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J O U R N A L O F M AT E R I A L S S C I E N C E : M AT E R I A L S I N E L E C T RO N I C S 1 1 ( 2 0 0 0 ) 2 9 1 ± 3 0 3

Probabilistic strength of {1 1 1} n-type silicon


A. A. WERESZCZAK*, A. S. BARNES 1 , K. BREDER**
Mechanical Characterization and Analysis Group, Oak Ridge National Laboratory, Oak Ridge,
TN 37831-6069, USA
E-mail: awerzak@arl.mil
SUKHMINDER BINAPAL
Gennum Corporation, Burlington, Ontario, Canada L7R 3Y3

The two-parameter Weibull strength distribution of {1 1 1} n-type silicon prismatic bars was
determined in four-point bending and analyzed as a function of specimen size (width),
loading rate, two different crystallographic orientations, and specimen orientation ( polished
or etched surface in tension). 100% fractography was performed to classify strength-limiting
¯aw types and to censor the strength data. All ¯aw types were extrinsic. Machining or cutting
damage in the form of chipped edges (an edge-type ¯aw) was the dominant strength-limiting
¯aw when the polished surface was subjected to tensile stress, while a ¯at-bottomed etch pit
(a surface-type ¯aw) was the dominant strength-limiting ¯aw when the etched surface was
subjected to tensile stress. The censored Weibull strength distribution was independent of
specimen width, loading rate (indicative of slow crack growth insusceptibility), and the two
crystallographic orientations; however, it was dependent on specimen orientation. Pooling
of the strength data was employed to tighten the con®dence intervals about the censored
parameters. The results from this study indicate that different extrinsic strength-limiting
¯aws and strength distributions will be operative depending on the manner in which a silicon
component is stressed.

1. Introduction process involves Au-Au thermo-compression bonding


The mechanical reliability of silicon and silicon devices while the wire bonding process typically involves
may be problematic during both device fabrication and thermo-compression or thermo-sonic methods. Both
service. Silicon is a classic brittle material (i.e., has a low these processes exert a combination of compressive
fracture toughness), meaning it is linear elastic until and tensile stresses on the silicon chip. Obviously it is
catastrophic fracture, and its fracture is not determinis- highly desirable that the bonding stresses do not exceed
tically predictable. During fabrication or service, if the silicon's probabilistic tensile strength to avoid damaging
applied tensile stresses exceed the probabilistic tensile the bulk or the underlying thin ®lm structures.
strength of silicon (limited by the presence of pre- Most of the silicon packages require mechanical and
existing ¯aws), then failure will occur [1]. It is desirable environmental prsotection, so molding or encapsulating
to be able to design for allowable stresses or to predict polymers are often used. Typical molding and encapsula-
service mechanical reliability by taking into account the tion processing involves applying the polymer materials
probabilistic nature of silicon's strength. on the assemblies then curing at elevated temperatures,
Failure can occur in the silicon during its wafering, cell typically around 160±175  C. The molded or encapsu-
processing, or module preparation [1±2]. For example, lated silicon chips and other components of the assembly
silicon chip cracking is sometimes observed during the are exposed to thermally induced stresses due to thermal
``die preparation process''. This process involves expansion coef®cient mismatches between the molding
mounting processed silicon wafers on a slice frame and compound, silicon, and carrier substrates. Consequently,
then dicing them into individual chips. Cracking is the thermal stresses must not exceed the strength of
sometimes observed during the process of picking up the packaged components for reliable assemblies.
diced chip from the slice frame tape and placing it into a Concerns have increased as integrated circuits have
waf¯e pack. It is assumed that chips fracture when the become larger in size with higher component densities
pick-up vacuum tip and poking pins on the bottom apply and device complexity and are utilized in harsher
contact or tensile stress in excess of the probabilistic thermo-mechanically demanding service conditions [2±
tensile strength. Silicon chip cracking has also been 4]. Cracking or mechanical failure of the silicon can lead
reported during the re¯ow process of ¯ip chip assemblies to modi®cation of the device's electrical response or
due to chip edge ¯aws [3]. even the complete loss of electrical function [5]. Chip
Typical applications for diced silicon chips are chip on cracking and crating has been reported during the ILB
board (¯ip chip/wire bonding), inner lead tab bonding process due to excessive temperature settings and/or
(ILB), and wire bonding for standard packages. The ILB thermode force settings.
0957±4522 # 2000 Kluwer Academic Publishers 291
Service mechanical reliability of silicon devices is also bar specimens were nominally 25 mm in length and were
of interest in enabling applications in the ®eld of machined to one of three widths: 2.0, 3.0, and 5.0 mm
microsystems technology (MST). Micromachined (i.e., strength examined as a function of specimen width).
silicon devices can be subjected to complex service The thickness of all wafers or specimens was 0.53 mm.
stresses which can cause their fracture and loss of Prior to the bend bar cutting, an adhesive sheet was
component functionality. It is very desirable to under- mounted on the polished surface; this facilitated keeping
stand the mechanical limits and strengths of silicon as an specimens in place during their sectioning, and also
engineering material [6] as applications for MST become protected them from pre-testing handling damage. Bend
more diverse and complex, including temperature bar specimens were cut from wafers in one of two
transducers, microphones, stress sensors, and chemical crystallographic orientations; the long dimension of the
sensors. bend bar perpendicular or parallel to 51 1 24. The
The intrinsic fracture of single crystal silicon is crystallographic orientations were veri®ed using the
controled by the cleavage of preferred crystallographic Laue technique [14]. The bend bar specimen widths and
planes. Improvements in technology have created a crystallographic orientation with respect to the original
®nished wafer which is virtually free of dislocations. The wafer are illustrated in Fig. 1.
intrinsic strength of the crystallographic planes in such a All strength testing was performed in four-point
single crystal is proportional to their respective surface uniaxial ¯exure in ambient air (25  C, 50±60% RH)
energies, with the preferred plane of fracture (i.e., the using a universal test machine3 and adhered to ASTM
weakest) having the fewest number of bonds per unit C1161 [15] with the exception of specimen size and span
area. The preferred cleavage plane in silicon is {1 1 1}, width. Each specimen was carefully placed in the ®xture
which has a surface energy of 1:23610ÿ4 J cmÿ2 [7]. with tweezers (which gripped their end outside of the
Interest existed in the present study to determine if, and specimen's test area). Cloth gloves were used at all times
how, the strength of the {1 1 1} affected the failure event during specimen handling to minimize the likelihood of
and subsequent strength distribution. any handling damage and skin-oil contamination. The
The goal of the present study was to determine the four-point bend ®xture had an upper and lower span of
two-parameter Weibull strength distribution of post- 3.0 and 6.0 mm, respectively. The measured maximum
processed silicon wafers. Such an extreme-valued load P†, span dimensions for the upper LU † and lower
distribution is typically used to represent the strength LL † ®xture spans, and the dimensions of the specimen
of classic brittle materials (i.e., low fracture toughness) width b† and height h† were combined to calculate
such as monolithic ceramics and silicon. Additionally, fracture strength S† using the classical beam bending
fractography was performed to identify and classify the equation for four-point loading,
strength-limiting ¯aws which cause fracture in the
3P LLÿLU
silicon, and to censor the strength data. Several articles Sˆ 1†
have been published concerning the strength of silicon 2 bh2
wafers after various chemical or thermal treatments The loading rollers had a diameter of 0.78 mm (i.e., 50%
[2, 8, 11]; however, fewer articles are available which larger than the thickness of the silicon specimens), and
investigate silicon's post-processing strength [12±13]. were free to rotate during testing.
The present study examined the effects of specimen size, The measurement of strength as a function of test rate
loading rate, crystallographic orientation, and surface was the fourth independent parameter examined. The
condition on the tensile surface (etched or polished side
in tension) strength. These results are amenable for use
by package designers and end-users to optimize or
predict the pre-service and service probabilistic mechan-
ical reliability of silicon devices.

