Asm - Metalografia de Aço Baixo Carbono

ASM Handbook, Volume 9: Metallography and Microstructures Copyright © 2004 ASM International®
G.F. Vander Voort, editor, p588–607 All rights reserved.

DOI: 10.1361/asmhba0003761 www.asminternational.org
Metallography and Microstructures of

Low-Carbon and Coated Steels
Arlan O. Benscoter, Lehigh University
Bruce L. Bramfitt, International Steel Group, Inc.
THIS ARTICLE distinguishes low-carbon further in the article “Classification and Desig- as laminations in electrical power transformers.
steels from plain carbon and low-alloy steels de- nation of Carbon and Low-Alloy Steels” in A thin iron oxide surface layer or organic coating
scribed in the article “Metallography and Micro- Properties and Selection: Irons, Steels, and electrically insulates these steel laminations
structures of Carbon and Low-Alloy Steels” in High-Performance Alloys, Volume 1 of ASM from each other in order to minimize power
this Volume. Low-carbon steels generally contain Handbook. losses.
less than approximately 0.10% C and are used in For many critical applications, these steels are This article discusses the techniques used to
vast quantities in the automotive, appliance, and coated with metallic, organic, or oxide layers to prepare metallographic specimens of low-carbon
container industries. One of the major attributes impart corrosion resistance, cosmetic appeal, steels and coated steels. Simple and proven man-
of low-carbon steels is good formability, that is, magnetic/electrical insulation, abrasion resis- ual sample preparation techniques are described.
the ease to form a part by stamping, pressing, tance, and color. Millions of tons of low-carbon Metallographic sample preparation for low-car-
bending, stretching, and so on. In the past few sheet steel for automobiles are coated with zinc- bon steels may be only slightly more difficult
decades, there has been a swirl of activity in the base alloys for corrosion protection from road than higher-carbon steels, because of the large
metallurgy of low-carbon steels that has become salts and moisture. These zinc-base coatings in- volume percent of ferrite present in the micro-
quite sophisticated, and several new types of clude conventional galvanized low-carbon steel structure. Ferrite is soft and can be mechanically
steels have evolved. These advanced steels in- sheet where the coated layer is applied in either cold worked during sample preparation. Me-
clude ultralow-carbon steels, bake-hardenable a hot dipping (liquid bath) process or by electro- chanical cold work can be serious enough to
steels, interstitial-free steels, dent-resistant steels, plating, as in producing an electrogalvanized range from a sloppy appearance of the micro-
electrical steels, dual-phase and transformation- layer. There are also commercial hot dipped alu- structure to an artifact that leads to a complete
induced plasticity (TRIP) steels, enameling minum-zinc alloys, including Galvalume (a Zn- misinterpretation of the metallographic features.
steels, and microalloyed high-strength steels. 55% Al Ⳮ 1.6% Si alloy) and Galfan (a Zn-5% Figure 1(b) shows an extreme example of a
These steels are produced in sheet form by hot Al alloy). There is also a zinc coating called gal- poorly prepared metallographic sample of UNS
rolling continuous-cast slabs on a hot strip mill. vanneal, which is a heat treated layer of a gal- G10100 sheet. When the sheet was sheared into
When produced from a hot strip mill, the steel is vanized coating on a low-carbon steel. In some a metallographic specimen, the grains were
called hot-rolled sheet or hot band. Many low- cases, an aluminum coating called aluminized is heavily distorted, and the carbides were frac-
carbon steels are further processed on a tandem applied to protect low-carbon steel sheet for ap- tured into small particles. Figure 1(a) represents
mill or cold mill by cold rolling, where the thick- plications where moderate heat resistance is re- the same sample properly prepared. The actual
ness is reduced approximately 70 to 80% (e.g., quired. Such applications include automotive ex- microstructure consists of equiaxed (polygonal)
from 0.110 in. to approximately 0.030 in.). Be- haust systems (tailpipes, mufflers, etc.). grains of ferrite with some carbide (cementite)
cause of the cold work, the steel must be annealed The appliance industry coats ultralow-carbon on the grain boundaries. An experienced metal-
by either batch annealing or continuous annealing sheet steel with a porcelain enamel layer to pro- lographer will prepare a specimen properly to
to soften the steel and make it formable. These tect the steel from corrosion and to enhance sur- avoid artifacts in the microstructure.
latter steels are the cold-rolled sheet steels that face appeal. These enameled steels are used in The metallographic preparation of coated
comprise a huge segment of the steel market kitchen appliances (stovetops, ovens, sinks, etc.) steels requires different techniques; for example,
around the world. and in lavatory fixtures (bathtubs and sinks). The it requires the absolute necessity to maintain
In the commodity cold-rolled sheet steel mar- food industry uses organic coatings or a metallic edge integrity (flatness of the specimen and
ket, much of this steel is classified as commercial tin coating on low-carbon sheet steel containers coated edge). Coatings are usually very thin, and
quality, drawing quality, or deep-drawing qual- for beverages and food. The tin can is a classic they can be softer (zinc) or harder (enamel) than
ity. For most of these low-carbon steels, the Uni- example of a food container. The metallographic the steel base. Methods to preserve a flat edge
fied Numbering System (UNS) does not apply. techniques used for all these coatings are dis- are discussed in this article. Also, metallic coat-
For example, the UNS classified steel G10080 cussed later in this article. ings on steel, for example, zinc-base coatings,
can be marketed as several other classifications Millions of tons of very-low-carbon sheet form an electrolytic cell in the presence of water
of sheet. These classifications depend on how the steels are used in the electrical appliance and and thus develop an electrochemical reaction.
steel was produced and what chemical elements power transmission industry. Electric motors Thus, alcohol-based liquids are used in prepa-
are contained in the steel. The steel may be alu- contain hundreds of steel sheets called motor ration. Many metallographic preparation steps
minum-killed, or the steel may contain microal- laminations that are stacked and wound with require water, and thus special precautions are
loying elements such as vanadium or niobium. copper wire in the rotor and stator of the motor. needed to deal with metallic-coated steels. These
The classification of these materials is discussed Very-low-carbon 3.25% Si sheet steels are used kinds of precautions are described in this article.
Metallography and Microstructures of Low-Carbon and Coated Steels / 589
Before describing metallographic techniques, iron carbide (Fe3C), a phase called cementite. morphology of pearlite, which is a two-phase
a quick review of the various phases and con- Cementite is a hard phase and is usually not de- constituent with alternating plates of cementite
stituents found in the microstructures of low-car- sired in most low-carbon steels because it is hard and ferrite. This morphology is classic for eutec-
bon and coated steels is given as follows. and brittle and is detrimental to formability. Ex- toid transformations under slow (near-equilib-
amples of cementite in sheet steel containing rium) cooling (see the article “Invariant Trans-
0.06% C are shown in Fig. 6. The carbides range formation Structures” in this Volume). For
Microstructural Constituents from massive carbides (Fig. 6a) to smaller and example, pearlite in low-carbon UNS G10080
rounded particles (Fig. 6c). These specimens steel is seen in Fig. 8. Note the lamellar mor-
Most low-carbon steels are essentially pure were unetched in order to show the carbide morphology of the cementite in the patches of pearl-
iron (99.5% Fe) with small amounts of alloying phology (the ferrite grains are not revealed). ite. This steel was slow cooled during transfor-
elements, such as manganese, silicon, and alu- However, in these microstructures, the matrix is mation from austenite to pearlite, and the pearlite
minum, to enhance properties. In fact, many ferrite, and the cementite has nucleated and interlamellar spacing is coarse. Another example
low-carbon steels, especially the very-low- and grown on the ferrite grain boundaries. This is can be seen in Fig. 9 for a faster cooled low-
ultralow-carbon steels, are actually pure iron seen more clearly in a specimen that has been carbon steel, where dark patches of pearlite ap-
(99.99%), because carbon is at such a low level attack-etched to reveal the ferrite grain bound- pear at the ferrite grain boundaries. The lamellar
that it is considered a residual element and is no aries. An example is seen in Fig. 7, where the morphology of the cementite is not apparent in
longer required to develop the properties of the cementite particles (arrows) are on the ferrite this micrograph, because the interlamellar spac-
material. In many cases, carbon is undesirable grain boundaries. Cementite can also be revealed ing of the ferrite and cementite plates is not re-
and detrimental to the properties of highly form- in a different morphology, as described in a con- solved, even at this magnification of 1000⳯. As
able steels. This is true in steels used for enam- stituent called pearlite (discussed subsequently). seen in the next article (“Metallography and Mi-
eling. In this case, the sheet steel for enameling Pearlite. In some low-carbon steels, the ex- crostructures of Carbon and Low-Alloy Steels”),
is not called a steel but an enameling iron. In cess carbon appears in the distinctive lamellar pearlite is a major constituent in many higher-
these steels, the microstructure is 100% ferrite. carbon plain carbon steels. The morphology of
Ferrite. With very few exceptions, ferrite is pearlite is also discussed extensively in the ar-
the major constituent in low-carbon steels. Fer- ticle “Physical Metallurgy Concepts in Interpre-
rite is essentially pure iron and contains less than tation of Microstructures” in this Volume.
0.005% C at room temperature. However, it can Martensite. When low-carbon steels are
contain alloying elements such as manganese moderately alloyed and rapidly cooled from the
and silicon. An example of ferrite is seen in Fig. austenite phase field or the two-phase ferrite Ⳮ
2. In most low-carbon steels, ferrite appears as austenite field, a constituent called martensite is
an equiaxed morphology (equal dimensions in formed. Martensite is not commonly found in
all directions), as seen in Fig. 2. This form is low-carbon steels; in fact, in most cases it is
also called polygonal ferrite. Ferrite can also ap- highly undesirable. However, it is a desirable
pear in an elongated morphology in steels that and necessary constituent in some special low-
have been cold worked. Figure 3 shows a low- carbon advanced high-strength steels. These are
carbon steel that has been cold rolled 30, 50, 70, the dual-phase and steels. Islands of martensite
and 90% from the original hot-rolled (hot band) can be seen in the dual-phase steel microstruc-
thickness; for example, a 30% reduction would ture in Fig. 10. Special etchants are required to
be from 2.55 to 1.78 mm (0.100 to 0.070 in.). distinguish these martensite islands from ce-
Note how the ferrite grains are elongated and mentite particles, pearlite patches, and retained
contain deformation bands (dark lines across the austenite. In this particular microstructure, the
grains) from the cold working process. When martensite constituent is shown as dark islands,
this steel is annealed, these cold-worked ferrite whereas the uncolored islands are retained aus-
grains recrystallize into new equiaxed grains, tenite. The metallographic techniques are de-
represented in Fig. 2. Another form of ferrite is scribed later. There are special low-carbon fully
epitaxial ferrite, formed when a steel is heated martensitic high-strength steels that are em-
into the two-phase ferrite Ⳮ austenite region. An
example of epitaxial ferrite can be seen (arrows)
in Fig. 4. During cooling, new ferrite has grown
epitaxially on the existing ferrite grains. Some
dual-phase steels show eptiaxial ferrite, because
they were annealed in the two-phase region. In
very-low-carbon steel (pure iron), a substructure
called veining can be seen within the ferrite
grains. Figure 5 shows an example of veining in
pure iron.
Because of its low carbon content, ferrite is
soft and easily deformed. This means that special
care must be taken to avoid cold work and sur-
face scratches in the sample during preparation.
An experienced metallographer will prepare a
metallographic specimen without cold work or
surface scratches. Fig. 1 Microstructure of a UNS G10100 steel sheet
Cementite. When the carbon content of the showing the effect of deformation during shear-
ing of the specimen. (a) The proper microstructure of
steel exceeds the carbon solubility limit in ferrite equiaxed ferrite grains. (b) An artifact microstructure show-
(approximately 0.005 wt% C at room tempera- ing elongated grains and broken carbides at sheared edge. Fig. 2 Microstructure of equiaxed (polygonal) ferrite
ture), the excess carbon appears in the form of Marshall’s reagent. 500⳯ and pearlite (dark) in a low-carbon steel. 500⳯
590 / Metallography and Microstructures of Ferrous Alloys
Fig. 4 Microstructure of epitaxial ferrite (arrows)

