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T • U • Tof•Metals

Fractography O • R I • A •(continued)
and• Plastics L by Ronald J. Parrington, P.E.

Fractography of Metals and Plastics

F
ractography is critical to failure analysis of metals and plastics. Fractography of plastics is a rel-
atively new field with
many similarities to
metals. Using case histories,
various aspects of failure analysis
and fractography of metals and
plastics are compared and
contrasted.
Failure modes common to
both metals and plastics include
ductile overload, brittle fracture,
impact, and fatigue. Analogies
can also be drawn between
stress-corrosion cracking (SCC)
of metals and stress cracking of
polymers. Other metal/plastic
failure analogies include corro-
sion/chemical aging, dealloying/
scission, residual stress/frozen-in
stress, and welds/knit lines. Stress raisers, microstructure, material defects, and thermomechanical history
play important roles in both types of materials. The key fractographic features for metals and plastics
are described in this paper.

Historical Perspective analysis methods. Although the cost working knowledge of fracture. Arch-
Plastics have been in existence for of failure analysis may exceed the eological findings of lithic imple-
approximately 130 years. John Hyatt value of the part, the cost of service ments, weapons, and tools shaped from
patented nitrocellulose, the first failures usually far exceeds the cost stone by controlled fracture indicate
commercial plastic, in 1869. However, of failure analysis. Many of the tech- that prehistoric man knew how to select
full-scale development and use of niques used over the years for the eval- rocks with favorable fracture behavior,
plastics is only approximately 50 years uation of metals have been success- use thermal spalling to detach bedrock
old. In contrast, metals have been in fully applied to plastics, with only from the working core, and shape stone
use for hundreds of years. minor modifications. by pressure flaking.

The application of engineering mat- Fractography is arguably the most Fractography, as we know it today,
erials is unavoidably accompanied by valuable tool available to the failure developed in the 16th century as a
the occurrence of failures, many of analyst. Fractography, a term coined quality-control practice employed for
which have been catastrophic. The in 1944 to describe the science of ex- ferrous and nonferrous metalworking.
consequences of material failures, in- amining fracture surfaces, has actually De La Pirotechnia, published by Van-
cluding deaths, financial losses, and been used for centuries as part of the noccio Biringuccio in 1540,[1] is one
legal ramifications, have encouraged field of metallurgy. Even before that, of the first documents to detail frac-
the development of effective failure however, Stone Age man possessed a tographic techniques.