2. Procedure
Bend bar specimens were sectioned from {1 1 1} n-type
silicon wafers in a manner to facilitate the analyses of
strength dependence on three of the four independent
parameters studied: specimen width, crystallographic
orientation, and specimen orientation. One side of the
wafer was polished while the other was etched (and
contained ¯at-bottomed pits). The strength character-
istics of both surfaces were examined in tension via
¯exure testing (i.e., strength examined as a function of
specimen orientation). A nickel-bonded diamond blade
was used for the specimen dicing or sectioning. It had a
40 mm width, was 108 mm in diameter with an arbor
diameter of 76.2 mm, and contained a diamond grit size
of 3±6 mm. The feed rate during specimen cutting was
5 cm min ÿ 1 and a spindle speed of 30 000 r.p.m. was Figure 1 Schematic drawing showing bend bar specimen widths and
used. The edges were not rounded or chamfered.2 Bend orientations with respect to the silicon wafer.

292
inert (or ``fast-fracture'') strength testing was performed 3. Results and discussion
in displacement control using a test displacement rate of 3.1. Validity of strength testing
0.5 mm min ÿ 1. To examine the activity of any time- The cumulative experimental error associated with the
dependent loss of strength, the strength of the silicon utilized test ®xture was analyzed and deemed to be 2% or
specimens was also measured at two slower rates: 0.05 less based on issues of de¯ections due to the used span,
and 0.005 mm min ÿ 1. Loss in strength with decreasing friction, wedging stresses, and contact point tangency
test or stressing rate is indicative of slow crack growth shifts [15, 20, 21]. If the ratio of the lower to upper span
susceptibility (i.e., time-dependent loss in strength), and LL =LU † ®xture dimensions is too low, then loading point
an established strength analysis and data reduction stresses increase and localized contact-crushing can
procedure was utilized to examine this [16]. occur and produce an invalid fracture strength event
A summary of the specimen and test conditions is and value. If LL =LU is too high, then excessive de¯ection
shown in Table I. Sixteen different test conditions were can occur at the moment of fracture, and result in errors
examined and a minimum of thirty specimens were associated with non-linearity being introduced into the
tested for each.4 Strength was measured as a function of calculation of strength. The use of the 3:6 mm span
specimen width, test rate, crystallographic orientation, dimensions resulted in the maintenance of elastic beam
and specimen orientation via these conditions. A bending and the avoidance of specimen/roller contact-
minimum of thirty specimens per condition was chosen crushing.
because this number yields acceptable statistical con- Other mechanical tests were considered prior to the
®dence estimates of the Weibull distribution parameters employment of four-point-¯exure testing. Standard test
[17]. methods, such as ASTM F417 three-point [22] and
The fracture surfaces of each specimen (472 total) ASTM F394 biaxial ¯exure [23], exist for the strength
were examined using optical microscopy to identify the testing of brittle electronic grade materials. For the
fracture location and its strength-limiting ¯aw. present study, four-point-¯exure was preferred over
Fractography and ¯aw identi®cation guidelines speci®ed three-point-¯exure because it inherently subjects a
in ASTM C1322 were adhered to [18]. Possible failure larger volume, surface area, and edge length to the
locations were sought within the specimen volume, on its maximum outer ®ber tensile stress. The biaxial ¯exure
tensile surface, or along one of the two cut edges strength testing (a ``ring-on-ring'' con®guration) of
subjected to tensile stress. Due to the small size of many uncut silicon wafers was attempted after careful design
of the strength-limiting ¯aws, numerous fractured considerations of the ring-on-ring ®xture dimensions.5
samples were additionally examined at higher magni®ca- However, when the polished surface was tested in biaxial
tions with a scanning electron microscope. ¯exure, the wafer was so strong that excessive
The two-parameter Weibull distribution ( parameters: de¯ections occurred and the top ring eventually
Weibull modulus and scaling parameter) for both ``punched'' through the silicon specimen resulting in
uncensored and censored strengths were determined the production of many dozens, if not hundreds, of
using the CERAMIC computer program [19] which silicon fragments. Adhesive tape was then mounted on
calculates the distribution parameters along with their one surface of several additional wafers in an effort to
con®dence intervals using maximum likelihood estima- retain the fragmented pieces of wafer after its fracture.
tion. These strength distributions were then compared as After these additional biaxial tests, this tape-retainment
a function of width, test rate, crystallographic orienta- procedure exhibited a ring-oriented pattern of fragments
tion, and specimen orientation. whose diameter was the same as the upper ring's

T A B L E I Summary of the specimen and test conditions examined to measure strength.

