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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
22 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
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:
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.
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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