16 Volume 2(5) October 2002 Practical Failure Analysis


Invention of the optical microscope orders of magnitude. The tools for by molecular bonding, and thermal
in 1600 provided a significant new modern fractography were essentially testing, differential scanning calori-
tool for fractography, yet it was not in place before plastics achieved wide- metry, and thermogravimetric analysis
used extensively by metallurgists until spread use. are also very important for polymer
the eighteenth century. In 1722, R.A. characterization. Energy-dispersive x-
de Réaumur[2] published a book with Failure Analysis Overview ray spectroscopy, used in conjunction
engravings that depicted macroscopic The general procedure for conduct- with the SEM, is a very practical tool
and microscopic fracture surfaces of ing a sound failure analysis is similar for elemental chemical analysis of
iron and steel. Interestingly, the cate- for metallic and nonmetallic mater- both metals and plastics. Also note-
gories of macroscopic features devel- ials. The steps include: (1) informa- worthy is that different chemical solu-
oped by de Réaumur have remained tion gathering; (2) preliminary, visual tions are required for metals and plas-
essentially unchanged through the examination; (3) nondestructive test- tics to clean and/or protect fracture
centuries. ing; (4) characterization of material surfaces and to etch cross sections to
Partly due to the development of properties through mechanical, chem- reveal microstructure.
metallographic techniques for exam- ical, and thermal testing; (5) selection,
ining cross sections of metals, interest preservation, and cleaning of fracture Causes of Failure
in microfractography waned during surfaces; (6) macroscopic examination Of course, the primary objective of
the nineteenth century. Metalworkers of fracture surfaces, secondary crack- a materials failure analysis is to de-
continued to use fractographic tech- ing, and surface condition; (7) micro- termine the root cause of failure.
niques for quality-assurance purposes, scopic examination; (8) selection, Whether dealing with metallic or
but, for the most part, researchers and preparation, and examination of cross nonmetallic materials, normally, the
publications ignored fractography. sections; (9) identification of failure root cause can be assigned to one of
Several technological developments mechanisms; (10) stress/fracture four categories: design, manufactur-
in the twentieth century revitalized mechanics analysis; (11) testing to ing, service, or material. Often, several
interest in fractography. Carl A. simulate failure; and (12) data review, adverse conditions contribute to the
Zapffe[3] developed and extensively formulation of conclusions, and re- part failure. Many of the potential
used fractographic techniques to porting. root causes of failure are common to
study the hydrogen embrittlement of Although the basic steps of failure metallic and nonmetallic materials.
steels. His work led to the discovery analysis are nearly identical, some Improper materials selection, overly
of techniques for photographing differences exist between metals and high stresses, and stress concentrations
fracture surfaces at high magnifi- plastics. Nondestructive testing of are examples of design-related
cations. The first fractographs were metals includes magnetic-particle, problems that can lead to premature
published by Zapffe in 1943. eddy-current, and radiographic in- failure. Materials selection must take
An even more revolutionary devel- spection methods that are not gener- into account environmental sensitivi-
opment was the invention of the ally applicable to plastics, for
scanning electron microscope (SEM). obvious reasons. However,
The first SEM appeared in 1943. ultrasonic and acoustic em-
Unlike the transmission electron mi- ission techniques find ap-
croscope, which was developed a few plications for both materials.
years earlier, it could be used for frac- Similarly, different chemical
ture surface examination. An SEM test methods are necessary.
with a guaranteed resolution of ap- Typical test methods for
proximately 500 Å became commer- metals are optical emission
cially available in 1965. Compared spectrometry, inductively
with the optical microscope, the SEM coupled plasma, and combus-
expands resolution by more than one tion. Fourier transform in-
order of magnitude and increases the frared spectroscopy is used Fig. 1 Fracture of a glass-filled polyamide threaded part
depth of focus by more than two extensively to identify plastics due to stress concentration at the thread root

Practical Failure Analysis Volume 2(5) October 2002 17


Fractography of Metals and Plastics (continued)

ties as well as requisite mechanical particularly in fatigue. Stress raisers Environmental degradation is one
properties and welding/joining char- include thread roots (Fig.1), sharp of the most important service-related
acteristics. Stress raisers are frequently radii of curvature, through holes, and causes of failure for metals and plas-
a preferred site for fracture origin, surface discontinuities (e.g., gate tics. Other degradation processes in-
marks in molded plastic parts). clude excessive wear, impact, overload-
Similarly, many manufac- ing, and electrical discharge.
turing and material problems
Failure Mechanisms
found in metals also are
observed or have a corollary Another key objective of failure anal-
in plastics. Weldments are a ysis is to identify the failure mechan-
trouble-prone area for metals, ism(s). Once again, some failure modes
as are weld lines or knit lines are identical for metals and plastics.
in molded plastics (Fig. 2). These modes include ductile overload,
High residual stresses can brittle fracture, impact, fatigue, wear,
result from metalforming, and erosion.
heat treatment, welding, and Analogies also can be drawn be-
machining. Similarly, high tween metals and plastics with regard
Fig. 2 Cross section showing fracture along the knit line of frozen-in stresses in in- to environmental degradation.
a perfluoralkoxyethylene-lined impeller jection-molded plastic parts Whereas metals corrode by an elec-
often contribute to failure. trochemical process, plastics are
Porosity and voids are com- vulnerable to chemical changes from
mon to metal castings and aging or weathering. Stress-corrosion
plastic molded parts (Fig. 3). cracking (SCC), a specific form of
Pores and voids serve as metallic corrosion, is similar in many
stress raisers and reduce ways to stress cracking of plastics.
load-carrying capability. Both result in brittle fracture due to
Other manufacturing- and the combined effects of tensile stress
material-related problems and a material-specific aggressive en-
that may lead to failure vironment. Similarly, dealloying or
include adverse thermomech- selective leaching in metals (Fig. 4),
anical history, poor micro- the preferential removal of one
structure, material defects, element from an alloy by corrosion,
Fig. 3 Cross section of a polyacetal hinge that fractured and contamination. is somewhat similar to scission of
(arrow) through an area of porosity
polymers (Fig. 5), a
form of aging that
can cause chemical
changes by selectively
cutting molecular
bonds.
Analogies can also
be drawn between
metals and another
type of polymer:
rubber. Internal hy-
drogen in steels can
Fig. 4 Microbiologically induced corrosion of a 304 SST precipitate and cause
vessel weld, characterized by pitting and selective Fig. 5 Hollowing out of a polyacetal hinge due to acid- hydrogen damage,
leaching (arrow) catalyzed hydrolysis which is frequently