Specimen width (mm) Testing rate (mm min ÿ 1) Orientation Surface tested in tension No. of samples

2 0.5 h 1 1 0 i* Etched 32
2 0.5 h110i Polished 32
2 0.05 h110i Polished 30
2 0.005 h110i Polished 31
3 0.5 h110i Etched 30
3 0.5 h110i Polished 30
3 0.05 h110i Polished 24
3 0.005 h110i Polished 24
5 0.5 h110i Etched 33
5 0.5 h110i Polished 31
5 0.05 h110i Polished 31
5 0.005 h110i Polished 30
5 0.5 h 1 1 2 i{ Etched 30
5 0.5 h112i Polished 33
5 0.05 h112i Polished 31
5 0.005 h112i Polished 30

*h 1 1 0 i orientation denotes samples with their longer dimension cut parallel to h 1 1 0 i or perpendicular to the wafer's primary ¯at.
{h 1 1 2 i orientation denotes samples with their longer dimension cut parallel to h 1 1 2 i or parallel to the wafer's primary ¯at.

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diameter; thus, the biaxial ¯exure strength test was concern that the contacting points, and the consequential
concluded to be an invalid test type for these silicon localized stresses they produced, may have been the
wafers because the ring itself caused the fracture, not a source of fracture initiation which would have produced
strength-limiting ¯aw in or on the specimen. a misleading strength distribution. The authors avoided
Others have employed biaxial ¯exure testing for these potential problems by appropriately employing
strength testing of silicon; however, many of the results four-point-¯exure in the present study.
were insuf®ciently reported, so it is dif®cult to interpret
or accept their validity. McLaughlin and Willoughby's
[8] biaxial ¯exure testing of (1 0 0) p-type silicon
3.2. Flaw-types and surface and edge
produced hundreds of fragments which creates concern
characteristics
that linear elasticity or contact-crushing-avoidance or
A signi®cant portion of the discussion of the uncensored
both were violated (similar to what the present authors
and censored strength distribution results relies on the
experienced). Chen and Leipold [12] and Chen [24]
untested silicon's surface and edge characteristics, as
performed biaxial ¯exure prooftesting on silicon wafers
well as the identity of the extrinsic strength limiting
using ASTM F394 and determined an uncensored
¯aws. Consequently, the discussions of these character-
Weibull strength distribution. However, it is unclear
istics, ¯aw-types, and correspondingly used designations
whether the strengths were valid because no fractography
are presented prior to the strength distribution results.
was conducted, and there was no mention of the ratio of
de¯ection at fracture to the specimen width (desired to be
less than 1/2 to maintain linear elasticity). Additionally,
there was no supplemental report of the wafer's surface 3.2.1. Intrinsic and extrinsic ¯aws
roughness with the reported estimated critical ¯aw sizes Although both intrinsic and extrinsic ¯aws limit the
( & 2±5 mm). The authors in the present study have strength of all polycrystalline brittle or ceramic materials

Figure 2 Examples showing the edge where (a) the polished surface and (b) the etched surface intersects the cut surface. A comparison (c) of the
surface roughness of the polished and etched surface and (d) the surface roughness of the polished surface at a ®ner scale.

294
and components, extrinsic ¯aws usually limit the silicon wafer in service, and its associated strength
strength of single crystal brittle materials. Intrinsic distributions, of course, is of paramount interest for
¯aws are inherent to brittle materials, are typically probabilistic design and mechanical reliability analysis:
volume-based, and may be volume-, or surface-, or edge- if these ¯aws are extrinsic, then the exploitation of
located. Examples of intrinsic ¯aws in polycrystalline intrinsic ¯aws and the determination of their associated
brittle materials are pores and relatively large grains. strength distributions are actually not required. For
Extrinsic ¯aws are extraneous to the material, and may example, if the failure of silicon wafers in service
be volume-, surface-, or edge-located (usually, the latter originates from stresses applied to edge-¯aws, then the
two locations). Examples of extrinsic ¯aws are foreign strength distribution dictated by those edge ¯aws needs
body inclusions in the volume, machining damage or to be determined. Although the determination of strength
grinding grooves on the surfaces, and machining-induced distributions for intrinsic ¯aws in silicon would be of
edge chips on the edges. Flaws which are a consequence academic interest, they are not applicable for service
of the act of mechanical testing itself (e.g., contact mechanical reliability analysis because extrinsic ¯aws
damage from a bend ®xture's roller or loading ball) are are likely to be larger and would limit the silicon's
also extrinsic ¯aws. For defect-free single crystal brittle mechanical performance.
materials such as silicon, extrinsic ¯aws such as
machining damage or edge chipping (i.e., surface- or
edge-located ¯aws) will limit its strength. For surface-
located ¯aws which limit the material's strength, 3.2.2. Surface and edge characteristics of
the local uniaxial stress state is inversely related as-received silicon
to the square of the ¯aw size according to the Grif®th The condition of the silicon wafer's surfaces was the
equation, source of the extrinsic strength limiting ¯aws (there were
no operative intrinsic or volume ¯aws limiting the
K strength of these specimens). The edges where the
s ˆ pIc 2†
Y c polished and etched surfaces intersect the cut surface are
shown in Figs 2a and b, respectively. The qualitative
where s is the applied maximum tensile stress or surface roughness of the polished and etched surfaces
strength, KIc is the material's fracture toughness, Y is a was measured using a surface pro®lometer6 over a
crack geometry factor (Y ˆ 29 for a surface-located, scanned distance of 1.2 mm. The qualitative differences
semi-circular ¯aw), and c is the ¯aw depth in this in the roughness of the two surfaces are shown in Fig. 2c
context. Literature reports the fracture toughness of which shows the roughness of the polished surface is
silicon to be a function of crystallographic orientation but signi®cantly less than that for the etched surface. A ®ner
in the range of &1:0+0:2 MPaHm [25±26]. The scale of the roughness of the polished surface is shown in
strength of silicon wafers or components will then Fig. 3d. The depth of the etch pits is approximately 5 m
depend on their surface or edge conditions; a ®nely while the depth of the roughness on the polished surface
polished surface which is ¯exed will produce a higher is two orders of magnitude ®ner at approximately 50 nm.
strength than a coarser polished surface because c will be Using these values as examples of strength-limiting ¯aw
lower. sizes in Equation 2 results in strengths of approximately
The intrinsic strength of defect-free single crystal 350 MPa and 3500 MPa for etched and polished surfaces,
silicon is high (bulk strength due to dislocations & 3± respectively, for a KIc ˆ 1:0 MPa Hm (latter strength
4 GPa and theoretical strength & 32 GPa [27]), and is value approaching that of dislocation-limited strength
almost impossible to measure using conventional [27]).7 Although the latter strength is an order of
specimen preparation and strength-testing techniques magnitude larger, it is still a strength value which is
due to its high value. The intrinsic defects are typically limited by an extrinsic ¯aw. The authors recognize that
much smaller than extrinsic defects (which are different ¯aw geometries will affect the value of Y in
typically a consequence of the specimen preparation Equation 2 and the above discussion of calculated
process or mechanical testing). Furthermore, the test strengths from the pro®lometry data. However, the
®xture used to apply the failure stress to the specimen strengths when considering a very severe case such as
must not produce strength-limiting damage (e.g., a long elliptical ¯aw (Y ˆ 1:99 [18] instead of 1.29)
contact-crushing, scratching from contacting friction decreases the above calculated strengths to approxi-
of the loading rollers, etc.). Wilson et al., [13] mately 225 and 2250 MPa for etched and polished
performed an interesting and unique fracture testing surfaces, respectively.
examination of silicon microcantilever beams; although The chipping on edges (which resulted from the bend
surface roughness and fracture markings were exam- bar machining) was the source of a strength-limiting
ined, no ¯aw identi®cation fractography results were ¯aw. An example of the chipping is evident on the
reported, so the reader is unable to conclude if the specimen edge shown in Fig. 2a. The size of these
surface or edge characteristics or intrinsic ¯aws limited chips on the specimen edges was much larger than the
the strength. Fractography is the only way to & 50 nm surface roughness of the polished surface, so
unequivocally identify intrinsic or extrinsic ¯aws; if they limited the strength when the polished surface was
not conducted or reported, then one should conserva- tested in tension. Such chipping of (1 1 0) and (1 0 0)
tively assume that unidenti®ed extrinsic ¯aws are silicon wafers occurs more readily than for (1 1 1) silicon
limiting the silicon's strength. wafers [4], so it may be argued that increased dominance
The exploitation of the strength-limiting ¯aw(s) of the of the edge ¯aw in (1 1 0) and (1 0 0) silicon wafers would
295
Figure 3 Four distinct ¯aw types limited the strength of the silicon: (a) edge, (b) surface 1, (c) surface 2, and (d) surface 3. The dominant ¯aw types
when the polished and etched surfaces were tested in tension were edge and surface 1 ¯aws, respectively.