formed by heating a low-carbon steel in the two-
phase ferrite Ⳮ austenite region. Marshall’s reagent. 500⳯
Fig. 3 Microstructure of a cold-rolled, low-carbon steel sheet showing ferrite grains at (a) 30%, (b) 50%, (c) 70%, and
(d) 90% cold reduction. Marshall’s reagent. 500⳯
ployed in side impact beams in doors of some gitudinal view will definitely reveal the most in- Fig. 5 Very-low-carbon steel (iron) showing large ferrite
grains with veining. Marshall’s reagent. 200⳯
automobiles. formation about a material that has been rolled.
Austenite. The austenite phase is a high-tem- This view, which is perpendicular to the surface
perature crystal structure that usually exists at and parallel to the rolling direction, more clearly shown in Fig. 13 and 14 make the point that the
temperatures above approximately 720 C (1330 illustrates the degree of grain elongation. For ex- metallographer must think before preparing a
F). However, if sufficient carbon or alloy is ample, elongated ferrite grains in hot-rolled UNS metallographic specimen for observation. The
present, a small amount of austenite can be re- G10200 steel plate are shown in Fig. 13(a), rolling or forging directions must be known so
tained at room temperature. This is the case of which represents the longitudinal view of the that the proper information is presented in the
the dual-phase steel shown in Fig. 11. This steel polished and etched specimen. The ferrite grains polished specimen. If these directions are not
was accelerated-cooled from the two-phase fer- are equiaxed in morphology but extend in long known, then the metallographer must prepare
rite Ⳮ austenite region. During initial cooling, bands, as does the pearlite (dark constituent). specimens perpendicular to each other in order
the regions of austenite were enriched with car- This morphology of ferrite and pearlite is called to determine the rolling (forging) direction.
bon as the ferrite grew and contained enough banding. Figure 13(b) affords a much different Creation of Artifacts. The metallographer
carbon (and alloy) to stabilize the austenite at view of the same plate. This is a planar view, must be careful in the selection of the proper
room temperature (i.e., the martensite start tem- where the polishing is parallel to the bands of sectioning procedure. The procedure must cause
perature was lowered to below room tempera- pearlite and ferrite. minimal damage to the microstructure from ex-
ture). Other than these special advanced high- Sometimes, there are striking differences be- cessive heat or mechanical deformation. An al-
strength steels, the metallographer should not see tween the longitudinal and transverse views of a tered microstructure is called an artifact. Any ar-
retained austenite in low-carbon steel. specimen. Figure 14(a) is a longitudinal view of tifact introduced into the microstructure points
an unetched wrought iron sample that was hand to poor metallographic practice. An artifact can
forged into a bar, showing the slag inclusions lead to misinterpretation of the real microstruc-
Metallographic Procedures (gray constituent) as elongated particles or ture hidden below the artifact. An example was
stringers in a matrix of ferrite running parallel to shown previously in Fig. 1(b). Another example
Orientation of View. Before the sample the forging axis. When viewed in the transverse is seen in Fig. 15(a), where deformation (cold
preparation of any metallographic material can plane (perpendicular to the longitudinal view in work) can be seen in a specimen that has been
begin, the metallographer must consider which Fig. 14a), as seen in Fig. 14(b), the microstruc- improperly prepared during grinding. Figure
view (longitudinal, transverse, or planar) will ture is much different. Here, the slag constituent 15(b) shows the correct microstructure.
yield the desired information. Figure 12 shows appears as rounded particles, when, in fact, we Figure 16(a) shows a low-carbon dual-phase
a sketch representing these three views. The lon- know they are actually stringers. The examples microstructure that has been altered due to me-
Fig. 6 Microstructure of a 0.06% C steel with various morphologies of cementite. (a) Massive carbides. (b) Medium-sized carbides. (c) Small, dispersed carbides. 4% picral etch.
1000⳯
chanical deformation during shearing, creating a Specimen Preparation gravity diamond saw, and wire saw. The micro-
microstructural artifact. As described previously, structure is more vulnerable to alteration during
the microstructure of a dual-phase steel should Sectioning. Generally, a sample to be metal- sectioning than in any other metallographic
consist of islands of retained austenite and mar- lographically examined must be sectioned to a preparation step. However, as mentioned previ-
tensite in a ferrite matrix. In the microstructure convenient size before performing the prepara- ously, damage to the specimen during sectioning
shown in Fig. 16(a), the severe cold working tion steps to reveal its microstructure. Methods can alter the microstructure. Those surface arti-
during shearing transformed the retained austen- to be considered, in the order of descending level facts, created by excessive heat or mechanical
ite to martensite, as seen in Fig. 16(b). The re- of degradation of the microstructure, are as fol- deformation, can normally be removed by rough
tained austenite of this particular grade of steel lows: acetylene cutting torch, plasma torch, elec- grinding.
is fairly stable at room temperature and can even trical discharge machining (EDM), shear, band Oxyacetylene torch, plasma torch, and EDM
exist at temperatures as low as ⳮ200 C (ⳮ330 saw, abrasive cutoff machine, high-speed cutoff, cutting all leave a melted and heat-affected zone
F) without transforming to a martensite, yet it that must be removed by further sectioning by a
can be readily transformed by mechanical defor- less aggressive method before the sample is
mation. This is a subtle example, but the met- mounted. If a sample is cut using an oxyacety-
allographer must be cognizant that sample prep- lene torch, approximately 50 mm (2 in.) of ma-
aration itself can alter the microstructural terial needs to be removed before getting to an
constituents in ways that can mislead a person unaffected area. Plasma cutting leaves a much
in the interpretation of the true microstructure. smaller heat-affected zone. Many metallogra-
Fig. 8 Microstructure of a slow-cooled UNS G10080

Fig. 7 Cementite (arrows) at ferrite grain boundaries in steel showing pearlite islands in a ferritic matrix. Fig. 9 Microstructure of a normalized UNS G10080
a batch-annealed 0.04% C steel. Marshall’s re- The lamellar morphology of the pearlite is resolved. 4% steel showing unresolved pearlite islands in a fer-
agent. 500⳯ picral etch. 500⳯ ritic matrix. 4% picral etch. 1000⳯
Fig. 12 Sketch showing the three planes of rolling. RD,

