Professional Documents
Culture Documents
06358G Sample BuyNow PDF
06358G Sample BuyNow PDF
Optical Metallography
M.R. Louthan, Jr., Department of Materials Engineering, Virginia Polytechnic Institute and State University
Introduction proximately 50x or higher; macroscopy Because the macro- and microstructure of
Optical metallography, one of three gen- (macrostructural examination), 50 x or metals and alloys often determine the behav-
eral categories of metallography, entails ex- lower. ior of the material, characterization of the
amination of materials using visible light to Optical microscopy and, occasionally, effects of composition, processing, service
provide a magnified image of the micro- and SEM are used to characterize structure by conditions, and other such variables on the
macrostructure. In scanning electron micros- revealing grain boundaries, phase bound- macro- and microstructure is frequently re-
copy (SEM), the second category, the sur- aries, inclusion distribution, and evidence of quired. Typical structure-property relation-
face of the specimen is bombarded with a mechanical deformation. Scanning electron ships that have been established using optical
beam of electrons to provide information for microscopy is also used to characterize frac- metallography include:
producing an image (see the article "Scan- ture surfaces, integrated circuits, corrosion
ning Electron Microscopy" in this Volume). products, and other rough surfaces, espe- • A general increase in yield strength and
Lastly, transmission electron microscopy cially when elemental microanalysis of small hardness of a metal with decreasing grain
(TEM) consists of passing a beam of elec- features is desired. Transmission electron size
trons through a very thin specimen and microscopy is used to examine dislocation • A general tendency for a decreased duc-
analyzing the transmitted beam for structural arrangements or structures and other small tility with increasing inclusion content
information (see the article "Analytical defects in metals and alloys. Second-phase • Correlations of weld penetration, heat-
Transmission Electron Microscopy" in this particles not observable using optical metal- affected zone (HAZ) size, and weld-
Volume). Microscopy (microstructural ex- lography can frequently be analyzed using defect density with the nature and char-
amination) involves magnifications of ap- TEM. acter of the welding
3 0 0 / M e t a l l o g r a p h i c Techniques
• Evaluation of such surface treatments as Edition of Metals Handbook). The most Fig. 1 One method of mounting
carburizing and induction hardening by widely used sectioning device is the abrasive the sample to retain flatness for
determinations of the depth and micro- cutoff machine, ranging from units using metallographic examination
structural characteristics of the hardened thin diamond-rimmed wafering blades to
The mount can also be filled with ground glass,
region those using wheels that are more than 1.5 pelletized AI203, or another hard material to
• Correlations of fatigue crack growth rates mm (1/16in.) thick, 30 to 45 cm (12 to 18 in.) maintain flatness.
and fracture-toughness parameters with in diameter, containing silicon carbide parti-
Test Specimen mounted in Bakelite
such structural variables as inclusion con- cles.
tent and distribution Heat is generated during abrasive cutting, Test specimen
• Association of failure initiation sites with and the material just below the abraded
microstructural inhomogeneities, such as surface is deformed. To minimize burning
second-phase particles and deformation, a lubricant or coolant is
• Correlations of anisotropic mechanical typically used. Wet cutting yields a flat
~ _ o o -- L
behavior with elongated grains and/or relatively smooth surface. However, because
preferred grain orientations of the abrasion associated with cutting, the
structure of the metal or alloy is damaged to
The microstructures of metals and alloys a depth of approximately 1 mm (0.04 in.).
are determined by composition, solidifica- The exact depth of damage depends on the
tion processes, and thermomechanical treat-
type of cutoff wheel used, the cutting speed,
ment. Therefore, these process variables de- and the hardness of the specimen. The harder
termine the response of metals and alloys to the specimen, the shallower the depth of
laboratory and service environments. Be- damage. This damaged layer must be re-
cause of the relationships between structure moved by grinding. However, before the
and properties, metallographic characteriza- specimen can be conveniently ground, it Hardened steel balls or chilled iron shot (typ)
tion is used in materials specification, qual- often must be mounted.
ity control, quality assurance, process con- Mounting facilitates handling of the
trol, and failure analysis. specimen. A procedure that does not damage
Optical metallography is applicable to the specimen should be selected. Because
studies ranging from fundamental research to
large specimens are generally more difficult
production evaluations. This article will dis- to prepare than small ones, specimen size
cuss use of optical methods to evaluate should be minimized. Standard or typical
structure and to relate that structure to pro-
specimen mounts are right circular cylinders
cess conditions and/or material behavior.
25 to 50 mm (1 to 2 in.) in diameter.