be expected over its dominance with the (1 1 1) silicon


wafers in the present study.
The dominance of one strength-limiting ¯aw over
others was a consequence of the differences in the
surface roughness of both sides, and their relative
severity compared to that of the depth of the chips on
the silicon bend bar edges.

3.2.3. Strength-limiting ¯aw types


Four distinct strength-limiting ¯aw types were observed
during fractography of the 472 silicon bend specimens
and all were extrinsic ¯aws; one was a corner ¯aw, and
the remaining three were different surface-type ¯aws.
These four ¯aw types were de®ned in the present study as
``edge,'' ``surface 1,'' ``surface 2,'' and ``surface 3''
¯aws, and representative examples of each are shown in
Figs 3a to d, respectively. The edge ¯aw was the result of Figure 4 A representative example showing the trends that uncensored
machining or cutting damage in the form of chipped Weibull modulus and characteristic strength was lower and higher,
edges; it was the dominant ¯aw when the polished respectively, for the polished surface than the etched surface.

296
surface was tested in tension. An oblique perspective of censored strength) was analyzed as a function of
these chips or edge ¯aws is also shown on the edge in specimen size (width), test rate, crystallographic orienta-
Fig. 2a. The surface 1 ¯aw was a ¯at-bottomed etch pit tion and specimen orientation.
which initiated fracture; it was the dominant ¯aw when Parameters may be added to Equation 3 to yield a
the etched surface was tested in tension. The surface 2 censored Weibull distribution representation which
¯aw was due to contacting damage caused by one of the accounts for how the specimen was loaded, what its
loading rollers; it was rarely active (caused fracture in size was, and whether an edge-, surface-, or volume-¯aw
only 4 of the 472 specimens). The surface 3 ¯aw was caused the specimen's failure. The two-parameter
located on the cut surface; it also was rarely active Weibull distribution representation for specimen
(caused fracture in only 9 of the 472 specimens). The strengths limited by edge-¯aws is:
strengths were censored with respect to these four ¯aw
Pf ˆ 17 exp‰7kL L S=sOL †m Š 4†
types.
where kL is an edge multiaxial and stress gradient factor,
L is the specimen's total edge length, and sOL is a scaling
3.3. Uncensored statistics parameter for edge ¯aws. The nature of edge loading, its
Uncensored statistical results provided insights into the subsequent stresses, and their dependence on the Weibull
trends in strength; however, they inherently did not modulus are accounted for in kL . The Weibull distribu-
acknowledge specimen size and dominant ¯aw type tion for the edge ¯aw shown in Fig. 3a is represented by
differences among the 16 test conditions, so only Equation 4. The two-parameter Weibull distribution
qualitative judgments were allowed from their examina- representation for strengths limited by surface-¯aws is:
tions and comparisons. The uncensored two-parameter
Weibull distribution for each test condition was Pf ˆ 17 exp‰7kA A S=sOA †m Š 5†
represented by,
where kA is a surface multiaxial and stress gradient
m
Pf ˆ 17 exp‰7 S=sy † Š; 3† factor, A is the specimen's total surface area, and sOA is a
scaling parameter for surface ¯aws. The nature of surface
where Pf is the probability of failure, S is the fracture area loading, its subsequent stresses, and its dependence
stress from Equation 1, sy is the characteristic strength, on the Weibull modulus are accounted for in kA . The
and m is the Weibull modulus. There is no account of Weibull distributions for the three different surface ¯aw
how the specimen was mechanically loaded, what its size types shown in Fig. 3b to d are represented by Equation
was, or what its strength-limiting ¯aw was in the form of 5, but were analyzed separately. Lastly, the two-
Equation 3; consequently, extreme caution must be made parameter Weibull distribution representation for
when comparing or interpreting uncensored statistics if strengths limited by volume-¯aws is:
strength distributions were generated using different
m
loading scenarios, specimen sizes, or if more than one Pf ˆ 17 exp‰7kV V S=sOV † Š 6†
strength-limiting ¯aw type was operative.
where kV is a volume multiaxial and stress gradient
The uncensored Weibull modulus was conclusively
factor, V is the specimen's total volume, and sOV is a
lower and the uncensored characteristic strength was
scaling parameter for volume ¯aws. The nature of
subtly higher for the polished surface tested in tension
volume loading, its subsequent stresses, and its depend-
than the etched surface tested in tension. Listings of the
ence on the Weibull modulus are accounted for in kV .
uncensored statistical results are shown in Tables II and
None of the bend bars failed from volume ¯aws so the
III for the polished and etched surfaces tested in tension,
use of Equation 6 was not required in any of the analyses,
respectively. A representative example of these trends in
however, it was included in this discussion for the sake of
uncensored Weibull modulus and characteristic strength
completeness.
is illustrated in Fig. 4, which shows existing differences
The censored strength distributions were determined
between the strength distributions for polished and
using a Weibull distribution statistics computer program
etched 2 mm h1 1 0i conditions. These trends in the two
called CERAMIC which considered their concurrent
parameters were independent of the investigated
activity and accounted for how each specimen was
specimen widths and crystallographic orientations.
mechanically loaded, what its size was, and whether an
edge-, surface-, or volume-¯aw caused its failure. The
3.4. Censored statistics total probability of failure Pft † when concurrent
The concurrent activity of strength-limiting ¯aws individual ¯aw populations (for example, Pfa and Pfb
required strength data censoring in order to validly functions representing ¯aw populations ``a'' and ``b,''
compare the strength distributions among the 16 test respectively) are limiting strength is represented by [28],
conditions. The concurrence of the four identi®ed ¯aw 17Pft ˆ 17Pfa † 17Pfb † 7†
types is illustrated in the graphical examples in Figs 5a
and b. The non-dominant strength-limiting ¯aw in any or
given set did not necessarily account for the weakest Pft ˆ 17 17Pfa † 17Pfb † 8†
strengths. Edge, surface 2, and surface 3 ¯aws were
concurrent ¯aws when the polished surface was tested in A third term would exist in the right-hand-side of
tension, while surface 1 and edge ¯aws were concurrent Equations 7 and 8 if three concurrent ¯aw populations
¯aws when the etched surface was tested in tension. The were limiting strength (etc. for four or more concurrent
activity or dependence of a single ¯aw type (i.e., ¯aws). The probability of failure expressions in
297
T A B L E I I Summary of the uncensored and censored Weibull distributions for the test conditions involving the silicon's polished surface being
testing in tension.