rolling direction
There are many abrasive wheel cutting ma-

chines available that range from small, gravity-
fed models using 100 mm (4 in.) diameter
wheels to large floor models with 355 mm (14
in.) diameter wheels 1.5 mm (1⁄16 in.) thick. Steel
Fig. 10 Microstructure of a dual-phase sheet steel with Fig. 11 Microstructure of a dual-phase sheet steel with
islands of martensite in a matrix of ferrite. 4% islands of martensite (dark) and retained aus- samples should be sectioned using alumina
picral etch. 500⳯ tenite (arrows) in a matrix of ferrite. 12% sodium metabi- (Al2O3) wheels of the proper rubber-bonded
sulfite tint etch. 1000⳯ hardness. The specimen is kept cool during cut-
ting by an ample flow of water; cutting also can
phers do not realize that an EDM cut has a heat- be performed with the specimen submerged in
affected zone that must be removed. The depth in Fig. 17(b) was sectioned using a band saw and the coolant. The appropriate wheel hardness
of the zone depends on the EDM parameters. shows that the ferrite grains have deformed at should be selected and the proper force applied
Generally, the metallographer must use caution the cut surface. Figure 17(c) was obtained by during cutting. Manufacturers have developed
and common sense when preparing metallo- shearing, and the deformation of the ferrite different kinds of wheels, ranging from a soft
graphic specimens from these sectioning grains is extensive. bond that readily deteriorates and exposes fresh
methods. Al2O3 particles needed for cutting hard speci-
Sectioning using a low-speed band saw or mens, to hard-bonded wheels that break down
power hacksaw can be slow and tedious. The slowly. The latter are preferred for softer mate-
specimen should be softer than 35 HRC for the rials (low-carbon steels).
saw to be effective, unless a special bi-metal
blade is used. The resulting surface is rough and
generally uneven if manually fed. Using oil or
water-soluble oil as the cutting fluid can mini-
mize the frictional heat generated. The cutting
fluid also prolongs the life of the saw blade by
preventing tempering of the teeth.
Shearing thin specimens on a tabletop hand
shear is a quick method of sectioning. However,
shearing results in extreme mechanical defor-
mation at the shear burr. Care must be taken to
remove the deformation zone by rough grinding.
If the sheared specimen is mounted in epoxy or
a thermosetting material, the thickness of the
mount should be measured to ensure that the de-
formed material is removed during grinding. An
artifact microstructure caused by mechanical de-
formation as the result of shearing a dual-phase
steel was previously shown in Fig. 16. The de-
formation produced during shearing can also be
seen in Fig. 17(c)
Abrasive wheel cutting is another common
method of sectioning steel samples. Most metal-
lographic laboratories have an abrasive wheel
device. Abrasive wheel cutting, if properly exe-
cuted, is, by far, the best technique for obtaining
a steel specimen surface that is smooth, has min-
imal deformation, and has minimal microstruc-
tural changes caused by overheating. Examples
of surface deformation in a UNS G10100 hot-
rolled steel specimen after abrasive wheel cut-
ting, band saw cutting, and shearing are shown
using dark-field illumination in Fig. 17. Figure
17(a) is a cross section illustrating the minimal Fig. 13 Microstructure of an as-rolled UNS G10200
depth of deformation caused by sectioning with
steel showing elongated bands of pearlite Fig. 14 Microstructure of forged wrought iron showing
(dark) and ferrite grains. (a) Longitudinal plane. (b) Planar slag stringers in a ferrite matrix. (a) Longitudinal
an abrasive cutoff wheel. The specimen shown view. 4% picral etch. 100⳯ plane. (b) Transverse plane. As polished. 100⳯
Care must be taken when cutting with an abra- tion that, when mixed together and heated to 70 ● 170 g CuSO4•5H2O
sive wheel. If the specimen is not properly se- to 80 C (160 to 180 F), forms a electroless ● 60 g H2SO4 (concentrated)
cured with a clamp, the wheel is likely to break. nickel coating. The nickel layer will plate out at
with a solution temperature at 15 to 50 C (60 to
A steady, firm pressure must be maintained a rate of 10 lm/h on the specimen surface. A
120 F), plating is done at 1 to 4 V, with a current
against the specimen. Careless use of an abrasive solution for electroless nickel coating can also
density of 10 to 20 mA/cm2. Agitation by mild
cutoff machine, even with coolant capability, can be prepared in the laboratory by adding the fol-
stirring is preferred, and use a copper anode.
result in artifacts, as depicted in Fig. 18. In this lowing chemicals to 1 L of water:
A second technique is to place a dummy steel
example, too much force and insufficient coolant ● 37.3 g NiSO4 (nickel sulfate) specimen as close as possible to the edge of in-
caused the steel specimen to heat above 720 C ● 26.4 g NaH2PO2 (sodium hypophosphite) terest; this will minimize the degree of rounding
(1330 F) at the surface. The metallographically ● 15.9 g sodium acetate during polishing. A third technique involves
prepared surface exhibits structures of martensite ● 5 to 6 drops H2SO4 (sulfuric acid) placing stabilizers (small steel pieces) every 90
in a ferrite matrix (Fig. 18a), islands of marten- around the specimen. A fourth method to main-
site surrounded by fine pearlite (Fig. 18b), and Some specimens with coatings such as zinc-
tain a flat edge can be accomplished by adding
islands of very fine pearlite in a ferrite matrix coated steel sheet (Galvalume, galvanneal, or
alumina particles to an epoxy mixture prior to
(Fig. 18c). The micrographs display scratch-free, galvanized) must first have a copper flash coat-
casting; this filler material can be purchased
well-defined microstructures, but all are artifacts. ing before the nickel layer, because the aqueous
through most metallographic supply houses. The
The true microstructure shown in Fig. 18(d) is a electroless nickel plating solution will attack the
alumina filler material is approximately 50 lm
coarse pearlite and carbide structure in a ferrite coating. The formula for a copper flash coating
matrix and was revealed after regrinding and re- and other plating solutions can be found in Ref
polishing the specimen. The artifact microstruc- 1. The chemical formula and technique for cop-
tures in Fig. 18(a) to (c) were caused by frictional per flash plating is to first add the following to
heating from insufficient cooling during the 1 L of water:
abrasive wheel cutting process. The patches of
coarse pearlite (original microstructure) were
heated into the austenitizing temperature range
during cutting, and rapid cooling created the
martensite and fine pearlite after the cutting
stopped.
Mounting. Not all metallographic specimens
must be mounted before examination. A bulk
specimen that is convenient to handle can be suc-
cessfully prepared and examined at magnifica-
tions up to 1000⳯. This requires beveling the
edges to prevent tearing or catching of the pol-
ishing cloths, which can cause an uneven sur-
face. However, most metallographic specimens,
particularly sheet specimens, are mounted in
castable epoxy, thermosetting resin, or a steel
clamp for ease of preparation.
Various considerations must precede the
mounting of a specimen, such as the use of an
etchant to reveal the microstructure that may also
attack the mounting medium. For example, al-
kaline sodium picrate (used to darken cementite)
attacks phenolic thermosetting resin mounts.
Thermosetting epoxy mounts are recommended
when etching with alkaline sodium picrate.
In addition, examination of a specimen edge
for decarburization, carburization, internal oxi-
dation, depth of oxide scale, coating thickness,
and so on will require a mounting material with
minimal shrinkage properties, such as castable
(liquid) epoxy resin or thermosetting epoxy
powder. Further, if an oxide scale is to be ex-
amined, a compression-mounting resin may get
in between and separate the scale from the base
material during pressure molding of the mount.
If edge retention is important, it is advisable
to closely match the polishing rate of the mount
material with that of the specimen. However, in
most cases this is not possible, and therefore, a Fig. 16 Microstructure of a dual-phase steel sheet
(0.11% C, 1.4% Mn, 0.58% Si, 0.12% Cr, and
number of different ways must be considered to 0.08% Mo) showing islands of martensite (dark gray), pearl-
maintain a flat edge. One possible way is to plate ite (black), and retained austenite (white; see arrows) in a
the surface with nickel (see the article “Mount- Fig. 15 Microstructure of a low-carbon steel showing matrix of ferrite. (a) In as-cooled condition. (b) Same spec-
the effect of improper grinding. (a) Scratches imen but in deformation zone from shearing. In (b), the
ing of Specimens” in this Volume). Some me- and deformation left on surface from previous grind. (b) The retained austenite transformed to martensite. 12% sodium
tallographic supply houses sell a two-part solu- true microstructure. 2% nital etch. 200⳯ metabisulfite tint etch. 1000⳯
in size and very porous, to allow the epoxy to ing was forced away from the base. In Fig. 19(b), microstructure or when pressure may disturb a
penetrate and hold it in place. However, this sys- the same sample was mounted using a castable fragile surface condition, as mentioned previ-
tem will produce a metallographic mount that epoxy, and the nickel coating is intact. Artifacts ously. A common technique used for castable
cannot be ground with silicon carbide papers, caused by improper mounting techniques are al- mounts is to glue a phenolic or aluminum ring
thus requiring a diamond disc for grinding, and ways permanent, and the sample is no longer form to a sheet of aluminum foil (the epoxy will
that can only be polished with diamond com- representative of the original specimen. not adhere to the aluminum foil) supported by a
pounds, except for the final polish with silicon Figure 20(a) shows that the pressure required glass plate or thin sheet steel. Plastic or rubber
dioxide. for mounting can physically damage the thin molds can also be used. The specimen is placed
Mounting methods can cause damage to the sheet steel specimens in a thermosetting resin face down in the ring. For sheet specimens, a
specimen, due to heat and pressure needed to mount. The sheet specimens were separated by steel or plastic clip can be used to hold the spec-
cure a thermosetting resin or thermoplastic steel spacers, and the high pressure that devel- imens upright. After the epoxy is poured into the
mount. Figure 19(a) illustrates the damage oped during the mounting process caused the mold, a vacuum is used to remove air bubbles
caused by the high pressure needed to process a specimens to deform. Similar specimens in the trapped in small cracks and crevices in the spec-
thermosetting resin mount. The electroless castable epoxy mount (Fig. 20b) show no dam- imen; it will also remove bubbles introduced
nickel layer that was plated on a low-carbon steel age. during mixing.
sheet has separated from the teel. The mounting Castable Mounting Materials (Epoxy). For If an epoxy mount does not completely cure
compound becomes fluid during the heating ease of preparation, many metallographers due to improper mixing or due to an incorrect
stage, then, at the high pressure of 30 MPa (4200 mount their specimens in castable epoxy. Epoxy ratio of resin to hardener, this condition can be
psi) needed to compact the compound, the coat- mounts should be used when heat may affect the corrected if the mount, after setting up, is placed
Fig. 17 Microstructures of a hot-rolled UNS G10100 sheet steel showing sectioning damage from (a) an abrasive cutoff wheel, (b) a band saw, and (c) from a shear. Marshall’s
reagent. Dark field illumination. 400⳯
Fig. 18 Artifact microstructures in (a), (b), and (c) that developed by heating the specimen during sectioning on an abrasive cutoff wheel. (a) Tempered martensite (gray) in a ferrite
matrix (white). (b) Tempered martensite (gray) and pearlite (dark) in a ferrite matrix (white). (c) Pearlite (dark) in a ferrite matrix. (d) The true microstructure consisting of
islands of very coarse pearlite (gray) in a ferrite matrix. 4% picral etch. 1000⳯
in an oven at 65 C (150 F) for 4 h. Mounts recessed approximately 6 mm (0.25 in.). Epoxy by the tape; the mount is placed in a vacuum for
larger than 38 mm (1.5 in.) in diameter should is then poured into the recess to a depth of ap- several minutes, purged several times, then al-
be placed in a refrigerator until they have set up, proximately 1.5 mm (0.0625 in.), and a vacuum lowed to cure.
to prevent an exothermic reaction; otherwise, is used to remove air from the voids, allowing Steel Clamp. Using steel clamps to mount
stresses resulting from such a reaction may cause the epoxy to flow between the compression me- specimens is very rapid and versatile. Multiple
the large mass of epoxy to crack. dium and the specimen. sheet, small bulk, and wire specimens can be se-
Another possible application of epoxy is ex- In using castable epoxy mounts in the scan- cured with clamps. The main disadvantage of
amination of a surface condition obscured by the ning electron microscope or electron probe mi- this technique is that a clamp mount must be
mounting medium. An example is shown in Fig. croanalyzer, electron charging can be minimized ultrasonically cleaned to remove debris after the
21. The coating material is a zinc powder mixed by adding an electrically conductive material to final grinding and after each polishing step.
with a polymer. The coating is covered with a the epoxy. For example, graphite powder (4.5 g Clamp mounts are shown in Fig. 23. The clamps
layer of black paint. If the specimen is mounted per 15 g of epoxy) can be added for conductivity. are usually fabricated of 3 to 6 mm (0.125 to
in an opaque mounting material (e.g., thermo- However, caution must be used so that the ad- 0.25 in.) thick UNS G10200 steel plate. For best
setting resin), it is very difficult to distinguish ditive does not contaminate the specimen. results, try to match the hardness of the clamp
the black paint layer from the mounting material. Thermosetting Mounting Material. Ferrous material with the hardness of the specimen. Each
This is illustrated in Fig. 21(b). Even in an epoxy specimens for routine examination are often clamp is approximately 13 mm (0.5 in.) wide and
mount, the transparent mount absorbs the re- mounted in a thermosetting material (phenolic 25 to 50 mm (1 to 2 in.) long, with holes at each
flected light from the microscope. However, if resins such as Bakelite). A mounting press is re- end. One half is threaded to receive a bolt, and
the specimen is lighted from the back or side of quired to soften and force the mounting material the other half has a mating hole through which
the mount, the edge of the black paint can be around the specimen. The specimen is placed on the bolt can pass.
clearly seen, as in Fig. 21(a). the steel insert of the pressure cylinder. Remem- Mounting with clamps involves placing the
If edge retention (edge flatness) is important, ber that the specimen(s) can move during this specimen or specimens so that enough material
a steel dummy sheet can be placed next to the mounting process. There are metal and plastic protrudes from the clamp to ensure adequate re-
sample edge to be examined. This will prevent clips that can be used to keep sheet specimens
rounding of the edge facing the dummy. An ex- upright. The dry powder is measured and placed
ample where edge retention is important is on top of the specimen. A steel piston is then
shown in Fig. 22, where a thin layer of the steel placed into the cylinder, and the cylinder is
has been penetrated by oxidation. This condition heated and pressurized. The powder should be
is called internal oxidation, and it occurred in free of moisture, and sharp corners on bulk spec-
this silicon-bearing electrical steel because sili- imens should be rounded when possible. Follow
con is less noble than iron and is preferentially the instructions of the mounting press manufac-
oxidized. For very hard specimens (usually not turer and read the safety warnings. The mount
the case for low-carbon steels), it is advisable to should be cooled before ejection from the mold.
mix aluminum oxide spheres into the epoxy liq- If ejected too hot, the mount may crack.
uid. These particles add hardness to the final Bakelite or similar thermosetting materials
cured mount. can be used to mount any gage wire by first pre-
Castable epoxy can also be used to salvage paring a blank mount, then drilling holes slightly
compression mounts having voids between the larger than the wire. The wire is placed into the
specimen and mount, which causes the etchant holes, and masking tape is wrapped around the
to bleed onto the specimen. Masking tape is mount, extending approximately 6 mm (0.25 in.)
wrapped around the mount, leaving the mount above it. Epoxy is poured into the recess created
Fig. 20 Six low-carbon steel sheet specimens, sepa-

