter) has been
placed over the image to illustrate the method.
There are 44 grains within the circle (ninside) and 34
grains intercepted by the circle (nintercepted).
The number of grains per sq. mm, NA, is calculated from:
NA = f {ninside + (nintercepted)}
The multiplier f is calculated from (M2/circle area), where M is the magnification of
the image.
For this example,
NA = 12.28 {44 + (34)} = 749.1 grains /sq. mm
From NA, we can calculate the ASTM grain size number, G,using the following
formula from E 112-96:
G = {3.322 (log10 NA) 2.954} = 6.6

Grain Size Example:

Intercept Method Solution
The ASTM grain size can also be determined using the intercept
method counting either the number of grains intercepted, N, or the
number of grain boundaries intersected, P, with a test line.
Using the same image (shown on previous page), the count of the number of grains
intercepted by the circle is N.
To calculate the number of interceptions per mm, NL, we divide N by the true length
(circumference) of the circle.
Since the diameter of the circle is 64.4mm, its circumference is D, that is, 202.3mm.
The true length is 202.3mm divided by the magnification, M, that is, 1.01mm.
NL = N/LT = 34/ 1.01 = 33.6 interceptions per mm.
To calculate the grain size, we first determine the mean lineal intercept length, l, which is the
reciprocal of NL (or of PL, the number of grain boundary intersections per unit length).
l = 1/ 33.6 = 0.0298mm.
G is calculated from an equation from E 112-96:
G = {-6.644 (log10 l) 3.288}
where l is in mm. In this example, G = 6.85.

The Accuracy of Grain Size

Measurement Methods
Since the two methods are sensing different geometric aspects of the
three-dimensional grain structure, they will not give exactly the same
value, but they will be close, generally within the experimental limitations
of the measurements.
In practice, we would repeat these measurements on a number of fields
in order to obtain a good estimate of the grain size

Inter-Lamellar Spacing

Interlamellar Spacing oof

Pearlite Example

Interlamellar Spacing Example

Traditionally, the metallographer has searched for the finest appearing interlamellar
colony and made a measurement of its spacing using a test line perpendicular to the
lamellae. This spacing is claimed to be the true interlamellar spacing.
However, this method is not reproducible as the longer you search, the finer the
measured spacing. A better approach is to measure a mean random spacing and
divide that by two to get the mean true spacing.
The micrograph shown above is that of an as-rolled carbon steel of about 0.45% C,
etched with 4% picral and photographed with the SEM (specimen perpendicular to
the beam) using secondary electrons at 17,800x magnification.
A circle with a diameter of 49.7mm was placed over the lamellae and the number of
carbide lamellae intercepted by the test line, N, was counted.
NL was again determined as N (23) divided by the true line length, D/M, where the
circle diameter, D, is 49.7mm and M is 17,800x.
The NL calculated as 2622 interceptions per mm.
The mean random spacing, r, is given by:
r = 1/NL = 0.381m = 381nm
The mean true spacing, t, is r /2 = 190.7nm.

Next Class

Optical MicroscopyImaging Techniques