Specimen Test Censored statistics Censored statistics Censored statistics


rate Uncensored statistics ``surface 2'' ¯aw type ``surface 3'' ¯aw type ``edge'' ¯aw type
(mm min) ÿ 1
Weibull Characteristic Weibull Scaling Weibull Scaling Weibull Scaling
modulus strength modulus parameter modulus parameter modulus parameter
m sy m soA m soA m soL
(MPa) MPa mm2=m † MPa mm2=m † MPa mm1=m †

2 mm 2.8 305 2.8 622


h1 1 0i 0.5 (2.2, 3.6) (266, 348) (2.2, 3.6) (530, 799)
n ˆ 32 n ˆ 32 n ˆ 32 n ˆ 32
3 mm 4.5 262 2.7 1515 4.6 404
h1 1 0i 0.5 (3.4, 5.9) (240, 285) (*,9 3) (415, *) (3.4, 6.0) (364, 478)
n ˆ 30 n ˆ 30 nˆ1 nˆ1 n ˆ 29 n ˆ 29
5 mm 2.9 302 5.2 871 2.9 612
h1 1 0i 0.5 (2.2, 3.7) (264, 343) (0.8, 14.0) (564, *) (2.2, 3.7) (522, 789)
n ˆ 31 n ˆ 31 nˆ1 nˆ1 n ˆ 30 n ˆ 30
5 mm 3.5 359 2.6 2699 3.6 635
h1 1 2i 0.5 (2.7, 4.5) (323, 398) (0.2, 8.4) (681, *) (2.7, 4.5) (559, 776)
n ˆ 33 n ˆ 33 nˆ1 nˆ1 n ˆ 32 n ˆ 32
2 mm 2.6 300 2.6 654
h1 1 0i 0.05 (2.0, 3.3) (257, 347) (2.0, 3.3) (549, 860)
n ˆ 30 n ˆ 30 n ˆ 30 n ˆ 30
3 mm 3.8 261 3.8 439
h110i 0.05 (2.7, 5.1) (232, 292) (2.7, 5.1) (383, 552)
n ˆ 24 n ˆ 24 n ˆ 24 n ˆ 24
5 mm 4.3 406 3.8 1141 4.3 654
h110i 0.05 (3.2, 5.6) (370, 423) (1.2, 8.1) (649, *) (3.1, 5.7) (483, 794)
n ˆ 31 n ˆ 31 nˆ3 nˆ3 n ˆ 28 n ˆ 28
5 mm 3.2 355 13 * 3.5 644
h112i 0.05 (2.4, 4.2) (315, 400) (0.2, 3.5) (2.6, 4.5) (564, 797)
n ˆ 31 n ˆ 31 nˆ2 nˆ2 n ˆ 29 n ˆ 29
2 mm 5.1 269 14.7 374 5.0 400
h110i 0.005 (3.8, 6.6) (249, 289) (2.0, *) (332, *) (3.7, 6.5) (363, 466)
n ˆ 31 n ˆ 31 nˆ1 nˆ1 n ˆ 30 n ˆ 30
3 mm 3.5 272 3.5 484
h110i 0.005 (2 5, 4 6) (239, 308) (2.5, 4.6) (418, 620)
n ˆ 24 n ˆ 24 n ˆ 24 n ˆ 24
5 mm 44 411 2.6 3130 2.0 4117 4.8 636
h110i 0.005 (3.3, 57) (376, 449) (*, 8.6) (723, *) (0.4, 5.4) (866, *) (3.6, 6.2) (577, 743)
n ˆ 30 n ˆ 30 nˆ1 nˆ1 nˆ2 nˆ2 n ˆ 27 n ˆ 27
5 mm 3.6 330 5.3 865 3.5 587
h112i 0.005 (2.6, 4.6) (295, 377) (0.6, 15.0) (523, *) (2.6, 4.6) 510, 738)
n ˆ 30 n ˆ 30 nˆ1 nˆ1 n ˆ 29 n ˆ 29
3.9 1216 2.2 3183 31 634
Pooled data Not applicable (1.6, 7.1) (721, *) (1.1, 3.6) (1263, *) (2.8, 3.3) (602, 674)
nˆ4 nˆ4 nˆ9 nˆ9 n ˆ 344 n ˆ 344

Note: Values in parenthesis constitute a 95% con®dence interval; n is the number of specimens in that distribution; and * represents an undetermined
result due to an insuf®cient number of data points and the inability of the statistical analysis software to obtain a convergent solution.