Fig. 19 A low-carbon steel sheet plated with electroless nickel showing (a) damage to the coating from mounting in rated by steel spacers, showing (a) damage
a thermosetting phenolic resin and (b) the lack of damage when mounted in a castable epoxy. As-polished. from mounting in a thermosetting phenolic resin and (b)
100⳯ lack of damage when mounted in a castable epoxy
moval during grinding of any deformation zone Grinding. As previously mentioned, regard- grit sizes). Silicon carbide papers should be used
caused by sectioning. Once secured, the two less of the type of equipment used to section a to prepare ferrous materials. The first grit size
bolts are then tightened, and the clamp with sample, surface damage will be present to some that is selected depends on the sectioning
specimen(s) is secured in a vise, after which the degree. Always keep in mind that grinding, like method used in preparation of the specimen. The
bolts are tightened further. This will minimize sectioning, creates a zone of deformation on the larger the grit-size numbers, the finer the particle
seepage. specimen surface. The sketch in Fig. 26 illus- size on the grinding paper. For example, a band-
An example of a microstructure of a low-car- trates the deformation zone that is created during saw-cut or sheared surface may require an 80-
bon steel specimen mounted in a clamp is shown grinding. A series of grinding steps, using suc- grit paper, followed by 120-, 240-, 320-, 400-,
in Fig. 24. In this micrograph, the clamp material cessively finer-grit silicon carbide papers, must and 600-grit papers, and a specimen sectioned
is shown at the top. Note that a flat surface is be used to remove most of the damaged layer using an abrasive wheel may require starting
maintained at the very edge of the specimen. and to produce a flat surface having minimal de- with a 320-grit paper (skipping the 80- and 240-
This is called edge retention and is very impor- formation (see Table 1 for a listing of standard grit papers). During grinding, water must be used
tant if the microstructural features at the edge are to flush the abrasive disk and keep the specimen
to be observed or if the steel has a coating. Edge cool. The exception is when water-soluble par-
retention is also maintained when several sheet ticles (for example, aluminum nitrides) are pres-
specimens are stacked within a clamp, as shown ent in the specimen. If water-soluble particles are
in Fig. 25. The butting edges of the two speci- present and require examination, mineral spirits,
mens in this micrograph show excellent edge re- kerosene, or commercial lapping oil that does
tention. not contain water must be used during grinding.
To obtain a flat surface with minimal defor-
mation, the specimen should be held with the
fingertips as close as possible to the grinding pa-
per. By using a moderately heavy pressure,
slowly move the specimen back and forth from
the center to the edge of the grinding disk. The
specimen surface should be examined periodi-
cally to determine when scratches from the pre-
vious grinding have been removed. Grinding
should continue two to three times longer than
the time required to remove the scratches from
previous operations. This will ensure elimination
of the deformed zone. If a bevel or facet occurs
Fig. 22 Internal oxidation penetrating the surface of a during grinding, the pressure point should be
motor lamination steel. Not only have oxides
formed in the grain boundaries, but fine oxides have
changed. For example, more pressure can be ap-
formed in the matrix. 4% picral etch. 1000⳯ plied with the thumb and less with the fingers,
or conversely. Grinding should proceed using the
abrasive on which the facet occurred or the pre-
vious grit paper; a finer grit should not be used
until the surface is flat. The specimen should be
rotated 90 between steps. This will allow the
metallographer to see if the scratches from the
previous grinding paper were removed during
the current step.
If the specimen—whether mounted or un-
mounted—is not square, the grinding sequence
Fig. 21 A zinc-particle polymer coating (Zincrometal)

with a top paint layer on a low-carbon steel
sheet showing (a) the extent of the top paint layer, using Fig. 24 Microstructure of a low-carbon steel sheet
transmitted light through a castable epoxy mount, and (b) mounted in a steel clamp. The clamp is at the
the difficulty of seeing the paint layer in a normal brightfield Fig. 23 Steel clamps used to mount tubular and sheet top. Note the excellent edge retention of the steel sample.
illumination (reflected light). As-polished. 200⳯ specimens Marshall’s reagent. 500⳯
should be planned so that the longest length is ally, the metallographer will know when the polishing times and an etch after each polishing
parallel to the direction of wheel rotation in the specimen is prepared properly. For example, step. Low-carbon steel specimens can be pol-
final grinding step; otherwise, the specimen can careful observation of the ferrite grains in Fig. ished using 6 lm diamond on a canvas or low-
rock, causing an uneven or rounded surface. 28 shows that the scratches from the last grind- nap cloth for 1 min with heavy pressure. This is
When changing papers, the wheel should be ing step were not removed. The ferrite phase in followed by 3 lm alumina for 2 min with firm
moistened with water to prevent slippage of the this ferrite Ⳮ pearlite microstructure is very soft, pressure on a medium-nap cloth. Use a low-
paper while grinding. and the scratches and associated deformation speed polishing wheel while rotating the speci-
Flushing of the specimen before proceeding zone are still present. When this is seen, the spec- men clockwise (the opposite direction to wheel
to the next step will prevent contamination of the imen needs to be repolished, or the specimen rotation).
succeeding grinding papers. After final grinding, should be reground on a 600-grit paper. Polish- If a water-soluble diamond compound is used,
all specimen surfaces should be cleaned with ing techniques for steel specimens depend on the specimen should be cleaned after polishing
cotton and water, flushed with alcohol, and then their microstructure. For a specimen with a with a good grade of natural cotton and water,
dried. Never allow water to sit on the surface of pearlite or carbide microstructure, polishing flushed with alcohol, then dried. The specimen
a ground (or polished) specimen between prep- times should be short and steps few to minimize should then be polished on a stationary wheel
aration steps, because corrosion will begin im- relief. A specimen in which the ferrite grain using a medium-nap cloth and a colloidal sus-
mediately. Clamp-mounted specimens should be boundaries are to be etched would require longer pension of 0.04 lm silicon dioxide (SiO2). If an
cleaned with cotton and water, ultrasonically
cleaned with alcohol, and dried.
An example of artifacts caused by improper
grinding was shown previously in Fig. 15. Fig-
ure 15(a) depicts the result of proceeding to the
next grinding step too soon. The scratches from
the previous step have not disappeared, and ran-
dom lines, mottled surface, and obscured grain
boundaries are visible. When this occurs, the
specimen must be reground to remove the arti-
facts. Figure 15(b) illustrates the same specimen
after correct grinding. Deformation caused by
grinding can also alter the microstructure.
Figure 27 shows the effect of grinding on re-
tained austenite in a dual-phase steel. The 25 by
50 mm (1 by 2 in.) specimen was planar polished
for x-ray diffraction, using a new paper for each
grinding step; it was then polished using 6 lm
diamond. X-ray diffraction revealed the presence
of 7.8% retained austenite. Repetition of the ex-
periment using worn papers resulted in a much
lower austenite count. The two chemically pol- Fig. 27 A histogram showing the amount of retained
ished planes were used as a standard. Both austenite present in a dual-phase steel after
planes that were polished using worn papers regrinding with new and worn grinding papers. The two bars
for chemical polish represent the true percentage of re-
sulted in the austenite transforming to martensite Fig. 26 Sketch showing depth of grinding scratches be- tained austenite in the specimen. The lower percentages,
due to mechanical deformation. low the surface of a specimen from grinding with worn papers, indicate that much of the
Polishing is the last mechanical step, and its retained austenite transformed to martensite due to me-
purpose is to remove the scratches and the sur- chanical deformation.
face deformation zone created by grinding. Usu-
Table 1 Grit sizes for metallographic
grinding papers
European grit No. U.S. grit No. Approximate particle size,
(FEPA) (ANSI/CAMI) lm
Standard sizes
P-60 60 250
P-80 180
P-120 120 125
P-180 180 75
P-220 63
240 59
P-320 46
320 41
P-500 30
400 26
P-800 22
P-1000 18
P-1200 600 15
Finer sizes
P-2400 800 8
P-4000 1200 3 Fig. 28 Microstructure of an ASTM A36 structural steel
showing ferrite Ⳮ pearlite. Note the remnants
Fig. 25 Two low-carbon sheet specimens butted to- FEPA, European Federation of Abrasive Particles; ANSI, American Na-
tional Standards Institute; CAMI, Coated Abrasives Manufacturers In-
of scratches in the softer ferrite phase. These subsurface
gether in a steel clamp. Note the excellent edge deformation zones from grinding (as shown in Fig. 26) were
retention of both specimens. Marshall’s reagent. 500⳯ stitute not removed in the polish. 2% nital etch. 100⳯
adhesive-backed cloth is used, a thick glass or example, SiO2 drying on the specimen can some- vanized, the zinc coating would not adhere to
plastic plate can be substituted for the wheel. If times appear as coarse pearlite. A commercially this portion of the sheet, and a coating defect
the specimen contains 1.0% Si or more (electri- available free-standing blow dryer (the type would form. If good edge retention procedures
cal steels, dual-phase and TRIP steels), the SiO2 found in most restrooms) works well on metal- were not followed, the metallographer may have
polishing compound should be cleaned off with lographic specimens because of the large volume missed these carbides on the surface. In this ex-
denatured alcohol and cotton to prevent staining; of warm air it produces. ample, a higher-hardness thermosetting mount-
otherwise, the specimen should be cleaned with During both grinding and polishing, it may be ing material was used to minimize rounding of
water, flushed with alcohol, and dried. Figure 29 important to preserve the edge of the specimen, the edge of the specimen.
shows a silicon-containing electrical steel spec- that is, maintain a flat surface right up to the Etching. The specimen should be etched im-
imen that was polished using this procedure. edge. If precautions are not taken, the edges on mediately after the final polishing. Etching so-
A specimen in which the ferrite grains are to a metallographic specimen are rounded, and the lutions used to reveal the microstructures of low-
be revealed can be polished 1 min using a low- edge is not in focus on the same plane as the carbon and coated steels are listed in Table 2 and
speed wheel and 6 lm diamond on a low-nap bulk of the specimen surface. An example where 3, along with their primary characteristics. Nital
cloth. The specimen is then etched 15 s in 2% edge retention is important is shown in Fig. 31, and picral are the most widely used etchants for
nital, repolished 2 min using 0.3 lm Al2O3 on a which represents the outer surface of a low-car- low-carbon steels.
medium-nap cloth and a low-speed polishing bon steel sheet with carbides (cementite) on the Nital is generally used in concentrations of 1
wheel, re-etched 15 s in 2% nital, and repolished surface. A planar view (looking at the sheet sur- to 3% nitric acid (HNO3) in ethanol or methanol.
1 min using 0.3 lm Al2O3. The final polishing face) of similar carbides can be seen in Fig. 32. In solutions containing more than 5% HNO3,
should be carried out with SiO2 for 30 s on a The carbides formed from surface contamination only methanol should be used, because the eth-
stationary medium-nap cloth. After each step, of carbon during the batch annealing process. If anol becomes unstable as the concentration of
the abrasive should be removed with cotton and the sheet from this batch anneal was to be gal- HNO3 increases. However, for the lower concen-
water and the specimen flushed with denatured trations, ethanol is preferred, because methanol
alcohol, then dried immediately. This etch-pol- is toxic and can be absorbed through the skin.
ish-etch technique will remove the deformed An example of a low-carbon steel etched with
layer.
Nonmetallic inclusions can be retained by pol-
ishing with 6 lm diamond on a stationary nap-
less cloth, then 1 lm diamond on a low-nap cloth
for 1 min. After each polishing, the specimen
should be cleaned with denatured alcohol and
cotton, flushed with alcohol, and dried.
The following procedures will keep speci-
mens flat and free of polishing artifacts during
polishing. The edges of a clamp, mount, or bulk
specimen should always be beveled to prevent
catching on the polishing cloth, which can result
in a rounded surface. Beveling also prevents
tearing of the cloth. The specimen should always
be rotated counter to wheel direction to avoid a
comet tail effect, as shown in Fig. 30(a). Figure
30(b) illustrates the same specimen polished cor-
rectly. Comet tails are developed when inclu-
sions are literally pulled from the specimen sur-
face. In the pulling process, the inclusions leave
a tail in the direction they were pulled. Fig. 31 Surface cementite (arrows) on a low-carbon
batch-annealed sheet. This specimen was pre-
Polishing abrasives should be removed from pared with excellent edge retention. 4% picral Ⳮ zephiran
the specimen as quickly as possible to prevent chloride wetting agent. 1000⳯
them from drying and causing an artifact. For
Fig. 30 A decarburized UNS G10100 steel sheet