Detailed information on the principles and
Mounting mediums should be compatible
instrumentation of optical microscopy is ,- / 32 mm (1.25 in.) diam ] -,
with the specimen regarding hardness and
available in the article "Optical Micros-
abrasion resistance. Two common mounting Bakelite mounting
copy" in Volume 9 of the 9th Edition of Nickel plate, 0.05 mm
materials are thermosetting phenolics, such
Metals Handbook. (0.002 in.) thick
as Bakelite, and thermoplastic materials,
Specimen Preparation such as methyl methacrylate (Lucite). A
thermosetting polymer develops a rigid
Section A-A
Fig. 4 Comparison of nital and picral for revealing a martensite Fig. 5 Macrostructure of as-cast
structure aluminum ingot
Ca) Specimen etched using nital (nitric acid in ethanol or methanol). (b) Specimen etched using picral (picric Transverse section shows outer chill zone and
acid in ethanol). Both 1000 × columnar grains that have grown perpendicularly to
the mold faces. Etched using Tucker's reagent.
1.5×
Ca) (b)
dye to fluoresce, and the cracks became
readily observable. Dye-penetrant tech-
Fig. 6 Macrostructure of a continuous-cast copper ingot niques are excellent for examination of
Ca) Spider cracks revealed using dye-penetrant inspection. Transverse section at top; longitudinal section at crack-like macrostructural defects in metals:
bottom. (b) Same ingot, etched using Waterbury's reagent. Cracks are not revealed. Both approximately However, grains and other microstructural
0.5x
features are visible only after etching, which
frequently obscures the presence of the
cracks. Therefore, different metallographic
techniques are necessary to reveal various
macrostructural elements.
Materials characterization by optical
\ macrostructural examination can be divided
into three categories. First, examination of
the macrostructure of metallographically
prepared sections removed from the compo-
nent of interest is used to evaluate such
structural parameters as:
Fig. 1 0 S k e t c h of g r a i n s in a Fig. 12 E x a m p l e of h o w f r a c t u r e s u r f a c e f e a t u r e s c a n p o i n t to t h e
t y p i c a l cast i n g o t f a i l u r e origin
(a) Fractograph of a high-velocityfracture in steel plate showingchevronpattern indicatingthe origin
Chill Columnar Central Columnar Chill
(left). (b) Schematicview of (a)
zone zone zone zone zone
Fibrous
Fig. 11 T r a n s v e r s e f r a c t u r e of a n
AISI 1075 steel railroad rail
Fracture nucleus(dark area near top of railhead)
initiated a fatigue crack (large light area around
nucleus).
(b)
on the fracture surface (Fig. 12) known as These two types of metallography are com-
chevrons or herringbone marks. The tip of plementary, but examination should always
the V generally points to the origin of the begin at low magnification and work up-
failure. The origin of fatigue failures can wards. Detailed information on sample prep-
also be isolated using macroscopic examina- aration, equipment and etchants used in
tion. For example, Fig. 13 shows a failure of macroanalysis, and interpretation of results
a steel housing tube initiated in four regions. is available in Volume 9 of the 9th Edition of
Each initiation region is observable in the Metals Handbook.
ent in the cross sections of macroetched macrographs, as shown by the four arrows.
ingots (Fig. 5 and 6). The outer chill zone
depth, shape and size of the columnar or
The position of the crack fronts at various
times during the failure process is also visi-
Microanalysis
dendritic grains perpendicular to the mold ble as the so-called beach marks that are The importance of microstructure to the
wall, and size of the central equiaxed zone in initially fairly concentric to the origin. The properties of metals and alloys has long been
a casting can be established (Fig. 10). One major problem with optical macroscopic or recognized. Grain size, twins, and the size,
benefit of the macroscopy of cast structures microscopic examination of fracture surfaces shape, and distribution of second-phase par-
is the ability to reveal the structure and is the technique's inability to obtain favor- ticles are important in determining the be-
associated defects. able focus over the entire surface if the havior of most structural metals. Therefore,
Optical macroscopic examination of a magnification exceeds 5 to 10 x . Therefore, characterization of the various microstruc-
fracture surface may reveal features that will SEM has become a standard metallographic tural elements in a metal or alloy is often
help establish the failure process. For exam- tool in failure analysis. necessary. Process-control parameters are
ple, Fig. 11 illustrates a fracture in a railroad Macroscopic evaluation of corroded parts established to provide specific grain sizes.
rail. The relatively smooth region in the can also provide considerable insight into The number, size, and distribution of sec-
photograph represents crack growth because corrosion processes. Each type of corrosion- ond-phase particles, such as inclusions, are
of cyclic or fatigue loading. The dark spot induced failure causes a characteristic frequently specified, and quantitative metal-
(or fish eye) in the center of the reflective macrographic appearance; therefore, evalua- lographic procedures have been developed to
area represents the fracture-initiation site. tion using optical macroscopy is generally describe microstructure.