Equations 3 to 5 represent the probability of failure terms logical because the specimen widths varied from 2.0, 3.0,
on the right-hand-side of Equations 7 and 8, and were and 5.0 mm, however, the edge lengths and edge-length-
computed as such by the CERAMIC program using stress-gradients did not vary among these differing
maximum likelihood analysis. The censored results for widths because the same 3 mm/6 mm ®xture was used
the 16 test conditions are listed in Tables II and III. These for all tests. Consequently, strength was not a function of
quantitative results facilitated the strength dependence specimen size (width) in this case because specimen size
examination on the various independent parameters. (i.e., edge length where the edge ¯aw type was operative
and dominant) was not changing between test conditions.
If strength indeed were dependent on edge length, then
3.4.1. Strength as a function of specimen additional and different ®xture sizes other than the 3 mm/
size (width) 6 mm ®xture used in the present study would have been
3.4.1.1. Polished side in tension: h 1 1 0i and h1 1 2i required to exploit it.
orientations. The edge ¯aw was the primary strength- The observed censored strength distribution independ-
limiting ¯aw and its censored Weibull modulus and ence on specimen width is consistent with results from a
scaling parameter (Equation 4) were statistically equiva- recently conducted study involving micro-tensile testing
lent for all specimen widths (see Table II). This result is of polycrystalline silicon. Tsuchiya et al. [29] performed
298
T A B L E I I I Summary of the uncensored and censored Weibull distributions for the test conditions involving the silicon's etched surface being
testing in tension.

Specimen Test Censored statistics Censored statistics


rate Uncensored statistics ``surface 1'' ¯aw type ``edge'' ¯aw type

(mm min) ÿ 1 Weibull Characteristic Weibull Scaling Weibull Scaling


modulus strength modulus parameter modulus parameter
m sy m soA m soL
(MPa) MPa mm2=m † MPa mm1=m †

2 mm 5.2 292 4.9 340 7.0 514


h1 1 0i 0.5 (3.8, 6.7) (271, 303) (3.5, 6.5) (314, 388) (3.2, 12.2) (420, 972)
n ˆ 32 n ˆ 32 n ˆ 27 n ˆ 27 nˆ5 nˆ5
3 mm 7.2 282 7.1 304 14.0 413
h1 1 0i 0.5 (5.3, 9.5) (257, 287) (5.2, 9.4) (288, 331) 1.6, 43.2) (338, *)
n ˆ 30 n ˆ 30 n ˆ 29 n ˆ 29 nˆ1 nˆ1
5 mm 6.3 284 6.3 351
h1 1 0i 0.5 (408, 8.0) (267, 300) (4.8, 8.0) (329, 389)
n ˆ 33 n ˆ 33 n ˆ 33 n ˆ 33
5 mm 5.9 261 5.9 330
h1 1 2i 0.5 (4.4, 7.6) (244, 278) (4.4, 7.6) (306, 372)
n ˆ 30 n ˆ 30 n ˆ 30 n ˆ 30
5.8 336 8.1 491
Pooled data Not applicable (5.1, 6.7) (323, 353) (4.2, 13.1) (415, 783)
n ˆ 119 n ˆ 119 nˆ6 nˆ6

Note: Values in parenthesis constitute a 95% con®dence interval; n is the number of specimens in that distribution; and * represents an undetermined
result due to an insuf®cient number of data points and the inability of the statistical analysis software to obtain a convergent solution.

tensile testing on specimens having different gage these differing specimen widths (see Table III).
section widths and lengths, and observed that the According to Equation 5, the strength of bend bars
measured strength was a function of specimen length with a larger surface area (e.g., 5 mm wide specimens)
and not width. This result is consistent with the results of should be lower than for bend bars with a smaller surface
the present study described in the preceding paragraph. area (e.g., 2 mm wide specimens) for equal probabilities
More quantitative comparisons cannot be made between of failure. The anticipated ratio of strength differences
these two studies because Tsuchiya et al. did not are represented by8
represent their tensile strengths using Equation 4 (for
fracture limited by edge ¯aws) nor scaled them to a unit 1=m
S2 mm =S5 mm ˆ A5 mm =A2 mm †
length. This is unfortunate because it would have been
the appropriate distributions to use, and it also would ˆ 15 mm2 =6 mm2 †1=6:1 ˆ 1:16 9†
have been interesting to compare scaling parameters and
interpret differences or similarities between the study's where S5 mm and S2 mm are characteristic strengths of the
two silicon materials tested. Tsuchiya et al. instead used 5 and 2 mm wide specimens, and A5 mm and A2 mm are
Equation 5 and 6 to show that distributions representing areas subjected to tensile stress for the 5 and 2 mm wide
surface area and volume strength-limiting ¯aws did not specimens.9 This example involving these two extreme
represent their strengths. specimen sizes indicates that the strength of the 2 mm
3.4.1.2. Etched side in tension: h1 1 0i orientation. The wide specimens should be approximately 16% greater
surface 1 ¯aw was the primary strength-limiting ¯aw for than the 5 mm wide specimens when a surface-¯aw is the

(a) (b)

Figure 5 Examples showing the concurrent activity of different strength-limiting ¯aw populations. Concurrent populations when the (a) polished and
(b) etched surfaces were tested in tension.