showing (a) comet tails from improper polish-
Fig. 29 Microstructure of a fully decarburized motor ing and (b) the true microstructure. A comet tail is produced Fig. 32 Large surface carbides shown in a planar view.
lamination steel showing large ferrite grains. when inclusions (manganese sulfides) are pulled from the Marshall’s reagent. 100⳯. Courtesy of Samuel
Marshall’s reagent. 200⳯ surface of the specimen. As-polished. 100⳯ Lawrence, International Steel Group
2% nital can be seen in Fig. 33. The nitric acid shall’s reagent (Fig. 36b) delineated all the ferrite but it highlights carbide boundaries. An example
in this etchant chemically attacks the ferrite grain boundaries, whereas the 2% nital (Fig. 36a) can be seen in Fig. 38, where several cementite
grains and is thus an “attack” etchant. The grain only delineated a few boundaries. The micro- particles (arrows) are easily visible on the ferrite
boundaries are delineated, because each ferrite graphs in Fig. 37 show a low-carbon steel etched grain boundaries.
grain has a different orientation with respect to in Marshall’s reagent, where the ferrite grain size Tint Etchants. Ferrite grain boundaries in low-
the plane of polish. The boundaries between the is duplex. This is an example where two micro- carbon, 1% Si, and titanium-bearing steels are
grains can be seen, because the reflected light graphs were required to qualitatively represent difficult to delineate. In this case, Beraha’s tint
from the light microscope is scattered and not the microstructure because of the large variabil- etchant will differentiate the grains by color. Fig-
returned back through the objective of the mi- ity in ferrite grain size and distribution. Looking ure 39 shows ferrite grains tinted with Beraha’s
croscope. at only one field in the microscope would have reagent. This specimen represents a very-low-
Picral generally consists of a 4% solution of been very misleading and would not have told carbon motor lamination steel containing silicon.
picric acid in ethanol. This etchant highlights the the whole story about the microstructure. Tint etchants such as Beraha’s or sodium meta-
boundaries around carbides and is thus used Another advantage of Marshall’s reagent is bisulfate (Na2S2O5) should not be agitated; the
when there are carbides present in the micro- that it not only sharpens ferrite grain boundaries, specimen should be pre-etched 2 to 3 s in picral
structure, for example, pearlite or cementite par-
ticles. An example of a specimen etched in 4%
picral is seen in Fig. 34. In this case, cementite
particles are clearly delineated from the ferrite Table 2 Common etchants for low-carbon steels
matrix. Note in this example that the picral etch
Etchant Ingredients Applications/remarks
did not delineate the ferrite grain boundaries.
Four or five drops of 17% zephiran chloride 2% nital 1–5 mL nitric acid (conc) Used to reveal ferrite grain boundaries and lath
99 to 95 mL ethyl alcohol martensite (low carbon)
per 100 mL of 4% picral solution will hasten the The authors recommend a 2% solution with an etching
etching reaction and prevent preferential attack. time of 10 to 20 s. Use gentle agitation, with the
Picral works best when it turns dark with use. polished surface upward. To reveal all ferrite
Etching times generally range from 15 to 30 s, boundaries, the last polishing step should be with
silicon dioxide for at least 1 min and etched
with the polished face held upward. The speci- immediately to prevent a passive layer from
men should be held with tongs and agitated forming on the polished surface.
gently. After etching, the specimen should be Marshall’s reagent Part A: For ferrite grain boundaries (more uniform than nital).
held under water to remove excess etchant, 5 mL sulfuric acid (conc) Colors cementite tan. Reveals prior-austenite grain
8 g oxalic acid boundaries in martensitic low-carbon steels
flushed with denatured alcohol, and dried. If the 100 mL water Can pre-etch in 2% nital for better results. Hold
water causes stains—for example, in steels con- Part B: polished surface vertical in solution to avoid pitting.
taining more that 1% Si—the etching solution 30% solution hydrogen peroxide Add 1 mL hydrofluoric acid per 100 mL of solution
should be removed by placing the specimen in a Part A can be mixed and stored, but for deeper etching response, especially in
do not store the mixture of parts A interstitial-free steels. If a haze covers the surface,
sequence of alcohol baths, flushing with alcohol, and B. Part B must be used fresh. immerse specimen in a 3% aqueous EDTA(a)
and drying. Keep in mind that picric acid crystals Mix equal parts (A and B) just solution in an ultrasonic cleaner for several minutes,
in their dry form are highly explosive. Always before using. flush with water, then alcohol, and blow dry.
keep the crystals moist and stored in a special 4% picral 4 g picric acid For structures consisting of ferrite and carbides (and
96 mL ethyl alcohol pearlite). For bainitic steels and tempered martensite
storage cabinet. Maintain safe procedures when 5 mL zephiran chloride (wetting Does not reveal ferrite grain boundaries
handling this compound. As a standard practice, agent) per 75 mL of solution For pearlite and carbides, usually etch for 20 s
the metallographer should always check the Ma- The addition of zephiran chloride improves etch rate
terial Safety Data Sheet information that accom- and uniformity.
Etchant improves with age
panies each chemical reagent. For chromium-bearing steels (above 0.5% Cr), add 5
Picral Ⳮ Nital. A serial etch of 4% picral and drops of hydrochloric acid per 100 mL of solution.
2% nital is sometimes used to delineate both the 4% picral Ⳮ 2% nital 4 g picric acid For ferrite plus carbide (pearlite) structures and ferrite
ferrite grain boundaries and the carbide particles. 96 mL ethyl alcohol plus bainite or martensite
5 mL zephiran chloride Etch first in picral followed by nital, or mix the two
The specimen is etched using picral, then nital. solutions. Either technique produces good results.
This technique is useful for etching ferrite grain 2 mL nitric acid (conc)
boundaries in a pearlite-ferrite microstructure 98 mL ethyl alcohol
without overetching the pearlite. Etching times Sodium metabisulfite 10 to 12 g sodium metabisulfite Tint etch. Darkens martensite in quenched steels and
100 mL distilled water dual-phase steels
are 10 to 15 s in 4% picral and 5 to 10 s in 2% Pre-etch for 3 s in 2% nital
nital. Immerse in solution for 20 s. Etch, with polished
Marshall’s Reagent. Ferrite grain boundaries surface facing upward, for 45 s and do not agitate.
can be etched using nital in most steels, although If over- or underetched, the specimen must be
repolished, which can be done in approximately 15
Marshall’s reagent appears to be the better etch- s with 0.3 lm alumina.
ant for low-carbon and decarburized steels. A Beraha’s reagent 10 g sodium thiosulfate (anhydrous) Tint etch. For ferrite grain boundaries
0.02% C steel etched in Marshall’s reagent can 3 g potassium metabisulfite Pre-etch for 3 s in 2% nital for better results. Etch,
be seen in Fig. 35. Note the sharpness and com- 100 mL water with polished surface facing upward, for 45 s and
do not agitate. If over- or underetched, the specimen
pleteness of the ferrite grain boundaries. This is must be repolished.
one advantage of Marshall’s reagent over nital, Klemm’s reagent 50 mL water saturated with sodium Tint etch. Colors ferrite grains and ferrite in pearlite
in that it delineates all the ferrite grain bound- thiosulfate Etching time, 40–120 s
aries in a low-carbon steel. This would be par- Add 1 g potassium metabisulfite
Alkaline sodium picrate 2 g picric acid Solution will darken pearlite and iron carbides.
ticularly important when measuring ferrite grain 25 g sodium hydroxide Add sodium hydroxide to water; when completely
size using image analysis. An example showing 100 mL distilled water dissolved, add the picric acid. Bring the solution to
the difference in etching response between Mar- a low boil; do not boil dry. Solution will attack
shall’s reagent (with a few drops of hydrofluoric phenolic mounts; thermosetting epoxy mounts are
recommended.
acid) and 2% nital can be seen in Fig. 36. In this
very-low-carbon interstitial-free steel, the Mar- (a) EDTA, ethylenediamine tetraacetic acid
or nital. A specimen etched in a tint etchant can- pearlite can be seen. However, the pearlite la- martensite and retained austenite in dual-phase
not be reimmersed if the structure is too light, mella cannot be resolved in most of the islands. and TRIP steels. Special cases require other etch-
but repolishing for 15 s using 0.3 lm Al2O3 will Figure 40(b) is a replica electron micrograph of ants to reveal pearlite, cementite, and other car-
remove the tint etchant. the pearlite patch circled in Fig. 40(a). The la- bides.
Picral Ⳮ Wetting Agent. Pearlite, cementite, mellar structure is visible when examined at this
and Fe3C carbides in all carbon steels can be higher magnification.
etched using 4% picral with zephiran chloride. Selective etching is used to differentiate be-
The wetting agent improves the etching response tween various constituents in a complex micro-
of picral. Pearlite will not always appear lamel- structure. Some etchants darken cementite, and
lar, because the spacing between the cementite some do not. Some tint etchants darken marten-
and ferrite cannot always be resolved using a site, and some etchants darken ferrite. This may
light microscope. In Fig. 40, many islands of be useful in trying to distinguish cementite from
Table 3 Common etchants for coated steels