18 Volume 2(5) October 2002 Practical Failure Analysis


characterized by localized brittle areas ture surfaces (Fig. 6). Similarly, explo- reinforced plastics and plastics
of high reflectivity, known as flakes sive decompression in rubber O-rings containing high filler content.
or fisheyes, on otherwise ductile frac- produces fisheye-like ovular patterns
on the fracture surfaces (Fig. Macroscopically Visible
7). Explosive decompression is Fractographic Features
the formation of small ruptures On a macroscopic scale, all fractures
or embolisms when an elasto- (metals and plastics) fall into one of
meric seal, saturated with high- two categories: ductile and brittle.
pressure gas, experiences an Ductile fractures are characterized by
abrupt pressure reduction. material tearing and exhibit gross
This failure mechanism is plastic deformation. Brittle fractures
analogous to the “bends” that display little or no macroscopically
afflict divers who surface too visible plastic deformation and
quickly. require less energy to form. Ductile
fractures occur as the result of applied
Fractography stresses exceeding the material yield
When material failure in- or flow stress. Brittle fractures may
Fig. 6 Hydrogen damage of induction-hardened steel volves actual breakage, frac- occur at stress levels below the material
piston rod displaying fisheyes tography can be employed to yield stress. In practice, ductile frac-
identify the fracture origin, tures occur due to overloading or
direction of crack propa- underdesigning and are rarely the
gation, failure mechanism, subject of a failure analysis. However,
material defects, environmen- the unexpected brittle failure of nor-
tal interaction, and the nature mally ductile materials is frequently
of stresses. Some of the mac- the subject of a failure analysis.
roscopic and microscopic Many macroscopically visible frac-
features employed by the tographic features serve to identify
failure analyst to evaluate the fracture origin(s) and direction of
fracture surfaces of metals crack propagation. Fractographic fea-
and plastics are described tures common to metals and plastics
subsequently. Note, however, are radial marks and chevron patterns.
that many of the fracto- Radial marks (Fig. 8) are lines on a frac-
Fig. 7 Explosive decompression fracture of rubber O-ring, graphic features described for ture surface that radiate outward from
characterized by fisheye-like patterns plastics are not observable for the origin and are formed by the in-
tersection of brittle
fractures propagating
at different levels.
Chevron or herring-
bone patterns are
actually radial marks
resembling nested
letter V’s and point-
ing toward the origin.
Fatigue failures in
metals display beach
marks and ratchet
Fig. 8 Beach and radial marks visible on torsional fatigue Fig. 9 Brittle fracture of an epoxy layer displaying a marks that serve to
fracture of a 6 in. diameter 4340 shaft mirror zone, rib marks, and hackles (continued on page 44)