299
strength-limiting ¯aw (similarly, the characteristic rates may be used for the design of silicon components
strength of the 2 mm wide specimen is anticipated to subjected to long-term tensile stress ®elds. Additionally,
be approximately 7% larger than that for the 3 mm wide the slow crack growth insusceptibility of the silicon
specimens according to Equation 9). Although there is a permits the application of proof testing to ®lter out the
slight indication that the characteristic strengths are weakest wafers without the concern that the actual act of
decreasing (see Table III) with increase in specimen size, proof testing would in itself weaken the survivors. Note
this indication cannot be statistically concluded within that this result was independent of specimen size and
95% con®dence. Therefore, the characteristic strengths only applied when the silicon's polished side was
for these three sets were deemed statistically equivalent. subjected to tensile stress.10 Lastly, the edge ¯aw type
The censored Weibull modulus and scaling parameter for was the primary strength-limiting ¯aw type for all these
the dominant surface 1 ¯aw was statistically equivalent test cases.
for all sets (see Table III). The identi®cation in the present study of silicon slow
The effect of size on silicon strength is rarely crack growth insusceptibility is consistent with results
presented in the literature. In one study conducted by from previous studies. Chen and Liepold [31] observed
Pearson et al. [30] a decrease in strength for increasing no subcritical crack growth in the {1 1 1} plane of silicon
silicon rod sizes up to 100 mm on a side tested in bending using the double torsion test method, and the same
was reported, and above that size the strength was authors in other studies [1±12] reported similar results,
independent of specimen size. However, the usefulness including no change in strength with stressing rate of
and interpretation of these results is limited because no f1 0 0g p-type silicon wafers tested in pin on three pin
fractographical examinations or strength-limiting ¯aw biaxial ¯exure. Slow crack growth insusceptibility has
discussions were presented. also been identi®ed in silicon at temperatures above
ambient [32].
Although its existence is infrequent, some evidence
3.4.2. Strength as a function of test loading exists in the literature that contradicts the above ®ndings
rate of slow crack growth insusceptibility in silicon. Bharduri
The scaling parameter of the Weibull distribution did not and Wang [33] identi®ed slow crack growth suscept-
change and was independent of the test loading rate ibility using the double torsion test technique, however,
within 95% con®dence. This independence of loading Chen and Liepold [31] were not able to replicate the
rate is evident by the equivalently valued censored ®nding using the same technique. Connally and Brown
scaling parameters listed in Table II. This indicates that [34] reported slow crack growth susceptibility using a
the silicon was not susceptible to slow crack growth (i.e., resonated cantilever beam silicon specimen, but their
fatigue, or time-dependent loss in strength) over the ®nding was based on only one specimen and the
examined loading rates [16]. This is a signi®cant possibility of a reverse cyclic fatigue effect [35] as a
observation because it indicates that the same silicon contribution to their result was not accounted for in their
strength data generated using relatively fast test loading analysis.

Figure 6 Different crystallographic orientations produced different fracture orientation. Schematics of the preferred fracture orientations for the (a)
h1 1 2i and (b) h1 1 0i specimens are indicated, along with examples of (c) h1 1 2i and (d) h1 1 0i fractured specimens.

300
3.4.3. Crystallographic orientation (1 1 1) and often branched as shown in Fig. 6d. This
The censored strength distributions were equivalent for difference in fracture orientation was independent of the
both examined crystallographic orientations independ- loading rate and specimen orientation.
ent of specimen orientation. The censored Weibull
parameters for the dominant edge ¯aw (i.e., polished
surface tested in tension) were statistically equivalent 3.4.4. Specimen orientation
for the h1 1 0i and h1 1 2i orientations independent of The censored distributions for the polished and etched
test rate. Additionally, the censored Weibull parameters surfaces were different because each had different
for the dominant surface 1 ¯aw (i.e., etched surface dominant strength-limiting ¯aws (edge versus surface 1
tested in tension) were also equivalent for both ¯aw), and this observation was independent of specimen
orientations. width and crystallographic orientation. This indicates
The two crystallographic orientations examined that different strength-limiting ¯aws and strength
produced differing fracture orientations. This was the distributions will be operative depending on the
result of the preferential fracture plane {1 1 1} having manner in which a silicon specimen (or component) is
differing orientations (see Figs 6a and b) with respect to stressed. Because of this difference in activity of
the long axis of the h1 1 2i or h1 1 0i bend bars. As dominant ¯aw type, a direct comparison of the censored
discussed earlier, the preferred cleavage plane of silicon scaling parameter cannot be made as a function of
is {1 1 1}, which has the lowest surface energy of any specimen orientation (analogous to trying to compare a
plane in the structure. Fracture in both orientations length to an area). However, the censored Weibull
followed the {1 1 1} set of planes, with preference modulus of each ¯aw type may be compared as they
towards the primary fracture surface 1 1 1† of bend bars represent how scattered the strengths were for each
having their length parallel to h1 1 2i, or perpendicular to distribution. The average censored Weibull modulus for
the tensile axis as shown in Fig. 6c. However, the fracture the four sets tested at 0.5 mm min ÿ 1 and with their
surfaces of bend bars having their length parallel to polished side loaded in tension was 3.5, while that for the
h1 1 0i were serrated in appearance ( planes 1 1 1† and four sets tested at the same rate but with their etched side

Figure 7 Example of ``cathedral-like'' fracture markings observed in many h1 1 0i specimens whose etched surface was tested in tension.