Etchant Ingredients Applications/Remarks
1% Amyl Nital 1 mL nitric acid (concentrated) Used to reveal the microstructure of zinc-based
99 mL amyl alcohol coatings (hot dipped galvanized, electrogalvanized,
Galvalume and Galfan)
This is basically a nital etchant but amyl alcohol
replaces ethyl alcohol. Etch between 10 and 20
seconds to start.
2% Nital 2 mL nitric acid (concentrated) For aluminum-based (aluminized), tin, copper, nickel,
98 mL ethyl alcohol brass and chromium coated steels. Does not etch the Fig. 35 Ferrite grains in a low-carbon (0.02% C) steel.
coating but contrasts the steel substrate. Marshall’s reagent. 500⳯
Works well with both Type 1 and Type 2 aluminized
steel. 10–20 seconds.
Rowland’s Reagent 0.075 g picric acid For etching galvanneal coatings
13 mL ethyl alcohol Etching time varies between 5 and 30 seconds.
35–60 mL water
Modified Rowland’s 50 mL water For etching zinc-based electrogalvanized coatings.
Reagent 45 mL ethyl alcohol Etching time varies between 5 and 30 seconds.
5 mL of 4% picral solution
Timofeef’s Reagent 100 mL 4% picral solution; add 6 For etching galvanneal coatings
drops of a solution of 6 g CrO3 in Etching time varies between 5 and 30 seconds.
100 mL of nitric acid
Amyl Nital Ⳮ Amyl Part A, mix equal parts of: For etching galvanneal coatings
Picral 1 mL nitric acid (conc.) Etch for 20 seconds in Part A, flush with alcohol and
99 mL amyl alcohol etch for 10 seconds in Part B
1 g picric acid
99 mL amyl alcohol
Part B, mix equal parts of:
1 mL nitric acid (conc.)
99 mL amyl alcohol
1 g picric acid
99 mL amyl alcohol
3–4 drops hydrofluoric acid per
30 mL solution
Fig. 36 Microstructure of a very-low-carbon intersti-

tial-free steel etched in (a) 2% nital and (b) Mar-
Fig. 33 Microstructure of ferrite grains and carbide par- shall’s reagent. Note that many of the ferrite grain bound-
ticles in a nondecarburized motor lamination Fig. 34 Carbides in a low-carbon steel. 4% picral etch. aries are not delineated in the specimen etched in 2% nital.
steel. 2% nital etch. 200⳯ 1500⳯ 400⳯
For example, Fig. 41 shows a number of pearl- Manual Preparation of mended sample preparation procedures for dif-
ite colonies etched using Beraha’s tint etchant to Coated Steel Specimens ferent groups of coated steel specimens. Some
darken the ferrite and highlight the cementite procedures were already briefly mentioned, but
white. Figure 42 illustrates a carburized UNS this section elaborates on a number of proven
G10200 steel, where carbides at the prior-aus- In addition to the previously described prep- techniques used for coatings. Precautions unique
tenite grain boundaries were darkened using al- aration steps, there are a number of recom- to the preparation of coated steels are also de-
kaline sodium picrate. If 4% picral had been scribed. This section describes preparation of
used, the prior-austenite grain boundaries would metallic (zinc- and aluminum-base coatings as
not have been revealed; if nital had been used, well as tin, copper, chromium, and nickel coat-
the small carbides would not have appeared in ings) and nonmetallic coatings (porcelain en-
the boundaries. amel and organic coatings). This is preceded by
a discussion on edge retention, which is of prime
importance when dealing with coatings. Many
of the coatings are thin, and a rounded edge
makes it impossible to observe the coating. Also,
most of the coatings on low-carbon steel are
softer than the steel, and the coating tends to
form a rounded edge. For most coated steel spec-
imens, the authors have successfully used the
specimen preparation procedure described as
follows.
Fig. 39 Microstructure of a very-low-carbon (decar-

burized) motor lamination steel showing co-
lumnar ferrite grains that grew toward the two sheet sur-
faces. Beraha’s tint etchant. 75⳯
Fig. 41 A pearlitic microstructure showing ferrite dark-

ened by the tint etch and cementite unaffected
Fig. 37 Microstructures of a low-carbon sheet steel (white). Beraha’s tint etch. 1000⳯
showing duplex ferrite grain size. (a) High mag-
nification, masking the duplex severity. 100⳯. (b) Low
magnification, showing true mixture of grain sizes. 100⳯.
Both etched in Marshall’s reagent
Fig. 40 Microstructure of a dual-phase steel showing

islands of martensite and pearlite in a ferrite Fig. 42 Microstructure of a carburized UNS G10200
Fig. 38 Microstructure of a batch-annealed 0.04% C matrix. An island of pearlite is circled in (a) and shown at steel showing cementite at the prior-austenite
steel sheet showing ferrite grains with grain- high magnification in (b). 4% picral etch. (a) 1000⳯. (b) A grain boundaries. The cementite was darkened by the boil-
boundary cementite (arrows). Marshall’s reagent. 500⳯ surface replica at 4970⳯ ing alkaline sodium picrate etch. 500⳯
Manual Preparation for the metallographer must keep in mind that, in imen should be cleaned with cotton and alcohol,
Coated Specimen Edge Retention most cases, the coating is there mainly to protect flushed with alcohol, and dried after each step to
the steel from corrosion. This means that expo- prevent an attack on the coating.
For most coated low-carbon steels, the follow- sure to aqueous solutions will create an electro- Polishing. Zinc-base coatings on low-carbon
ing hand grinding/polishing procedure has been lytic cell that attacks the less-noble metal ac- steel are particularly vulnerable during the pol-
proven to provide a flat edge on the prepared cording to the electromotive series of chemical ishing stage. When using a diamond-polishing
specimen. This procedure augments the previ- elements. Zinc coatings are less noble than iron, medium (e.g., paste), use an extender. The ex-
ously described procedure for low-carbon steel. whereas tin coatings are more noble than iron. tender pH should be adjusted to 9.6 Ⳳ 0.2; the
More details can be found in Ref 2: Also, the coating has different properties than the authors found that this pH works well for all
low-carbon steel substrate (hardness, thermal ex- zinc-base coatings on low-carbon steel. If the pH
1. Sectioning: Use a tabletop hand shear with
pansion, etc.). A soft coating will tend to form a is too high or too low, a reaction may develop
sharpened blades to cut specimens to proper
rounded edge on the specimen. Thus, the general between the coating and the specimen. Thus, the
size (this method is quick, convenient, and
provides minimal damage). Remove the de- procedure described previously for edge reten- metallographer must control the pH of the pol-
formation from shearing during the grinding tion should be followed. ishing medium to avoid a corrosion prob lem.
stage. Metallographic Preparation of Zinc-Base Polishing with 3-lm diamond on a stationary
2. Mounting: Use a castable epoxy, and mount Coatings. In the case of zinc-base coatings, the napless cloth with heavy pressure for 1 min
multiple specimens close together. A small zinc layer affords cathodic protection. This should remove all the scratches from the last
piece of double-sided sticky tape is attached means that the zinc is the cathode and the steel grinding grit. Next, polish on a stationary low-
at the two ends of each specimen as spacers. (iron) is the anode of an electrolytic cell when nap cloth charged with 1 lm diamond with
A sketch of this procedure is shown in Fig. exposed to an aqueous environment. In provid- heavy pressure for 60 s; continue polishing for
43. The spacer allows the epoxy to penetrate ing protection, the zinc coating is sacrificed (cor- another 30 s but back off on the pressure. The
the space between the specimens. Dummy roded away), while the steel remains intact. last step should be on a low-nap stationary cloth
sheet specimens can be placed at both sides Thus, when a zinc-coated steel is etched in an with 0.25 lm diamond with firm pressure for 20
of the stack of specimens. The coated edge aqueous solution, a cell is created, and the coat- to 30 s. After each step, clean the specimen with
should always face the same direction in the ing is attacked in preference to the steel (the zinc alcohol and cotton, flush with alcohol, and dry.
mount, and an indicator (small piece of bent is less noble than the iron in the steel). This at- Etching. A low-carbon sheet steel hot dip
sheet) can be in the mount to indicate the side tack is usually uncontrolled, and thus, water- coated with Galvalume is shown in Fig. 44. In
the coating is facing. This indicator would be based etchants should be avoided for these types this example, the etchant was 1% nitric acid in
important, so that the metallographer would of coatings. Also, if water is used during the final amyl alcohol. Amyl-alcohol-based etchants react
know the orientation of the specimen when stages of specimen preparation of the sample, a more slowly and the reaction is more easily con-
grinding and polishing. The epoxy liquid cell is created, and the microstructure of the coat- trolled than with ethanol-based etchants (Ref 2).
should be poured to a height to just cover the ing is compromised. This means that zinc-coated Also, ethyl alcohol is hygroscopic (absorbs wa-
specimens. At this point, the mount should be specimens should be rinsed clean with cotton ter) and can easily contain residual water. A two-
placed in a vacuum to remove air bubbles and and alcohol, flushed with alcohol, and dried with part mixture of equal parts (50 mL each) of 1%
to allow the epoxy to penetrate the space be- a blast of warm air. picric acid in amyl alcohol and 1% nitric acid in
tween specimens. Then, remove from the amyl alcohol can also be used. This is a modified
As mentioned in the introduction, there are a
vacuum and fill the remaining space in the version of Rowland’s reagent, which is water
variety of commercial zinc-base coatings on
mount with epoxy (no vacuum required). based. Then, 50 mL of the mixture are placed in
steel. Passing the steel sheet through a bath of
3. Grinding: During rough grinding, the defor- individual containers. In one container, add 3 to
mation zone created by the shear must be molten metal produces some of these coatings;
other coatings are plated on the surface of the 4 drops of hydrofluoric acid. A separate con-
fully removed. Also, during grinding, always tainer of ethyl alcohol is placed nearby. The first
rotate the specimen 90 after grinding on each steel sheet by an electrolytic plating process. The
former coatings are called hot dipped coatings stage of etching is conducted with the specimen,
paper. In one position, the coated edge of the face up, in the container of the mixture without
specimen must be parallel to the direction of and are galvanized (pure zinc), Galvalume (a Zn-
the hydrofluoric acid. The specimen is slightly
rotation, and the coated edge should be to- 55% Al alloy coating with 1.6% Si), and Galfan
agitated for approximately 20 s. The specimen is
ward the center of the grinding wheel. When (a Zn-5% Al coating). The latter coating is called
then rinsed in the container of ethyl alcohol, then
grinding perpendicular to the wheel rotation, electrogalvanized steel. These coatings are
placed in the other container of the mixture with
the coated edge must be the leading edge (first mostly zinc with a small amount of alloying ele-
hydrofluoric acid. Slightly agitate the specimen
edge to encounter the motion of the paper) to ment (nickel, iron, etc.). Another important zinc-
for approximately 10 s. The specimen is flushed
the direction of rotation. For the last step, it base coating is the galvannealed coating. This
(rinsed) in ethyl alcohol and blown dry. Examine
is recommended that the coated edge of the coating is formed when a hot dipped galvanized the specimen. If underetched, repeat the se-
specimen be parallel to the direction of rota- steel is annealed at 760 to 815 C (1400 to 1500 quence but double the time in the first solution.
tion to maintain complete flatness and that the F) for 2 to 3 min. The metallographic proce-
specimen and the mount be on the same dures used to prepare these various zinc-base
plane. coatings are described as follows (see also
4. Polishing: During polishing, use the lowest Ref 3).
nap (or napless) cloth possible. Polishing on Sectioning. A convenient way to section a
a stationary wheel will maintain flatness (or zinc-base coated steel is by a tabletop hand shear.
a very low revolutions per minute rotation). Mounting. Follow the procedure described in
Specific procedures for both metallic and non- the previous section on edge retention of coated
metallic coatings on low-carbon steel are de- specimens.
scribed in the remaining sections. Grinding. It is important to remove all evi-
dence of deformation from the sheared surface
Metallic Coatings during rough grinding. After rough grinding,
continue with 120-, 240-, 320-, 400-, 600-, and
All coatings on a steel surface must receive 800-grit silicon carbide papers, finishing with the Fig. 43 A schematic of multiple zinc-base coated spec-
imens showing the double-backed sticky tape
special attention. When preparing coated steels, coating parallel to the 1200-grit paper. The spec- spacers, indicator, dummy strips, and metal stabilizers
The microstructure shown in Fig. 44 illustrates A 1% nitric acid in amyl alcohol can be used (spangle pattern) of a zinc-base coating. An ex-
the various components of the hot dipped solid- for etching a simple hot dipped galvanized sam- ample of the dendrites in a spangle of Galvalume
ified coating. The solid gray particles are silicon, ple. This coating is essentially pure zinc, an ex- is shown in Fig. 49. In this case, the sheet spec-
and the diffused gray patches are a zinc-rich eu- ample of which can be seen in Fig. 45. Figure imen was suspended over a beaker of fuming
tectic; the white matrix is dendritic aluminum. 46 shows a galvanized coating that was electro- nitric acid. The acid fumes attacked the surface
Also, there is a silicon-rich intermetallic layer plated to the low-carbon steel surface. This is of the coating, revealing the dendrites. A similar
(light gray) at the interface between the steel and called an electrogalvanized coating. In general, spangle, as viewed in the scanning electron mi-
the coating. This etch, because of the nitric acid, electrogalvanized coatings are thinner than hot croscope, is seen in Fig. 50. This technique is
also attacked the steel substrate, with some of dipped galvanized coatings. useful in that the secondary dendritic arm spac-
the ferrite grain boundaries revealed. Another form of zinc coating is a hot dipped ing can be measured. The spacing of the den-
galvanized coating that is heat treated. It is called dritic arms is directly related to the cooling rate
a galvannealed coating. In a galvannealed coat- during solidification of the coating.
ing, a number of iron-zinc intermetallic phases Metallographic Preparation of Tin, Cop-
are formed during the heat treating process. Fig- per, Chromium, and Nickel Coatings. Some
ure 47 shows an example of a galvannealed coat- coatings, such as tin, copper, and nickel, have
ing. The phases in the coating are zeta (the crys- the opposite effect of corrosion protection from
tals at the top surface of the coating), delta (the zinc-base coatings. These elements are more no-
matrix phase), and gamma (the phase at the steel/ ble than iron, and thus the iron becomes the cath-
coating interface). ode and they become the anode. Tin coatings are
One more example of a zinc-base coating is used as a protective coating by preventing the
Galfan. As described previously, it is a hot corrosive environment from reaching the steel
dipped Zn-5% Al coating. Figure 48 shows the substrate. Tin coatings are applied to the steel
microstructure of a Galfan coating on a low-car- sheet by either passing the steel sheet through a
bon steel. bath of molten tin or by an electrolytic plating
Sometimes, the metallographer is asked to re- process.
veal the microstructure of the dendritic pattern
Fig. 44 Microstructure of a Galvalume (zinc-alumi-