The remainder of the surface failed by over- effective. A frequent mistake in failure anal- The upper limit of useful magnification in
load. This macroscopic observation of the ysis is to neglect examination of the broken the optical microscope is approximately
failed rail shows that the failure was initiated pieces at low magnifications. Too frequently 1500 x , and the fundamental limitations of
because of the dark-appearing defect in the the component is sectioned immediately, and light optic systems limit resolution to fea-
rail. the failure, casting, or other type of speci- tures which are --1 Izm or larger. Although
The macroscopic nature of many fractures men examined at high magnification. Opti- this value is small, many microstructural
is such that the fracture origin is easily cal microscopic evaluation clearly is signif- features influencing the properties of metals
recognizable. Brittle or low-ductility frac- icant in any structural evaluation, but should and alloys are too small to be observed using
tures have characteristic V-shaped markings not replace characterization by macroscopy. optical microscopy. Dislocations, numerous
Optical Metallography / 305
(a) (b)
Fig. 14 C o p p e r a l l o y 2 6 0 0 0 ( c a r t r i d g e b r a s s , 7 0 % ) s h e e t , h o t r o l l e d t o a t h i c k n e s s o f 10 m m ( 0 . 4 i n . ) ,
annealed, cold rolled to a thickness of 6 mm (0.239 in.), and annealed to a grain size of 0.120 mm
(0.005 in.)
At this reduction, grainsare basicallyequiaxed.Comparewith Fig. 15. Diagramin lower left of each microgrophindicatesorientationof the view relative to the
rolling plane of the sheet. Etchedusing NH40H plus H202. 75 ×
types of second-phase particles, spinodal and Optical characterization of the microstruc- microstructure in several directions. Figure
ordered structures, and many aspects of mar- tures of metals and alloys involves determi- 14 shows an annealed microstructure exhib-
tensitic structures can be categorized as too nation of the size and shape of the grains, the iting similar grain shapes in all three views.
small for optical microscopy. Therefore, me- extent of twinning, and some of the charac- Grain size is characterized by placing a line
tallographic observations of these very fine teristics of grain boundaries and other ob- of known length (or preferably a circle of
structural features is generally restricted to servable defects. Solidification, solid-state known circumference) on the magnified im-
electron microscopy. Optical microscopy, transformation, deformation, and annealing age of the microstructure and counting the
then, is used primarily to examine grain microstructures are the four basic types in number of intersections between the line and
structures and the morphology of large metals and alloys. Each of these has distinct grain boundaries in the microstructure. The
second-phase particles. Specialized optical characteristics. number of intersections, N, can be converted
metallographic techniques, such as polarized Microstructural features exist in three di- to a measure of grain size, d, using:
light microscopy and interference micros- mensions, and in a typical metallographic
copy, can add significantly to the informa- observation, only two dimensions are ob-
tion obtained in a microscopic investigation, served. Therefore, effective microscopy fre- d- L
NM (Eq 1)
and interference microscopy can be used to quently requires microstructural observa-
identify height differences on a sample sur- tions in two or more directions. Figures 14
face that are far smaller than 0.2 ixm. and 15 illustrate the value of viewing the where M is the magnification of the image
~ ~ iii¸ iiii!iiii ¸
~1 ~ h
Fig. 18 Continuous Fig. 20 The effect of prior cold require controlling defects to regulate their
g r a i n - b o u n d a r y precipitate in w o r k on recrystallized g r a i n size number, size, and shape in a particular
U - 7 0 0 nickel,base heat-resistant manner. For example, a component having a
0.4 stringer distribution such as that shown in
alloy ~ o 700 °C '" Fig. 17(c) would have better ductility if
EtchedusingHCI, ethanol,and H202. 500 × E /| • 600 °C I Recrystallization specimens or components were tested with
E / " 500 °C '-
r~ • 450 °C / temperature _ the major stresses parallel to the stringer than
0.3 . . . . .
o 400 °C J if specimens were oriented with the major
c
stresses perpendicular to the stringer.
'~ 0.2 Transformation structures almost always
contain two phases. In such structures, the
major phase is typically termed the matrix,
or base structure, and the minor phase is
~ 0.1
termed the second phase. The size, shape,
I c-t I t °--~ and distribution of second-phase particles are
important in determining the properties of
0
0 10 20 30 40 metals and alloys. Characterization of
Amount of cold work, % second-phase morphology can sometimes be
accomplished using optical metallography.
However, the second phase is sometimes so
small that the resolution necessary to char-
render the grain structure--and the resulting acterize the phase morphology exceeds the
mechanical properties---anisotropic. Be- limits of the optical microscope. In these
cause of the interrelationships between grain cases, transmission electron microscopy
Fig. 19 Discrete precipitates morphology (size and shape) and mechanical must be used. Age-hardenable or preci-
properties, characterization of the grain pitation-hardened metals and alloys gener-
along g r a i n boundaries in a
structure is a typical metallurgical function. ally must be characterized using electron
nickel-base heat-resistant a l l o y
The most commonly observed solidifica- microscopy.