Practical Failure Analysis Volume 2(5) October 2002 19


Fractography of Metals and Plastics (continued
(continued)
from page 19)

identify the origin and the failure coalescence. Ductile fracture in plas- may result from numerous failure
mode. Beach marks (Fig. 8) are mac- tics (Fig. 11) is characterized by mat- mechanisms, but there are only a few
roscopically visible semielliptical lines erial stretching related to the fibrillar basic microfractographic features that
running perpendicular to the overall nature of the polymer response to clearly indicate the failure mechan-
direction of fatigue crack propagation stress. Although a part may fail in ism. These features are cleavage facets
and marking successive positions of a brittle manner, ductile fracture (Fig. 12), intergranular facets (Fig.
the advancing crack front. Ratchet morphology is frequently observed 13), and striations (Fig. 14). Cleavage
marks are macroscopically visible lines away from the origin. For example, facets form in body-centered cubic
running parallel to the overall the final fast fracture by ductile (bcc) and hexagonal close-packed
direction of crack propagation and overload produces the shear lip in metals when the crack path follows a
formed by the intersection of fatigue many metal failures, even when the well-defined transgranular crystallo-
cracks propagating from multiple crack originated and was propagated graphic plane (e.g., the {100} planes
origins. by SCC, fatigue, or hydrogen em- in bcc metals). Cleavage is character-
Brittle fractures in plastics also ex- brittlement processes. The extent of istic of transgranular brittle fracture.
hibit characteristic features, several of this overload region is an indication Intergranular fracture, recognizable
which are macroscopically visible (Fig. of the stress level. Generally, the larger by its “rock candy” appearance, occurs
9). These features may include a mir- the overload region, the higher the when the crack path follows grain
ror zone at the origin, a mist region, stress level on the failed component. boundaries. Intergranular fracture is
and rib marks. The mirror zone is a Brittle fracture of metallic materials typical of many forms of SCC, hy-
flat, featureless region
surrounding the
origin and associated
with the slow crack-
growth phase of
fracture. The mist
region is located
immediately adjacent
to the mirror zone
and displays a misty
appearance. This area
is a transition zone
from slow to fast
crack growth. Rib Fig. 10 Dimpled appearance typical of ductile fracture of Fig. 12 Brittle fracture of an FC-0205 powder metal
marks are semi- metallic materials control rod displaying cleavage facets
elliptical lines re-
sembling beach
marks in metallic
fatigue fractures.
Microscopically
Visible
Fractographic
Features
On a microscopic
scale, ductile fracture
in metals (Fig. 10)
displays a dimpled
surface appearance Fig. 11 Fracture of a polyethylene tensile-test specimen Fig. 13 Intergranular fracture of an embrittled cast steel
created by microvoid exhibiting material stretching pneumatic wrench

