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FRACTOGRAPHY

Fractography of Brittle Materials:Analysis


of Fractures in Ceramics and Glasses
George D. Quinn, Ceramics Division, National Institute of Standards and Technology, Gaithersburg, MD, USA

BIOGRAPHY INTRODUCTION to make a permanent record of the breakage


George Quinn is a mas- Why did it break? Where is the fracture origin? pattern. In some instances, the breakage pat-
ter fractographer and Was there a problem with the material or was tern is all that is necessary and further exami-
has analyzed many com- the part overloaded or misused? A skilled frac- nation of fracture surfaces is unnecessary. For
mercial, military, and tographer can often give definitive answers to example, even novices can recognize an
research fracture prob- the above questions. The curse of brittle mate- impact site on an automobile windshield with-
lems. He is the author of rials is that they are prone to catastrophic frac- out examining the fracture surfaces. Often a
the newly published- ture. Nature has partially compensated for this simple visual examination can tell the observer
book ‘Guide to Fractography of Ceramics shortcoming by furnishing clear fracture pat- whether a component fracture was thermally
and Glasses’. As a ceramics engineer and terns and fracture surface markings that pro- or mechanically driven, whether the stress was
standards writer at NIST, he has crafted vide a wealth of interpretable information. In large or small, and whether the stresses were
many documentary standards for properties many respects, fractographic analysis of uniaxial (one primary tensile stress) or multi-
such as strength, fracture toughness, hard- ceramics and glasses is easier and can produce axial (two or more tensile stresses in different
ness, as well as procedures for fractographic more quantitative information than the frac- directions).
analysis. tographic analysis of metals or polymers. The fracture surfaces are examined to ascer-
The National Institute for Standards and tain the directions of crack propagation, the
ABSTRACT Technology (NIST) in the USA has published a stress state, and, ideally, the fracture origin,
The tools and techniques used to interpret new recommended practice guide to fractog- i.e. the source from which brittle fracture
fractured brittle materials are documented raphy of ceramics and glasses [1] to encourage begins. Various microscopy tools are used to
in new Recommended Practice Guide for and facilitate the greater use of fractographic examine features on the fracture surfaces of
the Fractography of Ceramics and Glasses. analysis of brittle materials. In this article, I brittle materials that are the direct conse-
Fractography is a powerful but underuti- give a brief overview of the principles of frac- quence of crack perturbations during propa-
lized tool for the analysis of fractured tographic analysis of ceramics and glasses with gation.
glasses and ceramics. It is applicable to frac- some practical illustrations of the methods An important element of fractographic
tures created under controlled conditions in used in fractographic analysis. analysis is pattern recognition. Certain types
the laboratory and to component failures in of fracture leave tell-tale fracture patterns on
service. Fractography can identify the origin PRINCIPLES OF FRACTOGRAPHIC the fracture surfaces or in the shapes and sizes
of fracture, the cause of failure, and can A N A LY S I S : T H E T O O L S of the fragments. The fracture surface on the
even provide quantitative information The principles of fractographic analysis are cover of the Guide (Figure 1) is a good exam-
similar for glasses and for single-crystal and ple. It shows the fracture surface of a ceramic
about the stresses in the part. Fractographic
polycrystalline ceramics. Examination of the rod that was broken by flexure. At the bottom
analysis requires pattern recognition and
fractured surfaces of broken pieces is an is a fracture mirror, a relatively smooth, semi-
the Guide includes many illustrations of
important element of fractographic analysis, circular region surrounding the fracture ori-
common and obscure patterns. The Guide
but much can be gleaned by first looking at gin. Attention is drawn to the origin by the
includes a full chapter on equipment and
the overall breakage pattern and the size and radiating hackle lines that were formed when
techniques used for fractographic analysis.
shape of the fragments. Conventional pho- the crack reached terminal velocity. On the
tography with film or digital cameras is used top, the crack progressed into what originally
KEYWORDS
light microscopy, stereomicroscopy, scan-
ning electron microscopy, fractography, Figure 1:
ceramics, glasses, brittle fracture, fracture The cover picture of the the
origin new Practice Guide: A stereo-
microscope image of the frac-
A U T H O R D E TA I L S ture surface of a ceramic rod
Mr George D. Quinn that was broken in flexure. At
Ceramics Division, the bottom is a fracture mirror,
Stop 8529, a relatively smooth semicircular
National Institute for Standards and Tech- region surrounding the fracture
nology, origin.
Gaithersburg, MD 20899, USA
Tel: +1 301 975 5765
Email: george.quinn@nist.gov