Specimenwas etchedusing35 mLHCI, 65 mL tion structure is dendritic. A dendritic struc- High-temperature phase transformations
ethanol, and 7 dropsH202. 500 ×
ture usually exhibits compositional varia- frequently nucleate at grain boundaries. The
tions, with the dendrite arms containing less grain-boundary structures can be discrete or
alloying element or impurity than interden- continuous. Continuous grain-boundary con-
dritic regions. Because of such composi- stituents (Fig. 18) provide easy fracture
tional changes (termed coring), the rate of paths when the grain-boundary phase is less
etching at interdendritic regions differs from ductile than the matrix phase. For the mate-
that at dendrite arms. If the alloying element rial shown in Fig. 18, the expected failure
or impurity content is high, interdendritic would be fracture along the grain-boundary
regions may develop a two-phase structure carbides. Figure 19 also shows discrete
(Fig. 16). Because dendrite arm spacing second-phase precipitates at grain bound-
tends to decrease with increasing cooling aries. Comparison of the microstructures
rates, the properties of as-cast metals depend shown in Fig. 18 and 19 reveals differing
on the solidification rates. second phase morphologies in two similar
Most metals shrink during solidification. alloys. Therefore, the properties of these two
Therefore, the liquid trapped between den- alloys are also different, with the structure
drite arms during solidification is frequently illustrated in Fig. 18 exhibiting the highest
insufficient to fill the space between the arms strength but the least ductility.
when solidification is complete. This inabil- The microscopic details of deformation
ity to fill the remaining space leads to shrink- structures typically cannot be established
age porosity, which can be observed micro- using optical metallography. Deformation
scopically. Porosity is generally easier to changes number and arrangement of disloca-
observe on as-polished specimens than on tions (crystal defects) in the metal o n an
polished and etched ones. Figure 17(a) atomic scale. This dislocation substructure is
shows a typical example of shrinkage poros- best characterized using TEM. Optical met-
ity. allography can be used to supplement TEM
Other structural defects, such as inclu- through characterization of the grain size and
sions and stringers (Fig. 17b and 17c), can anisotropy in grain shape and distribution.
observed, and L is the length of line on the also be observed microscopically in Microstructural changes due to annealing
image. as-polished specimens. Such defects as those may be studied using TEM or optical micros-
The microstructure of the cold-rolled cop- shown in Fig. 17 can serve as failure- copy. The most important structural changes
per alloy shown in Fig. 15 differs from that initiation sites in metals and alloys; there- that occur during annealing are recovery,
of the annealed metal. Rolling elongated the fore, characterization of their size, shape, recrystallizafion, and grain growth.
grains in the rolling direction and flattened and distribution is necessary to establish Recovery is the rearrangement and anni-
the grains in directions transverse or normal material properties and engineering reliabil- hilation of imperfections (primarily vacan-
to the rolling directions. This change can ity. Quality-assurance programs frequently cies and interstitials) within each grain of a
308 / Metallographic Techniques
cold-worked polycrystalline component. Be- amount of cold work, the finer the grain size SELECTED REFERENCES
cause recovery deals mainly with point de- (Fig.20). Because grain boundaries are a
fects, any microstructural observations of it crystalline defect, continued annealing will * J.L. McCall and W.M. Mueller, Ed.,
are difficult, and optical microscopy cannot cause this array of grains to be unstable, and Metallographic Specimen Preparation,
be used because of its limited resolution. grain growth will take place. Grain growth Plenum Press, 1974
Recrystallization is the formation of new in a recrystallized specimen decreases the * Metallography and Microso-uctures, Vol
strain-free grains within the previously cold- grain-boundary surface area to specimen 9, 9th ed., Metals Handbook, American
worked (strained) grains. The initial stages volume ratio because the average grain size Society for Metals, 1985
of recrystallization occur on such a fine scale increases as grain growth takes place. The • Metallography, Nondestructive Testing,
that TEM is necessary; however, oPtiCal rate of grain growth depends on temp- Vol 03.03, Annual Book of ASTM Stan-
metallography can be readily used to study erature and time. Detailed information on dards, ASTM, Philadelphia, 1984
most of the recrystallization. The size of the all of these types of structures and on the • G. Petzow, Metallographic Etching,
recrystallized grains depends on the amount metallography and microstructures of specific American Society for Metals, 1978
of cold working of the specimen before the metals and alloys is available in Volume 9 • G.F.Vander Voort, Metallography: Prin-
recrystallization anneal. The greater the of the 9th Edition of Metals Handbook. ciples and Practice, McGraw-Hill, 1984