Aplicaciones metalográfica en general

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Aplicaciones metalográfica en general

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Metallography

Applications

Ashraf Ali

NED University of Engineering and Technology, Karachi

1

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.

because of variations in chemical composition, method of

manufacturing, heat treatment and many other variables.

Macro-etching reveal important information e.g., grain

structure

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.

because of variations in chemical composition, method of

manufacturing, heat treatment and many other variables.

Macro-etching reveal important information e.g., grain

structure

Macro Examination

Macro-etching of Steel Ingot

shrinkage defects

Macro Examination

Macro-Examinations are also performed on a

polished and etched cross-section of a welded

material.

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

examinations.

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

photomacrograph.

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

material.

Weld Microstructure

Weld

Heatd

Affected

Zone

(HAZ)

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

Nodular

Cast Iron

Nodular

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

results.

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

carburization.

The depth is determined as the depth

where a uniform microstructure,

hardness, or carbon content, typical of

the interior of the specimen is

observed.

This method will detect surface losses

in carbon content due to heating at

elevated temperatures, as in hot

working or heat treatment.

steel

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

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

pre-etched with sodium hydroxide, colour etched

with potassium permanganate.

heading. Nickel base alloy Etchant: modifi ed Kallings

Quantitative

Metallography

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

(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

manually.

AA=

LL=

PP=

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.

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.

(Accuracy)

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

points).

Counting 5000 points generally give 2-5% accuracy.

(Accuracy)

Relative Error

%

No. of Particles

required to

be counted

1.0

48000

2.0

12000

4.0

3000

5.0

1920

10.0

480

Fe-0.18C-0.43Mn steel

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.

ASTM

E112

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).

with outline grain structures

at various dimensions by

which grain sized range

form 1 (very coarse) to 10

(very fine).

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

n = 2G-1

where n is the number of grains per square inch at 100X.

multiply n by 15.5.

The four ASTM grain size charts show graded series of grain

structures of different types.

(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.

Grains must be marked to avoid biasing

(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

ASTM112:

LT

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.

Parameters to the Microscopically Determined

ASTM Grain Size, G

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 can be measured using either the planimetric or the intercept

methods.

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

structure.

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.

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

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.

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

Pearlite 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.

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