44 Volume 2(5) October 2002 Practical Failure Analysis


drogen embrittlement, and temper- fications of 500 to 2,500× are re- physical boundaries with the ad-
embrittled steel. Fatigue failures of quired.) Striations are semielliptical vancing crack front. Conic marks are
many metals exhibit striations at high lines on a fatigue fracture surface that parabolic-shaped lines pointing back
magnifications. (Normally, magni- emanate outward from the origin and toward the origin. Hackles and
mark the crack-front position Wallner lines may or may not be visi-
with each successive stress ble without the aid of a microscope.
cycle. The spacing of fatigue
striations is usually ver y Closing Remarks
uniform and can be used to Fractographic techniques, develop-
calculate the crack growth ed and applied to metal failures for
rate, if the cyclic stress centuries, have been readily adapted
frequency is known. Stria- to the fracture analysis of plastics
tions are discriminated from since their emergence as a key engi-
striation-like artifacts on the neering material over the last 50 years.
fracture surface in that true However, more work remains to be
fatigue striations never cross done to advance fractography of
or intersect one another. plastics. One notable area for research
Fig. 14 Fatigue striations visible on type 302 stainless steel
Plastics do not display is fracture analysis of composites,
spring fracture
cleavage and intergranular reinforced plastics, and plastics con-
fracture. However, similar to taining high filler content. Fractures
metals, striations are found of these materials too often are
on fatigue fracture surfaces dismissed as inherently lacking
(Fig. 15, 16). Striations in meaningful fractographic features.
plastics typically are observ- Finally, there is a definite need for an
able at much lower magnifi- authoritative publication on fracture
cations (50 to 200×). How- in plastics.
ever, local softening and
melting due to hysteretic Acknowledgments
heating can obliterate fatigue The author gratefully acknowledges
striations in less rigid plastics. the contributions of Dave Christie
and Steve Ruoff of IMR Test Labs.
In addition to mirror
zones, mist regions, and rib References
Fig. 15 Fatigue striations emanating from fracture origin of
polycarbonate latch handle marks, which are normally 1. V. Biringuccio: De La Pirotechnia, Venice,
visible without the aid of a 1540; see translation by C.S. Smith and
microscope, brittle fracture of M.T. Gnudi: The ‘Pirotechnia’ of Vannoccio
Biringuccio, American Institute of Mining,
plastics may display hackles, Metallurgical and Petroleum Engineers,
Wallner lines, and conic New York, 1942.
marks. Hackles (Fig. 9) are 2. R.A. de Réaumur: L’Art de Convertir le Fer
divergent lines radiating Forgé en Acier, et L’Art d’Adocir le Fer Fondu,
outward from the fracture (in French), Michel Brunet, Paris, 1722;
origin. They are analogous to see translation by A.G. Sisco: Réaumur’s
Memoirs on Steel and Iron, University of
river patterns observed on the
Chicago Press, 1956.
cleavage facets of trans-
granular brittle fractures of 3. C.A. Zapffe and G.A. Moore: Trans.
AIME, 1943, 154, pp. 335-59.
metals. Wallner lines are
faint, striation-like markings Selected References
Fig. 16 SEM micrograph of fatigue striations shown in formed by the interaction of • W. Brostow and R.D. Corneliussen: Failure
Fig.15 stress waves reflected from of Plastics, Hanser Publishers, Munich, 1986.

Practical Failure Analysis Volume 2(5) October 2002 45


Fractography of Metals and Plastics (continued)

• T.J. Davies and I. Brough: “General Practice • F.R. Larson and F.L Carr: “How Failures • U. Portugall and K. Steinlein: Prac. Met-
in Failure Analysis,” Metals Handbook (9th Occur…Topography of Fracture Surfaces,” allography, 1999, 36(8), pp. 446-62.
ed.), vol. 11, Failure Analysis and Prevention, Source Book in Failure Analysis, American
American Society for Metals, Metals Park, Society for Metals, Metals Park, OH, 1974.
OH, 1986. Credit Info
th
• M. Ezrin: Plastics Failure Guide: Cause and • Metals Handbook (8 ed.), vol. 9, Fracto- Ronald J. Parrington, IMR Test Labs, 131
Prevention, Hanser Publishers, New York, graphy and Atlas of Fractographs, American Woodsedge Drive, Lansing, NY 14882. Con-
1996. Society for Metals, Metals Park, OH, 1974. tact e-mail: ron@imrtest.com.

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Sections include: Engineering Aspects of Failure and Failure Analysis,
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1996 • 1,057 pages Volume 12: Fractography
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1987 • 517 pages • ISBN: 0-87170-018-2 • ASM Publication
This volume contains the essential data necessary for you to make
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test data and helping you understand the key variables that affect the fracture mode to the microstructure. The Atlas of Fractographs
results. contains more than 1,300 fractographs invaluable for your understanding
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Engineering Aspects of Fatigue Life, Fracture Mechanics of Sections include: History of Fractography, Modes of Fracture, Prep-
Engineering Materials, Fatigue and Fracture Control, Castings, aration and Preservation of Fracture Specimens, Photography of
Weldments, Wrought Steels, Aluminum Alloys, Titanium Alloys and Fractured Parts and Fracture Surfaces, Visual Examination and Light
Superalloys, Other Structural Alloys, Solders, Advanced Materials. Microscopy, Scanning Electron Microscopy, Transmission Electron
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46 Volume 2(5) October 2002 Practical Failure Analysis