Microscopy and Analysis 22(4):21-24 (EU),2008

M I C R O S C O P Y A N D A N A LY S I S J U LY 2 0 0 8 21
was a compressively loaded portion of the rod Figure 2:
and the hackle lines disappear. The crack Stereomicroscope image of
curved over and formed a cantilever curl. The classical fracture markings in a
location of the origin can be determined in glass rod broken by flexure.
Figure 1, but microscopical analysis is needed
to discern the origin.
The most important tools of the fractogra-
pher’s craft are the binocular stereomicro-
scope and the scanning electron microscope.
The stereomicroscope affords to the eyes a
magnified, naturally appearing, three-dimen-
sional view of the fracture surface that retains
all color and reflectivity information. Its high
depth of field and broad magnification capa-
bilities makes it invaluable for viewing rough
fracture surfaces. Figure 2 is an image of a
glass rod broken in flexure that was recorded
by a digital camera mounted on a stereomi-
croscope. Although it is only a two-dimen-
sional image, it nonetheless provides a good
sense of the three-dimensional nature of the
fracture. Glass and ceramic fracture markings
are very similar, but the microstructure of the
latter create greater roughness on the fracture of photos at the same magnification are taken most common surface-origin flaws in glasses
surfaces (Figure 1) that masks some subtle frac- while slightly readjusting the focus in sequen- although internal-volume flaws sometimes
ture markings that are more easily seen in tial steps. The software interprets the regions cause fracture. Ceramics fracture from vol-
glasses. that are in focus and stitches these together to ume-, surface-, or edge-distributed sources.
Fracture origins and flaws in ceramics and create a single focused image. Microstructural irregularities or inclusions are
glasses can be detected with the stereomicro- often the internal fracture origins. The frac-
scope, but higher magnifications are often F R A C T O G R A P H I C A N A LY S I S : ture origin is the site that had the worst com-
needed to see the flaw clearly. The scanning SOME EXAMPLES bination of tensile stress and flaw severity. The
electron microscope serves this need and has Hackle lines form on the fracture surface run- latter is determined by the flaw size, shape,
excellent depth of field, high magnification ning in the local direction of cracking, sepa- and thermoelastic or chemical interactions
capability, and chemical analysis features. rating parallel but non-coplanar portions of with the matrix. A large flaw may not neces-
Other tools such as hand magnifiers, com- the crack surface. Figure 3 shows one form sarily trigger fracture, especially if it is located
pound optical microscopes, or even atomic termed wake hackle. The crack encountered in a portion of a part that has low stress or it is
force microscopes play supportive roles. The round pores as it traversed through a glass very blunt, such as a spherical pore. The sever-
Guide [1] has an entire chapter on the various body. The crack ran around and to either side ity of a flaw and whether local stresses are suf-
tools and techniques for fractographic of the pores but linked up on the downstream ficient to trigger fracture are determined by
analysis. side with a small step that trailed away from the principles of fracture mechanics. Figures 4
Dramatic advances in digital camera tech- the pore as the crack ran further. Wake hackle and 5 show flaw origins in glass and a poly-
nology and computer software, memory and lines are convenient ‘weather vanes’ showing crystalline ceramic, respectively.
processing speeds are revolutionizing imaging the direction of crack propagation. Some of our work has recently focused on
technology. The new technologies are quite The majority of brittle fractures start at one strength test method miniaturization for
affordable, are rendering film photography origin and radiate outward. Severe thermal MEMS scale and smaller structures [2,3]. An
obsolete, and are opening up new capabilities stresses or impact loadings can create multiple attractive test method is the theta specimen
not heretofore available. The shortcomings of origin sites. Contact-damage cracks, scratches, shown in Figure 6. This clever configuration
conventional compound microscopes (e.g. lim- polishing flaws, and grinding cracks are the was invented by Durelli and Parks in the 1960s
ited depth of field) or of scanning electron
microscopes (e.g. flat-appearing images) can
be overcome or mitigated. The blending of Figure 3:
optical microscopy with the new digital imag- Wake hackle lines from pores
ing technologies is leading to clever new in a glass. This stereomicro-
microscope designs based upon interferome- scope image shows both the
try or the processing of multiple images. For fracture surface and some
example, virtual three-dimensional images can pores beneath the surface. The
be created by a confocal microscope, an auto- wake hackle steps formed
matically rastering optical microscope, or by where the crack intersected
analysis of multiple images from a scanning some of the pores. The arrow
electron microscope taken with slightly differ- shows the direction of crack
ent specimen tilts. Pseudo three-dimensional propagation.
images can be displayed, tilted and rotated to
afford different perspectives. Various quanti-
tative numerical analyses of surface topogra-
phy (e.g. surface roughness or even fractal
dimension analysis) can be performed at
almost no extra effort since the surface topog-
raphy has been recorded digitally. Simple low-
cost software programs are now available that
can conveniently overcome the depth of field
limitations of virtually any microscope. A series