301
loaded in tension was 6.2. The larger-valued censored consequence of the silicon wafer's preparation (etch pits),
Weibull modulus for the surface 1 ¯aw indicates that it the cutting of the specimens (edge and surface chips), and
produced less scatter in strength than the edge ¯aw (or from test-®xture-induced damage. Intrinsic ¯aws did not
that the size of the etch-pits had a narrower size limit the strength because their size (if present) was much
distribution). smaller than any of the extrinsic ¯aw sizes.
Fractography revealed the presence of unique fracture The uncensored Weibull modulus was conclusively
markings associated only with the h1 1 0i specimens lower and the uncensored characteristic strength was
whose etched surface was tested in tension (Table III). A subtly higher for the polished surface tested in tension
typical fracture surface of such a specimen is shown in than the etched surface tested in tension. These trends
Fig. 7. Rice [36] described such a fracture surface as were independent of specimen widths and crystallo-
having a ``cathedral-like'' mirror followed by ``whisker- graphic orientations investigated.
lance mist hackle,'' which then branched onto a more The censored results from the polished surface being
preferred plane of crack propagation. No ``cathedral- tested in tension yielded several conclusions. Machining
like'' patterns were identi®ed on the h1 1 2i specimens or cutting damage in the form of chipped edges (edge-
whose etched surface was tested in tension. The fracture type-¯aw) was the dominant strength-limiting ¯aw. It
surface of such h1 1 2i specimens typically only was the dominant ¯aw for all test specimen widths,
contained a long parallel series of ``whisker-lance'' loading rates, and investigated crystallographic orienta-
lines (e.g., Fig. 3b). tions. The censored Weibull modulus and scaling
parameter were independent of crystallographic orienta-
tion. All bend specimens had the same edge length, so
3.4.5. Pooled censored statistics strength-dependence on specimen width was not
Pooling fracture strengths from multiple specimen types expected and the strength results con®rmed this. The
may be used to validate size-scaling, calculate parameter Weibull modulus and scaling parameter for the pooled
estimates with smaller con®dence intervals, combine censored machining chip edge ¯aw were 3.1 and
data that was generated with different specimen sizes and 634 MPa mm1/m, respectively (344 of 357 specimens).
geometries, and initial component test data may be The 95% con®dence intervals for these censored
combined with laboratory specimen fracture data to parameters were 2.8±3.3 and 602±674 MPa mm1/m.
determine self-consistency [37]. The intent of pooling Lastly, the silicon was not susceptible to slow crack
the censored data in the present study was to lessen the growth (i.e., fatigue or time-dependent loss in strength).
con®dence intervals of the censored Weibull parameters. The censored results from the etched surface being
The CERAMIC computer program was used to calculate tested in tension also yielded several conclusions. A ¯at-
the pooled censored statistics. bottomed etch pit (surface-type-¯aw) was the dominant
The edge ¯aw was the dominant strength-limiting ¯aw strength-limiting ¯aw. It was the dominant ¯aw type for
when the polished surface was loaded in tension for all all test specimen widths and investigated crystal-
test specimen widths, loading rates, and crystallographic lographic orientations. The censored Weibull modulus
orientations investigated. As a consequence of this, the and scaling parameter were independent of crystal-
strengths which were limited by the edge ¯aw were lographic orientation. The strength of the silicon was
pooled, and the Weibull modulus and scaling parameter independent of specimen width; however, the surface
were determined to be 3.1 and 634 MPa mm1/m, area differences among the 2, 3, and 5 mm wide
respectively (344 of 357 specimens). The 95% con- specimens may not be suf®cient to exploit any existence
®dence intervals for these censored parameters were 2.8± of size-dependent strength. The Weibull modulus and
3.3 and 602±674 MPa mm1/m. These pooled statistical scaling parameter for the pooled censored etch pit
values are recommended for use in the design and ¯aw were 5.8 and 336 MPa mm2/m, respectively (119 of
mechanical reliability analysis of silicon components in 125 specimens). The 95% con®dence intervals for
service. these censored parameters were 5.1±6.7 and 323±
The surface 1 ¯aw was the dominant strength-limiting 353 MPa mm2/m.
¯aw when the etched surface was loaded in tension for all
test specimen widths and crystallographic orientations
investigated. As a consequence of this, the strengths that Acknowledgments
were limited by the surface 1 ¯aw were pooled, and the The authors wish to thank G. R. Romanoski and J. H.
Weibull modulus and scaling parameter were deter- Schneibel for their review and their helpful comments
mined to be 5.8 and 336 MPa mm2/m, respectively (119 and suggestions. Additionally, gratitude is expressed for
of 125 specimens). The 95% con®dence intervals for the pro®lometry results generated by R. J. Parten.
these censored parameters were 5.1±6.7 and 323± Research sponsored by the US Department of Energy,
353 MPa mm2/m. Likewise, these pooled statistical Assistant Secretary for Energy Ef®ciency and Renewable
values are recommended for use in the design and Energy, Of®ce of Transportation Technologies, as part of
mechanical reliability analysis of silicon components in the Advanced Automotive Materials Program, under
service. contract DE-AC05-00OR72564 with UT-Battelle, LLC.

4. Conclusions Notes
Extrinsic ¯aws limited the strength of the f1 1 1g n-type * Currently with the U.S. Army Research Laboratory, Aberdeen
silicon examined. The presence of these ¯aws was a Proving Ground, MD.

302
** Currently with Saint-Gobain Abrasives, Worcester, MA. Society for Testing and Materials, West Conshohocken, PA,
1. Currently with the Department of Materials Science and 1998).
Engineering, Pennsylvania State University, University Park, PA. 17. ``Practice for Reporting Uniaxial Strength Data and Estimating
2. The data generated in this study are in reference to this sectioning Weibull Distribution Parameters for Advanced Ceramics,'' ASTM
procedure and the possible strength-limiting ¯aws it produces; their C1239 ``Annual Book of ASTM Standards, Vol. 15.01,''
extension for use with silicon machined by differing procedures is (American Society for Testing and Materials, West
cautioned because there is no guarantee that the same operative Conshohocken, PA, 1998).
strength-limiting ¯aws would exist. 18. ``Standard Practice for Fractography and Characterization of
3. Model 1605, Applied Test Systems, Butler, PA. Fracture Origins in Advanced Ceramics,'' ASTM C1322,
4. Only twenty-four specimens were tested in two of the test sets due ``Annual Book of ASTM Standards, Vol. 15.01,'' (American
to limited numbers of specimens. Society for Testing and Materials, West Conshohocken, PA,
5. The analysis and choice of the two ring diameters was analogous to 1998).
the choice of the 3 mm/6 mm span dimensions being used for the 19. ``Life Prediction Methodology for Ceramic Components of
uniaxial four-point-¯exure testing; namely, the required main- Advanced Heat Engines, Phase 1,'' Prepared By AlliedSignal
tenance of linear elasticity and avoidance of contact-crushing Engines, Phoenix, AZ, ORNL/sub/89-SC674/1±2 (DOE Of®ce of
during biaxial ¯exure testing. Transportation Technologies, 1995).
6. Form Talysurf 120, Rank Taylor Hobson Limited, Leicester, UK. 20. F. I . B A R AT TA , W. T. M AT T H E W S and G . D . Q U I N N , ``Errors
7. This qualitative analysis assumed a uniaxial stress state, which is Associated with Flexure Testing of Brittle Materials,'' ``U.S.
what largely exists with a ¯exure test. In service though, multiaxial Army Materials Technology Laboratory, Report Mtl Tr 87-35,''
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strictly used in its form. Probabilistic design and life prediction 21. T. L U B E , M . M A N N E R and R . D A N Z E R , Fatigue Fract. Eng
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8. This is achieved by dividing Equation 5 for a 2 mm wide specimen ``Annual Book of ASTM Standards, Vol. 10.04,'' (American
by Equation 5 for a 5 mm wide specimen. Society for Testing and Materials, West Conshohocken, PA,
9. For this illustration, m ˆ 6:1 was used, and was an average value of 1998).
the censored moduli for the 2 mm h1 1 0i, 3 mm h1 1 0i and 5 mm 23. ``Standard Test Method for Biaxial Flexure Strength (Modulus of
h1 1 0i test conditions. Rupture) of Ceramic Substrates,'' ASTM F394, ``Annual Book of
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``Annual Book of ASTM Standards, Vol. 15.01,'' (American and accepted 27 January 2000

303

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