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MME 467

Ceramics for Advanced Applications

Lecture 28
Design with Brittle Ceramics 1
Ref: Barsoum, Fundamentals of Ceramics, Ch11, McGraw Hill, 2000;
Richerson, Modern Ceramic Engineering, Ch15, Marcel Dekker, 1992
Topics to discuss....

1. Scatter in strength data


2. The statistical approach
3. The Weibull distribution
4. Determination of Weibull parameters
5. Factors affecting Weibull Modulus
6. Interpreting Weibull Modulus
Scatter in Strength Data

 Ceramics do not have uniquely defined failure strength.


 A given batch of ceramic specimens usually does not show a constant
measured strength – instead they show a range of strengths.

 The strength of ceramic is determined by a combination


of material parameters, the toughness and the crack size.
 Since fracture toughness is not a variable, the variation in strength
comes from a variation in the size of the biggest defect.

 Because of the variation in flaw size, the failure strength


of ceramics shows an unacceptable reliability with a
considerable degree of scatter in the test data.
 The scatter in strength data of ceramic materials
is significantly larger than that of metals
 due to the presence of flaws and a large scatter in the size, shape and
distribution of flaws
 variation in strength up to 25 % can be encountered – a high variability
which can lead to problems when it comes to relying on ceramics for certain
engineering applications

 The failure probability of a box of chalks, of which 3 out of


10 sticks break during writing, is Pf = 0.30
 for a chalk, Pf = 0.30 is acceptable (just barely !!)
 for cutting tool, Pf = 10–2 (1 out of 100) can be accepted
 for glass window in vacuum system, Pf = 10–6 is needed
 for protective ceramic tiles of space shuttle, Pf > 10–8 is simply unacceptable.
 Given this variability, is it still possible to design critical
load-bearing parts with ceramics?
 Theoretically, if the flaws in a part were fully characterised and the stress concentrations
at each crack tip could be calculated, then given KIC, the exact stress at which the
component would fail could be determined and the answer to the question would be
YES.
 Needless to say, such a procedure is quite impractical
considering the large number of flaws to be characterised, and the time and effort that
would entail

 As an alternate approach, the behaviour of large number of


data can be characterised using a statistical approach.
 In such design, a single failure stress (like UTS for metals) of a ceramic is not considered,
rather the probability of failure or survival of a part at a given stress is determined.
E.g.: there is a 70% chance that a chalk would survive at 15 MPa stress during writing.
 The design engineer must then assess an acceptable risk factor and, using the
distribution parameters, estimate the design stress.
The Statistical Approach
 The scatter in strength data, s, can be described by a statistical
distribution density function, f(s). This function can be obtained
from the histogram of the measured data.
The strength region in which the measured data were found is divided into k classes and the
number of strength values ni falling in the i-th interval is plotted as a function of the class
number.
k
n = å ni f(s)
ni i
ni = number of strength data in class i
k = total number of class
n = total number of data
(or tested specimen)
s
Class number, i Density distribution of strength
data, which is an analytical
Histogram of strength data description of the histogram
The distribution density has the following properties:

The integral extended over the whole


strength is f(s)

∫0 f(s) . ds =1
P (s1 ≤ s ≤ s2)
The integral between two strength values s1 F(s)
and s2 represents the probability of a
measured strength value being found
between the two limits:
s2
s1 s2 s
P (s2 ≤ s ≤.s1) = ∫s1
f(s) . ds

The probability of strength being less than a


value sC is the cumulative distribution of the  The scatter of the flaw size a can
function : also be described similarly by a
sC distribution density, f(a):
¥
P (sC) = ∫0 f(s) . ds
ò f (a) da = 1
0
Typical Strength Distribution Curve

f(s) Metals f(s) Ceramics

s s

Strength distribution curve Strength distribution curve


for metals for ceramics
 Narrower curve  Wider curve
 Symmetrical  Not symmetrical, skewed towards
 Peak point in the curve low-strength values with a long tail
corresponds the average strength  Peak point in the curve does not
correspond the average strength
Reliability in Test Data

design material design material


Frequency

strength strength strength strength

Frequency
margin
of safety

Strength Strength

Acceptable Marginal / Unacceptable


Reliability Reliability
(a) (b)

Strength distribution curves for (a) metals with acceptable reliability,


(b) ceramics with marginal/unacceptable reliability
The Weibull Distribution

 Currently, the most popular means of characterising


the flaw distribution is by the Weibull approach.