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FRACTOGRAPHY
for testing brittle materials [4] and had the Figure 4:
advantage that elaborate grips to apply load Stereomicroscope image of a
were unnecessary. One merely needs to com- nickel sulfide inclusion that was
press the specimen on its rim. The configura- the fracture origin in a plate of
tion never caught on since it is very complex to tempered glass.
prepare and is inefficient in its use of material.
Only a tiny portion in the middle is loaded in
pure tension.
We have resurrected this configuration since
it is ideal for testing tiny structures. We have
prepared single-crystal silicon test coupons
prepared by deep reactive-ion etching (DRIE)
procedures. Preliminary work has been done
on other materials and preparation proce-
dures. Figure 6b shows a fracture origin in one
of the broken theta specimens. The field-emis-
sion scanning electron microscope image
reveals a cathedral fracture mirror. Fracture
mirrors in single crystals can have many forms
depending upon the plane of fracture and
whether or not a fracture is on a preferred
cleavage plane. The origin flaw was a 250-nm
deep surface pit formed by the DRIE etching
procedure in the side wall of the test coupon.
The Guide has an entire chapter on the topic
of fractography of brittle single crystals. Many
more theta specimens fracture origins are
shown in [3]. The etch pits tended to form
rows in the side walls that ran perpendicular
to the side wall bands that develop as a result
of the sequential DRIE etching and passivation
steps.
Quantitative fractographic analysis can pro-
vide much information. The angles of crack
branching can reveal whether a part was uni-
axially or biaxially loaded. The size of the frag-
ments can be used to estimate the energy and
stress at fracture. One of the most remarkable
tools is fracture mirror size analysis. The local
stress s at the fracture is inversely related to
the square root of the fracture mirror radius R
by the formula:

where A is the ‘mirror constant’ with units of


stress intensity (MPa m0.5 or ksi in0.5) and is con-
sidered by most to be a material property. This
relationship, now known as Orr’s equation,
has tremendous practical significance. The
mirror radius may be measured from a frac-
ture surface, the mirror constant found from a Figure 5:
data table, and then the origin stress calcu- Scanning electron microscope image of the pore fracture origin in an aluminum oxynitride ceramic bend bar. In addition to the obvious large flaw,
lated. notice the tiny wake hackle lines triggered by the microstructure that radiate away from the large flaw.
So, for example, the mirror radii of the two
fracture mirrors shown in Figures 1 and 2 may
be used to get estimates of the fracture digital camera on a compound optical micro- Using the radii along the surface to both sides,
stresses, accurate to within 10%, without even scope with brightfield illumination, the best and ignoring minor surface irregularities, one
knowing how the parts were loaded! The his- examination condition for glasses. The slight obtains a radius estimate of 236 micrometers.
tory of how this relationship was derived is elongation of the mirror shape in the vertical Using a mirror constant of 1.9 MPa m0.5, one
covered in detail in the Guide [1]. Although direction is a consequence of the bending obtains a fracture stress of 124 MPa.
Johnson and Holloway offered a physical stress gradient in the rod. The mirror, mist, and Mirror constants for many materials, recom-
interpretation of the relationship based on hackle regions are shown and the mirror-mist mendations for ceramics, illumination and
the energetics of crack propagation in 1966 boundary is marked by the dashed line. photographic recommendations, and instruc-
[5], Leighton Orr of the Pittsburg Plate Glass The word ‘boundary’ must be used with tions on how to deal with asymmetric mirrors
Company had discovered the relationship and some caution. It is now clear from a number of and residual stresses are all included in the
used it to solve many glass fracture problems studies that there probably is not a discrete or Guide [1].
as far back as the mid 1940s. sudden transition point on the fracture surface
Figure 7 shows a fracture mirror centered on corresponding to a mirror boundary. The CONCLUSIONS
a surface flaw in a fused silica rod broken by mode of viewing and magnification affects Fractographic analysis is the science of inter-
bending. The photograph was made with a the judgement of the boundaries’ location. preting the fracture surfaces, the overall

M I C R O S C O P Y A N D A N A LY S I S J U LY 2 0 0 8 23
a b

Figure 6:
Single-crystal silicon theta specimen. (a) A compound optical microscope frontal view. The ring is supported on the bottom and is compressed at the top in the testing apparatus. When loaded, the sides expand outwards putting
the horizontal middle web into pure tension. The web is 7.3 µm tall by160 µm long. (b) A 250-nm deep fracture origin as imaged by a field-emission scanning electron microscope.

breakage patterns, and as much background a


information about the processing, the
microstructure and the testing or service con-
ditions as possible.
Most people recognize that fractography is
a valuable tool for failure analysis, but fewer
appreciate its value in routine mechanical test-
ing or support of materials processing.
Although thousands of ceramic or glass items
and test specimens are broken daily, only a tiny
fraction is examined fractographically. A
wealth of information is lost about the causes
of fracture and the nature of the material. The
flaw type may be just as important as the frac-
ture stress in a strength test.
When a fractographer first sees broken frag-
ments, he or she sees pieces that are trying to
tell a tale. With good microscopy equipment
and with the fractographic skills summarized
in the new NIST Guide, a fractographer can lis-
ten to the pieces, interpret their story, and
unlock the secrets of the fracture.

REFERENCES
Figure 7:
1. Quinn, G. D. Fractography of Ceramics and Glasses. National b
(a) Brightfield compound optical
Institute of Standards and Technology Special Publication
microscope image of the fracture mir-
960-16, 2007, NIST, Gaithersburg, MD 20899, USA. Printed
ror in a fused silica rod showing the
copies are available at no cost on request from: www.nist.
hackle, mist and mirror compart-
gov/public_affairs/practiceguides/practiceguides.htm
ments.
PDF versions also are available from the same website.
(b) Stereomicroscope reflected light
2. Quinn, G. D. et al. A Novel Test Method for Small Scale
image of the whole fracture surface.
Structures: The Theta Specimen. Ceram. Eng. and Sci. Proc.
26(2):117-126, 2005.
3. Quinn, G. D. Fractographic Analysis of Miniature Theta
Specimens. Submitted to Ceram. Eng. and Sci. Proc., Jan.
2008.
4. Durelli, A. J. et al. The Theta Specimen for Determining
Tensile Strength of Brittle Materials. Mat. Res. and Stand
2:114-117, 1962.
5. Johnson, J. W. and Holloway, D. G. On the Shape and Size of
the Fracture Zones on Glass Fracture Surfaces. Phil. Mag.
14:731-743, 1966.
©2008 John Wiley & Sons, Ltd

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