num) coating on a low-carbon steel sheet.
Etched in 1% nitric acid in amyl alcohol. 1000⳯
Fig. 48 Microstructure of a hot dipped Galfan coating

on a low-carbon steel sheet. Etched in 2% ni-
Fig. 46 Microstructure of an electrogalvanized coating tric acid in amyl alcohol. Differential (Nomarski) interfer-
on a low-carbon steel sheet. Etched in 1% ni-
ence contrast illumination. 1500⳯
tric acid/amyl alcohol. 100⳯
Fig. 47 Microstructure of a galvannealed coating on a

low-carbon steel sheet. Note the various inter-
metallic compounds that developed. Etched in 100 mL Fig. 49 Microstructure of the dendritic pattern in a
Fig. 45 Microstructure of a hot dipped galvanized amyl alcohol containing 1 mL nitric acid and 1 g picric spangle on the surface of a Galvalume coating.
coating on a low-carbon steel sheet. Etched in acid for 20 s, followed by the same concentration solution Etched by suspending the coated surface over fuming nitric
1% nitric acid/amyl alcohol. 1000⳯ plus 4 drops of hydrofluoric acid for 15 s. 100⳯ acid. 200⳯
Sectioning. Generally, this type of material is Metallographic Preparation of Aluminum- Grinding. Start grinding with 120-grit silicon
sectioned with a tabletop hand shear to prevent Base Coatings. When aluminum is coated on carbide paper to remove the deformed micro-
distortion. steel, it comes under the classification of alu- structure caused by sectioning. Grind with the
Mounting. Thin-coated specimens can be minized steel. The steel sheet is passed through coated side of interest parallel to the direction of
mounted in a thermosetting epoxy compound. a molten bath of the aluminum alloy. There are wheel rotation (coated edge facing the center of
One suggestion is to bend the specimens in the generally two types of aluminized coatings: type the wheel). During the next step (240 grit), the
shape of an “L” in order to stand up in the mount. 1, which is aluminum that contains 9% Si, and sample should be turned 90 to the previous
Also, place them as close together as possible to type 2, which is pure aluminum. The microstruc- grind, with the edge of interest as the leading
maintain edge flatness. For thin specimens, the ture of types 1 and 2 aluminized sheet can be edge to the rotation of the wheel. Continue for
observable coating thickness can be increased by seen in Fig. 52. Both coatings have an alloy layer at least twice as long to remove the deformation
placing them in a commercial holder designed to at the coating/steel interface that is essentially an layer caused by the silicon carbide grit of the
hold circuit boards that has been modified by iron aluminide intermetallic compound. In ad- 120-grit paper. Next, proceed to 320 grit, rotat-
cutting it on a 45 or less angle. The modified dition, type 1 aluminized steel (Fig. 52a) has paring the mount 90, with the edge of interest again
holder is then placed in a mold with the samples ticles of silicon (darker gray) in the coating. parallel to the rotation and facing the center of
and cast with epoxy. Figure 51 shows a compar- Sectioning. This type of material can be sec- the wheel, and continue grinding twice as long
ison of a normal cross-sectional view and a 45 tioned with a shear, band saw, or abrasive saw, as it took to remove the previous scratches.
view of two thin coatings on low-carbon steel. as long as the effect of sectioning is removed Then, proceed to 400 grit, rotating the mount
This technique can be used for other thin coat- during rough grinding. The sample prepared for 90, with the edge of interest as the leading edge
ings. this article was sectioned by shearing. to the rotation of the wheel. Continue grinding
Grinding should begin with coarse grit in or- Mounting. When mounting in thermosetting for at least twice as long it took the 320-grit
der to remove the deformation caused by sec- epoxy, multiple samples are bent in an “L” shape scratches to remove the deformation layer. For
tioning. Note: The deformation zone will in- in order for them to stand up in the mount. Place the last grinding step (with 600 grit), the sample
crease as the sample thickness increases. If a as close together as possible. Fine epoxy powder is turned 90, with the edge of interest again par-
certain side of interest is to be examined, it is poured on top, followed by normal-sized pow- allel and facing the center of the wheel; continue
should always be facing the center of the wheel der. The pressure needed to polymerize the ther-
when grinding parallel to the rotation; when mosetting epoxy will push the samples closer to-
grinding perpendicular to rotation, the side of in- gether, thereby minimizing rounding during the
terest should be the leading edge. Also, on the polishing steps.
last grinding step (600 or 800 grit), the coating
should be parallel to the wheel rotation. This
grinding procedure will minimize rounding of
any coating.
Polishing is done on a very-low- or no-nap
cloth charged with 6 lm diamond, using heavy
pressure until the scratches from the last grinding
step have disappeared. This usually takes 1 min.
Next, polish the sample on low-nap rayon cloth
with 0.3 lm aluminum oxide slurry for 2 min,
using firm pressure, followed by 1 min on a low-
nap rayon cloth with firm pressure with the
wheel stationary. After all polishing steps, the
sample is cleaned with cotton under running wa-
ter, flushed with alcohol, and dried.
Etching for 10 to 20 s in 2% nital will develop
sufficient contrast between the base steel and the
coating.
Fig. 52 Microstructure of aluminized low-carbon steel.