 Weibull distribution is a cumulative probability distribution


 it predicts the fraction of samples which survive/fail at stresses up to
the stress in question
 it does not give the probability of failure at that stress

 Based on a “weakest link” model, which is analogous


to the breaking of a length of chain.
 Failure occurs when the weakest link breaks.
 Suppose that, there is a probability Ps(L) that a chain of length
L does not possess a link with a breaking stress less than s.
Then the probability of a longer chain of length 2L surviving under the
stress s will be

Ps (2L) = Ps (L) . Ps (L)

 Assume the probability of some length L0 of a link failing


at a stress s is R(s).
 Then the probability of a length L failing at the given stress will be
L
Pf (L)  R(s )
L0

 The probability of surviving of L will be


DL
Ps (DL) = 1 – P f (DL) = 1 – R(s)
L0
 The probability of the chain of length (Lo+L) surviving is
 L 
Ps ( L0  L)  Ps ( L0 ) . Ps (L)  Ps ( L0 ) . 1 – R(s ) 
 L0 
Ps ( L0  L) – Ps ( L0 ) L
 – R(s )
Ps ( L0 ) L0

 Considering the 3D model, instead of 1D, replacing linear


terms with volumes

Ps (V0  V ) – Ps (V0 ) V
 – R(s )
Ps (V0 ) V0

 For an infinitesimal volume change, replacing V with dV:

dPs (V ) dV
= – R(s)
Ps (V ) V0
dPs (V ) dV
= – R(s)
Ps (V ) V0

 Integrating and rearranging


é Vù
Ps (V ) = exp ê– R(s) ú + C
ë V0 û

 Since for V = 0, PS(V) = 1, we get C = 0. Then


é Vù
Ps (V ) = exp ê– R(s) ú
ë V0 û

 If stress varies from point to point in the component


é dV ù
Ps (V ) = exp ê– ò R(s) ú
ë V V0 û
 Weibull proposed a simple, three-parameter model for R(s):

æ s – s c öm
R(s) = ç ÷
è sv ø

sc = the critical stress below which fracture is assumed to have zero


probability, implying an upper limit to the flaw size (in many cases,
sc can conveniently be taken as zero).

sv = a normalising stress (at which probability of failure is 0.632) of no


physical significance.

m = a shape factor, usually referred to as the Weibull modulus, which


reflects the degree of variability in strength – the higher the m is, the
less variable is the strength. Values for m of 5 – 20 are common for
ceramics.
é æ s – s c öm dV ù
Ps (V ) = exp ê– ò ç ÷ ú
êë V è s v ø V0 úû

 If the material is under constant stress

é æ s – s c öm V ù
Ps (V ) = exp ê– ç ÷ ú
êë è s v ø V0 úû

 For a two-parameter model of Weibull distribution for


ceramic materials, the presence of a critical stress below
which no fracture occurs is usually ignored. Thus, sc = 0, and
the probability of failure, writing simply Pf instead of Pf(V):

é æ s öm V ù
Pf = 1 – Ps = 1 – exp ê– ç ÷ ú
êë è s v ø V0 úû
é æ s öm V ù
P f = 1 – exp ê – ç ÷ ú
êë è s v ø V0 úû

é æ s öm ù æV0 ö1/m
Pf = 1 – exp ê – ç ÷ ú ; s0 = sv ç ÷
êë è s 0 ø úû èV ø

 The strength distribution of a ceramic component is


described by
1. the material parameter m, and
2. the parameter s0, which depends on the material and also on the size
of the component and stress distribution in the component.
é æ s öm ù
Pf = 1 – exp ê – ç ÷ ú
êë è s 0 ø úû

 In this Weibull function, the Weibill modulus, m, defines the


shape of the failure distribution curve.
 m 0, the failure probability Pf becomes independent of applied stress.
 m = 1, Pf becomes a simple asymptotic exponential distribution.
 m = , the distribution is a step function with Pf = 0 when s<s0, and
Pf = 1 when s<s0.

