Alteration of Microstructure / 81

Fig. 3.56 Microstructure of the various layers of the rail steel in Fig. 3.55. (a) The white layer at the surface (unattacked by the etchant), (b) tempered plate
martensite, (c) as-quenched plate martensite and pearlite (dark), and (d) pearlite base microstructure. 4% picral etch. 1000
82 / Metallographers Guide

these sites, sufficient hydrogen gas pressure can create a separa-
tion at the steel/inclusion interface. As the component is stressed,
the separation can extend into a crack. Hydrogen akes or
cracks form in this manner. An example of hydrogen akes in an
AISI/SAE 1080 steel bar is shown in Fig. 3.58. From these
micrographs, it is evident that hydrogen cracks can more easily be
detected in a sample in the unetched condition (Fig. 3.58a) than in
the etched condition (Fig. 3.58b). Many times, the etched micro-
structure can obscure the cracks, because there are so many other
features present. Also, differential interference contrast (Nomar-
ski) can be very helpful in locating cracks.
Note the vast improvement in the same AISI/SAE 1080 steel
shown in both bright-eld (Fig. 3.59a) and differential interfer-
ence contrast (Fig. 3.59b). One way to detect hydrogen damage is
in the fracture appearance of through-thickness tensile specimens.
If hydrogen akes are present, sheyes appear on the fracture

Fig. 3.57 Microstructure of a Ni-Cr-Mo steel held at 565 C (1050 F) under a load of 210 MPa (30 ksi), showing (a) initial void formation at the austenite
grain boundaries, (b) void linkup, and (c) separation of an austenite grain boundary. 4% picral and HCl etch. 500

surface. Fisheyes are shiny, rounded regions that have developed
by internal cracks caused by hydrogen damage. These regions
were there before the tensile fracture took place.
An unusual example of a decarburized region surrounding a
hydrogen ake in an AISI/SAE 1080 steel can be seen in Fig.
3.60. In this case, the component was heat treated after the
hydrogen crack formed. Here, exposure to 870 C (1600 F) for
ve hours allowed the hydrogen gas to react with the carbon in the
steel to form methane gas (CH4). The result was carbon depletion
Fig. 3.58 Hydrogen akes (crackssee arrows) found in an AISI/SAE
1080 steel bar in the (a) unetched and (b) etched condition. 4%
picral etch. 1000
Alteration of Microstructure / 83
(decarburization) along the crack surface, seen as the white
nonetching constituent in Fig. 3.60.
An example of severe hydrogen damage is shown in Fig.
3.61(a), representing an ASTM A516 steel plate. In this micro-
graph, one can see cracks that developed by grain-boundary
separation along the banded regions. Usually these cracks are not
noticed until the part is in service, where it is exposed to some
kind of stress, that is, thermal or mechanical stress. Under
continued stress, the part usually fails as the crack or cracks grow
Fig. 3.59 Another example of a hydrogen ake (crack) in an AISI/SAE
1080 bar showing (a) the crack in bright-eld illumination and
(b) in differential interference contrast (Nomarski). Unetched. 1000
84 / Metallographers Guide

in length. Also, as atomic hydrogen diffuses into the steel, it forms the dissolution of the pearlite colonies adjacent to the cracks
molecular hydrogen that cannot leave, because in its molecular caused by the reaction of the hydrogen with the iron carbide. Once
state, the diffusivity is extremely low. As hydrogen diffusion grain-boundary separation occurs, the strength of the tube will
continues, the molecular hydrogen begins to form gas pockets that decrease, and the tube will eventually fail.
are under very high pressure. In the previous example, one can see Corrosion Effects. Corrosion is generally thought to affect only
in the the enlarged view of Fig. 3.61(b) that the gas pressure the outer surface layer of a part. This is not always the case. For
actually expanded the cracks and plastically deformed the regions example, as in the case of a gray cast iron, corrosion can penetrate
between cracks (note the bending of the ferrite/pearlite bands into the interior of a component, for example, an underground
between the two expanded cracks). Once a hydrogen-related crack water pipe, due to the connectivity of the graphite akes. An
forms, the process is irreversible, and the part must be taken out
of service before catastrophic failure occurs.
Another form of hydrogen damage can occur in service from
electrochemical corrosion reactions. Such a reaction can occur in
steel boiler tubes exposed to high temperature and high-pressure
steam. Water can react with iron at high temperature to create
atomic hydrogen (as opposed to molecular hydrogen, H2) and iron
oxide. The atomic hydrogen can easily diffuse into the steel boiler
tube and cause damage. One form of damage occurs when
hydrogen can combine with the carbides (cementite) in the steel to
form methane gas, CH4, which can cause internal grain-boundary
separation similar to the hydrogen akes described previously. An
example of this type of damage is illustrated in a SA 210 boiler
tube exposed for hundreds of hours to superheated steam at 360
C (675 F) under a pressure of 18 MPa (2.6 ksi). Figure 3.62(a)
shows the microstructure of the boiler tube in its original
condition, and Fig. 3.62(b) shows the result of the methane
damage. The damage is in the form of grain-boundary separation
created by the increased pressure developed by the reaction of
hydrogen with cementite. The methane gas is in molecular form,
and the molecules are too big to easily diffuse in the steel. Note