(a) Type 1 aluminized (aluminum with 9% Si).
Fig. 50 A spangle dendrite similar to that shown in Fig. Fig. 51 (a) Microstructure of a brass coating with a (b) Type 2 aluminized steel. Both coatings have the alloy
49, viewed in the scanning electron micro- clear lacquer film on a low-carbon sheet with layer (iron aluminide intermetallic layer), and silicon par-
scope. Etched by suspending the coated surface over fum- a 45 mount. (b) Microstructure of a nickel coating on low- ticles can be seen in type 1 aluminized. 2% nital etch.
ing nitric acid. 200⳯ carbon sheet without the 45 angle. 2% nital etch. 1000⳯ 1000⳯
for at least twice as long as it took to remove the last grinding step, the coating should be parallel Polishing on a stationary wheel will minimize
400-grit scratches. Keeping the edge of interest to wheel rotation. Clean the sample with cotton edge rounding.
parallel to the rotation and facing the center of under running water, flush with alcohol, and dry. Etching. In both types of aluminized steel
the wheel, plus making the edge of interest the The coating and mount should be on the same shown in the examples, a simple 2% nital etch
leading edge when grinding perpendicular to the plane after the grinding step; if not, it must be is generally sufficient to reveal the microstruc-
wheel, will greatly reduce rounding. Also, on the corrected before polishing. ture of the coating.
Polishing. Polish on a nylon cloth with 6 lm
diamond abrasive with heavy pressure. Rotate Nonmetallic Coatings
the sample in the opposite direction to the wheel
rotation (150 rpm) until the parallel scratches Metallographic Preparation of Enamel
from the 600 grit have been removed. Clean with Coatings. Enamel coatings on steel are much
cotton under running water, flush with alcohol, different than metallic coatings. Enamel is a
and dry. The diamond paste remaining on the glass (porcelain) layer that is physically melted
specimen can be mistaken for parallel grinding on the steel surface. Generally, a frit (crushed
scratches; therefore, the sample must be cleaned glass particles) suspended in an aqueous solution
to observe if the scratches have been removed. is applied to the steel surface, and the component
Next, polish with 0.3 lm alumina, using a firm is heated to the firing temperature, where the frit
pressure on a medium-nap rayon cloth for 2 min, melts into a layer of glass. Some enamel coatings
with the wheel stationary. Clean with cotton un- are applied and fired in multiple layers. Enamel
der running water, flush with alcohol, and dry. coatings do not have an electrochemical prob-
The last step is with 0.05 lm silicon dioxide on lem, as found in zinc-base coatings. The coating
a medium-nap rayon-cloth stationary wheel for is essentially an inert glass. The enamel coating
60 to 90 s, with firm pressure. Clean with cotton is also harder than most metallic coatings, and
under running water, flush with alcohol, and dry. usually, edge retention is not a problem. How-
ever, the enamel coating is brittle and can easily
chip if the specimen is not handled properly (i.e.,
during sectioning).
Sectioning. Because of the brittleness of the
enamel, the specimen should be sectioned with
a low-speed gravity diamond saw, using mineral
spirits as a cutting fluid. Align the sample in the
holder so that the edge of interest is facing the
blade. This will minimize damage to the coating.
If a shear is used, the coating will crack and spall
from the surface of the steel.
Grinding. Start grinding with 320-grit silicon
carbide paper, with the coating side of interest
parallel to the direction of wheel rotation and
facing the center of the wheel. During the next
Fig. 53 Microstructure of a low-carbon sheet with a step (400 grit), the sample should be turned 90
two-part enamel coating. (a) Without back-
to the previous grind, with the edge of interest
lighting. (b) With backlighting through the epoxy mount to Fig. 54 Microstructure of an enamel coating, same as
as the leading edge to the rotation of the wheel.
differentiate the coating from the mount. The bubbles are Fig. 53, shown with dark-field illumination to
desired for trapping hydrogen gas. illustrate the ground coat When all the scratches from the 320-grit paper
Fig. 55 Defect in an enamel coating on a low-carbon steel. (a) Defect shown through coating as a line in this macrograph (scale in mm). (b) Cause of line defect shown in (a). As-
polished. 200⳯. Courtesy of Samuel Lawrence, International Steel Group
are removed, continue for at least twice as long a two-coat enamel coating on a low-carbon steel. Sectioning. Cutting into the painted surface is
to remove the deformation layer caused by the The ground coat and the topcoat can both be seen recommended; this will minimize the possibility
silicon carbide grit of the 320-grit paper. For the in bright-field illumination, as opposed to the of pulling the paint off the steel substrate. A thin-
last grinding step (600 grit), the sample is turned case shown previously. The bubbles in the en- sheet specimen can also be sectioned with a ta-
90, with the edge of interest again parallel and amel coating are desirable as traps for hydrogen bletop hand shear.
facing the center of the wheel; continue for at gas. Hydrogen gas, if trapped between the steel Mounting. It is recommended to mount
least twice as long as it took to remove the 400- and the coating, can expand and create a spall in painted specimens in epoxy, keeping the speci-
grit scratches. Clean the sample with cotton un- the coating. This defect is called a fishscale be- mens as close together as possible to prevent
der running water, flush with alcohol, and dry. cause of its appearance. The enamel layer is usu- rounding. Making a sandwich out of the mate-
The coating and epoxy mount should be on the ally not etched, but dark-field illumination and/ rial, as described in the zinc-base coating sec-
same plane after the grinding step. or polarized light can sometimes be used to tion, will ensure good edge retention. Mounting
Polishing. Polish on a nylon cloth with 6 lm observe the structure of the enamel coating. For in epoxy will not damage the paint and will al-
diamond abrasive with heavy pressure, rotating example, Fig. 56 shows a defect in an enamel low lighting from the back-side of the mount if
the sample in the opposite wheel rotation (150 coating on a low-carbon steel. Figure 56(a) the paint contrast in reflected light is the same as
rpm) until the parallel scratches from the 600 grit shows the microstructure in bright-field illumi- the epoxy mount.
have been removed. Clean the sample with cot- nation (standard illumination practice), and Fig. Grinding should begin with coarse grit in or-
ton under running water, flush with alcohol, and 56(b) shows the same field in dark-field illumi- der to remove the deformation caused by sec-
dry. The diamond lubricant can be mistaken for nation. Note the detail in the dark-field micro- tioning. Note: The deformation zone will in-
parallel grinding scratches; therefore, the sample graph. crease as the sample thickness increases. If a
must be cleaned to observe if the scratches have Metallographic Preparation of Organic certain side of interest is to be examined, it
been removed. (Paint) Coatings. The metallographer may en- should always be facing the center of the wheel
Next, polish on a nylon cloth with 1 lm dia- counter low-carbon steel specimens that have an when grinding parallel to the rotation. When
mond abrasive for 1 min, using heavy pressure. organic coating such as paint. In fact, there may grinding perpendicular to rotation, the side of in-
Rotate the sample in the opposite direction of be multiple layers of paint. These painted spec- terest should be the leading edge. Also, on the
wheel rotation, which should be rotating at 150 imens are prepared a little differently from spec- last grinding step (600 or 800 grit), the coating
rpm. Clean the sample with cotton under running imens with metallic coatings. should be parallel to the wheel rotation. This
water, flush with alcohol, and dry. Next, polish grinding procedure will minimize rounding of
with 0.3 lm alumina abrasive with a medium- any coating.
nap rayon cloth for 2 min. Use a firm pressure Polishing is done on a very-low- or no-nap
in a direction opposite the wheel rotation, which cloth charged with 6 lm diamond abrasive, us-
should be set to low speed. Clean with cotton ing heavy pressure until the scratches from the
under running water, flush with alcohol, and dry. last grinding step have disappeared. This usually
The last step is with 0.05 lm silicon dioxide on takes 1 min. Next, the sample is polished on low-
a medium-nap rayon-cloth stationary wheel for nap rayon cloth with 0.3 lm aluminum oxide
60 to 90 s, with firm pressure. Clean with cotton slurry for 2 min, using firm pressure, followed
under running water, flush with alcohol, and dry. by 1 min on a low-nap rayon cloth with firm
Etching. First, etch with 4% picral to examine pressure, with the wheel stationary. After all pol-
for carbides or pearlite. The sample can be re- ishing steps, the sample is cleaned with cotton
etched with 2% nital to reveal the ferrite grains. under running water, flushed with alcohol, and
If the sample is first etched in nital, grain-bound- dried.
Etching for 10 to 20 s in 2% nital will develop
ary carbides can be obscured. No etch is neces-
sufficient contrast between the base steel and the
sary to see the enameled coating. However, fiber
paint. Polarized light or dark-field illumination
optic lighting can assist in delineating the coat-
will help separate multiple paint layers. See Fig.
ing. Figure 53 shows a black-colored enameled
57 for an example of a 0.06% C steel painted
steel sample prepared following this procedure.
with a single layer of paint and backlighted
Figure 53(a) is without fiber optic lighting. The through the back of the epoxy mount.
micrograph in Fig. 53(b) was taken using light
from a fiber optic lamp transmitted through the
transparent mount. This procedure assisted in de-
lineating the enamel coating from the mounting
material.
By using dark-field illumination, coating de-
fects and different enamel layers applied during
pocessing will become apparent. Figure 54 was
taken with dark-field illumination to show the
ground coat. Note that dark-field illumination
delineates a ground coat (first enamel layer) on
the sheet. This initial coat could not be seen in
the bright-field micrograph. Also, note that dark-
field illumination highlights the bubbles in the
enamel coating.
The steel used for enameling must have a low
carbon content in order to eliminate the presence
of cementite. Cementite particles on the sheet Fig. 57 Microstructure of a paint layer on a 0.06% C
surface can decompose and react with the en- Fig. 56 Microstructure of a defect in an enamel coating steel sheet, backlighted through the mount to
on a low-carbon sheet. (a) Bright-field illumi- differentiate the paint from the mount. Etched in 2% nital.
amel layer to create a defect. Figure 55(b) shows nation. (b) Dark-field illumination. 2% nital etch. 100⳯ 200⳯
REFERENCES 3. E. Weidman, “Metallographic Preparation of ● B.L. Bramfitt and A.O. Benscoter, The Met-
Zinc Coatings,” Application Notes, Struers, allographers Guide: Practices and Proce-
1. L.E. Samuels, Metallographic Polishing by Copenhagen, 2002 dures for Irons and Steels, ASM Interna-
Mechanical Methods, ASM International, 2003 tional, 2002
2. C.E. Gordan, K.M. Goggins, A.O. Benscoter, ● L.E. Samuels, Light Microscopy of Carbon
and A.R. Marder, Metallographic Preparation SELECTED REFERENCES Steels, ASM International, 1999
Technique for Hot-Dip Galvanized and Gal- ● G.F. Vander Voort, Metallography Principles
vannealed Coatings on Steel, Mater. Char- ● E. Beraha and B. Shpigler, Color Metallog- and Practice, McGraw-Hill, 1984. Reprinted
act., Vol. 31 (No. 2) 1993, p 107–114 raphy, American Society for Metals, 1977 by ASM International, 1999

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Asm - Metalografia de Aço Baixo Carbono

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ASM Handbook, Volume 9: Metallography and Microstructures Copyright © 2004 ASM International®

G.F. Vander Voort, editor, p588–607 All rights reserved.

Metallography and Microstructures of

Fig. 4 Microstructure of epitaxial ferrite (arrows)

Fig. 8 Microstructure of a slow-cooled UNS G10080

Fig. 12 Sketch showing the three planes of rolling. RD,

There are many abrasive wheel cutting ma-

Fig. 20 Six low-carbon steel sheet specimens, sepa-

Fig. 21 A zinc-particle polymer coating (Zincrometal)

Fig. 30 A decarburized UNS G10100 steel sheet

Table 3 Common etchants for coated steels

Fig. 36 Microstructure of a very-low-carbon intersti-

Fig. 39 Microstructure of a very-low-carbon (decar-

Fig. 41 A pearlitic microstructure showing ferrite dark-

Fig. 40 Microstructure of a dual-phase steel showing

Fig. 44 Microstructure of a Galvalume (zinc-alumi-

Fig. 48 Microstructure of a hot dipped Galfan coating

Fig. 47 Microstructure of a galvannealed coating on a

Fig. 52 Microstructure of aluminized low-carbon steel.

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