Pf Pf

1 1

m=
m=1

0 s 0 s
s0
 The Weibull modulus, m, also defines the width of the
probability distribution.
 Large m  narrow distribution, small scatter in strength data, high reliability material
 Small m  wide distribution, large scatter in strength data, poor reliability material

Pf Pf

1 1

large m small m

0 s 0 s

 Weibull plot is a good representation of material behaviour even


at low stress and the designer can predict failure behaviour
without any knowledge of flaw distribution.

 Poor ceramics have m in the range of 3 – 10, while good engineering


ceramics have m in the range 10 – 40 (For metals, m > 100).
Determination of Weibull Parameters

é æ s öm ù
Pf = 1 – exp ê – ç ÷ ú
êë è s 0 ø úû

m
æsö ln (– ln (1–Pf))
ln (1 – P f ) = – ç ÷
è s0 ø

ln [ – ln (1 – P f )] slope = m
= m ln s – m lns 0
c = – m ln s0
ln [ – ln Ps ] = m lns – m lns 0 ln s
Problem
A series of square section bars are tested in 3-point bend test. Determine
(1) the Weibull modulus, m
(2) the median strength, sm (for which Pf = 0.5), and
(3) the normalised stress (s0) of the ceramic.
The failure strengths (MOR) data: 178, 318, 345, 210, 296, 235, 248, 276, 262.

Solution:
1. Rank all stress data (n) in ascending order and numbered.
2. Calculate the failure probability Pf of each data as:
Pf = (1– Ps) = n / (N+1)
where n is the rank of individual data and N = total no. of data.
3. Arrange data and plot ln (– ln (1–Pf)) vs. ln s.
4. Obtain m and s0 from the plot.
s (MPa) ln s Rank, n Pf ln (- ln(1-Pf))
178 5.18 1 0.1 -2.25
210 5.35 2 0.2 -1.50
235 5.46 3 0.3 -1.03
248 5.51 4 0.4 -0.67
262 5.57 5 0.5 -0.37
276 5.62 6 0.6 -0.09
296 5.69 7 0.7 +0.19
318 5.76 8 0.8 +0.48
345 5.84 9 0.9 +0.83

1. From the plot: Weibull modulus, m = 4.76


2. From data: Median strength, sm = 262 MPa (stress for which Pf = 0.5)
3. From the plot: - m ln s0 = - 26.9; s0 = 284.6 MPa
Factors Affecting Weibull Modulus

 From design point of view, it is important to have a high m


value. But a high m value does not result a high strength.

 Solids having large but uniform defects have


 low strength (due to large flaw size)
 high reliability, m (due to uniform defects, which yields smaller scatter)

 Uniformity in microstructure (flaws, grain size, inclusions)


produces high modulus.
Does increasing KIC of truly brittle material increases m?

 If survival probabilities at stress s1 and s2 be Ps1 and Ps2, then

ln Ps1 = – (s1/s0)m ln (ln Ps1 / ln Ps2) = m ln (s1/s2)

ln Ps2 = – (s2/s0)m ln (ln Ps1 / ln Ps2)


m =
ln (s1/s2)

Numerator  a constant, depends only on the total no. of sample tested.