Fig. 3.60 An internal hydrogen ake (crack) in an AISI/SAE 1080 steel bar
that was exposed to a temperature of 870 C (1600 F) for 5 h.
The crack surface was decarburized (white area surrounding crack) by the
reaction of the hydrogen with the carbon in the steel. Pearlite matrix. 4%
picral etch. 1500
Fig. 3.61 Microstructure of an as-rolled ASTM A516 steel plate showing
hydrogen akes along the pearlite bands. 2% nital and 4%
picral etch. (a) 50 and (b) 400
 Alteration of Microstructure / 85

example is shown in Fig. 3.63(a). Here, corrosion products can be
found surrounding the ake graphite and graphitic cells (a cell is
a connected network of graphite akes). Figure 3.63(b) shows the
corrosion product and graphite akes at higher magnication. The
penetration of corrosion, in a way, proves that the graphite akes
are interconnected.
Corrosion engineers often call this type of corrosion graphiti-
zation, which, to a metallurgist, is obviously incorrect, because
the graphite was present before the corrosion took place. What has
happened in this case is selective leaching of the iron matrix
around the graphite akes. In very severe cases, the entire outer
skin of the corroded pipe or component is graphite, with all the

Fig. 3.62 Microstructure of an ASME SA 210 steel tube consisting of (a) ferrite (light etching constituent) and pearlite (dark etching constituent) and (b) a
hydrogen-damaged region showing cracks (arrows) at the pearlite/ferrite interfaces. 4% picral etch. 1000

Fig. 3.63 Microstructure of a gray cast iron water pipe with corrosion penetrating below the surface along graphite ake networks (cells) (see arrows). (a)
unetched, 50 and (b) 4% picral etch, 500
86 / Metallographers Guide
iron leached from the surface. From a corrosion viewpoint, the
graphite and iron act as a galvanic cell, where the graphite is the
cathode and the iron is the anode. Because of the galvanic action,
corrosion is enhanced next to the graphite akes. In a previous
section in this chapter, the term graphitization has been shown
to be the formation of graphite during a long-term exposure of a
carbon steel to temperatures between 315 and 370 C (600 and
700 F).
SELECTED REFERENCES
Atlas of Microstructures of Industrial Alloys, Vol 7, Metals
Handbook, 8th ed., American Society for Metals, 1972
The Heat Treaters GuideStandard Practices and Procedures
for Steel, American Society for Metals, 1982
Heat Treating, Vol 4, ASM Handbook, ASM International,
1991
G. Krauss, Principles of Heat Treatment, 2nd ed., ASM
International, 1993
Properties and Selection: Irons, Steels, and High-Perfor-
mance Alloys, Vol 1, ASM Handbook, ASM International,
1990
L.E. Samuels, Optical Microscopy of Carbon Steels, American
Society for Metals, 1980
H. Thielsch, Defects and Failures in Pressure Vessels and
Piping, Reinhold Publishing, 1965
Metallographer's Guide: Practices and Procedures for Irons and Steels Copyright 2002 ASM International
Bruce L. Bramfitt, Arlan O. Benscoter, p87-107 All rights reserved.
DOI:10.1361/mgpp2002p087 www.asminternational.org

CHAPTER 4

The Metallographer and the

Metallographic Laboratory

MATERIALS PLAY A MAJOR ROLE in the world economy ing wrought iron, wrought iron armor plate, and blister steel. He
and in the development of nations. This is particularly true of found that the samples had denite microstructural features. A
metals, with steels and cast irons being the most widely used. copy of Sorbys 1864 macrograph of blister steel can be seen in
Metals not only enhance our life-style, but have become a Fig. 4.2. This macrograph, taken at 9, shows distinct grain
necessity of modern life. Science and engineering, particularly in boundaries. This discovery was signicant, because it eventually
the areas involving metal, ceramic, polymeric, electronic, and led to the realization that microstructural features imparted certain
superconducting materials, have advanced rapidly and will con- properties to steel. The development of ferrous physical metal-
tinue to outpace technology as a whole. In this swirl of activity, a lurgy, and physical metallurgy in general, depended on this
metallographer is vital to our basic understanding of the link important link.
between microstructure and the properties of these materials. By
understanding microstructure and its origin, one can begin to
develop a basis on how to achieve specic properties tailored for
a particular engineering application. For example, an application
for an earth-moving shovel in mining requires a steel with very
high tensile strength and hardness, combined with a high degree
of wear resistance and some toughness. What optimal microstruc-
ture would provide these properties? This book provides a
beginning to the basic understanding of the development of
microstructure and gives instructions on how to employ proper
techniques to reveal microstructure, that is, the techniques of
metallography. In this book we, of course, restrict our attention to
the metallography of iron and steel.

The Metallographer
What is a metallographer? In general terms, a metallographer is
a person who has the skill to properly prepare a specimen of a
metal or alloy in order to allow examination and interpretation of
its microstructure. In this technological age, the term metallog-
rapher is becoming somewhat of a misnomer, because today it
covers not only metals but ceramics and the other materials
mentioned previously. The term at some time in the future may be
changed to materiallographer, but for the moment, the term
metallographer is still in place.
The eld of metallography, which involves the study of the
microstructure of metals, is almost a century and a half old. It all
began with Henry Clifton Sorby on July 28, 1863. Sorby, whose
photograph can be seen in Fig. 4.1, was an English geologist,
petrographer, and mineralogist who was the rst person to
examine polished and chemically etched metal samples under the
microscope. His samples included Swedish wrought iron, Bowl- Fig. 4.1 Henry Clifton Sorby, the father of metallography