Denominator  depends on the ratio (s1/s2), which is proportional to the ratio of flaw
size (c1/c2), which is independent of KIC (for samples showing no R-curve behaviour)

 Thus toughening (or, increasing KIC) of ceramics would not increase


Weibull modulus.
 But for those ceramics exhibiting R-curve behaviour, the increase in
KIC would result an increase in m value.
Effect of specimen volume/size

é æ s öm V ù
P f = 1 – exp ê – ç ÷ ú
êë è s v ø V0 úû

 On average, a large sample will fail at a lower stress than


a small one, since it is more likely that the big sample will
contain bigger flaws

 Thus, ceramic strength is volume dependent.

 For the same reason, ceramic in bending shows higher strength


than in simple tension (MOR > sTS)
 because in tension, the entire sample carries the stress, while in bending
only the surface layer carries the peak stress
 Compare two sets of data from the same material but
having different stressed volumes, V1 and V2.

 Since the mean values of each data set have the same
survival probability

é æ s öm V ù é æ s öm V ù
Ps, mean = exp ê – ç 1 ÷ 1 ú = exp ê– ç 2 ÷ 2 ú
êë è s v ø V0 úû êë è s v ø V0 úû

s2 æ V1 ö1/m
= ç ÷
s1 è V2 ø

 With increasing volume,


strength is decreased for a constant m.
Effective volume (Ve) under load (or, the LOAD FACTOR, Lf)

1. Tensile testing: Ve = V
2. 3-point bend test: Ve = Lf3-pt . V L2

3. 4-point bend test: Ve = Lf4-pt . V


L1
1
3-point bend: Lf =
2 (m+1)2
Example: m = 10
(L1 + mL2) Ve = 0.004 V (3-pt bend)
4-point bend: Lf = Ve = 0.025 V (4-pt bend)
2L1 (m+1)2

 The ratio of two strength values


measured using two different For example, TS vs. 3-pt Bend:
methods: s3-pt
sTS =
1/m [ 2 (m+1)2 ]1/m
s1 Lf2
s2 = Lf1
Effect of number of test specimens

 A substantial number of test samples are required


to determine an accurate and reliable value for m.

 Larger the value of number of sample, N (where V = NV0),


higher is the accuracy of m value.

+40
90% confidence
Error in m
(% of expected ±40%
value) 0
±10%

20 samples  ±40% error in m value


Over 60  ±90% confidence in m value
-60
0 20 40 60 80 100
Number of Specimen
Interpreting Weibull Modulus
Predicting failure stress

 If m is known, we can use failure data at one stress to predict


the probability of failure at some other stress.

ln Ps1 = – (s1/s0)m ln (Ps1 / Ps2) = (s1 / s2)m

ln Ps2 = – (s2/s0 )m (s1 / s2)m


Ps2 = Ps1 e

 Thus, if the Weibull modulus m and survival probability Ps1


at a given stress s1 are known, then the survival probability
Ps2 for any other stress s2 can be predicted.

Condition: Specimen volume/size must be the same.


Interpreting Weibull plots before and after service

 A reduction in m
indicates the introduction
of flaws, or extension of
flaws during service.

 Frequency distribution
curve would show a long
tail of flaws.
Data not fitting
a Weibull plot

Data would fit better if two


separate curves were
drawn. This is referred to as
“Bimodal Distribution.”

Further examination of the


fractured surface revealed that a
separate type of flaw population Materials having two
controlled the two regions different types of flaw
results bimodal
distribution

 These flaws were eliminated in subsequent materials to


achieve a monomodal Weibull distribution with an
increased modulus and strength.
Some other examples of using Weibull plot

Weibull plot for comparing processes


SC – slip casting, IP – isostatic pressing,
Weibull plot for comparing materials IM – injection moulding
Proof Testing

Finished components are


subjected to a stress above their
design stress.

Weaker samples having largest


flaws fail and, thereby eliminated.

Survived samples can be used


below design stress with high level
of confidence.

Danger:
 Sub-critical cracks growth may occur during proof testing.
 So effective proof testing demands inert, moisture-free test environment
with a rapid loading/unloading cycle (to minimise the time at maximum
stress).