MME 467

Ceramics for Advanced Applications

Lecture 25
Time, Temperature and
Environmental Effects on Ceramics 1
Ref: Richerson, Modern Ceramic Engineering, Ch8, Marcel Dekker, 1992
Topics to discuss....

1. Creep of ceramics
2. Static fatigue of ceramics
 Introduction
 Ceramics are often used in severe environments (high
temperatures, chemical attack (oxidation, corrosion), erosion,
impact, and thermal shock that metal cannot tolerate.
 new flaws are generated, which are larger than those initially present,
and cause premature failure of material.

 If a constant load is applied slowly in such corrosive

environment, initial flaws can grow into larger size and result in
fracture at a much lower stress. This is known as Static Fatigue,
Slow Crack Growth (SCG), or Stress rupture.

KI
 Ceramics exhibiting R-curve
behaviour are also susceptible to KI0
cyclic loading, the phenomenon
commonly known as Fatigue.
Da
Crack resistance curve (R-curve)
 Slow deformation of ceramics can also occur when
subjected to a constant stress at high temperature (T > 0.5 Tm).

 with time, a part experiencing such stress either fails or

undergoes shape or dimensional changes

 this phenomenon, similar to that occurs in metals, is known as Creep

 Although the atomic processes and micromechanisms of

these three phenomena are quite different, there is a
communality among them.

 in each case, a nucleated or pre-existing flaw grows with time,

leading to a disastrous failure

Thus, ceramic material has a lifetime

that one has to contend with.
 Creep of Ceramics

 Deformation occurs at constant stress as a function

of time and temperature.

 The deformation is plastic, rather than elastic.

 not recovered after releasing the stress

 Creep in ceramics is very complex.

 Several mechanisms can lead to creep deformation

 different mechanisms are operative over different

temperature and stress regimes
 Typical Creep Curve
At constant T or s

Failure
material deforms
e
Creep
Strain, plastically at a faster very high rate of
pace with time deformation causing
eventual failure
Primary
Creep Tertiary
Creep
D e
D t
Secondary Creep rate of deformation
with time is constant
material deform Elastic Deformation during this period
elastically when
load is applied
Time, t
Creep curve for hot-pressed silicon nitride
 The secondary creep region is the most useful in predicting
the life of ceramic component.

 This part of creep curve is characterised by its constant rate

of deformation, often referred to as steady-state creep and
represented by the equation

n, A = constants for specific materials

de
e= = As ne-Q/RT n = stress exponent
s = applied stress
dt Q = activation energy for creep

 The value of n and Q provide information about the

mechanism of creep, i.e. whether it is controlled by
1. viscoelastic effect
2. diffusional
3. dislocation motion (controlled by porosity and others)
 Factors determining the creep life of ceramic component :
1. mechanism of creep (controls the kinetics of flaw growth)
2. initial flaw distribution (determined by statistical evaluation)
3. fracture mechanics theory
4. stress rupture test

 Factors affecting creep rate of ceramics:

1. temperature of environment and applied stress
2. crystal structure (for single crystal ceramics)
3. microstructure (for polycrystalline ceramics)
4. viscosity (for non-crystalline/amorphous ceramics)
5. composition and stoichiometry
6. environment
Effect of temperature and stress on creep

de
e= = As ne-Q/RT
dt

As temperature and applied

stress is increased
 the rate of creep increased, and

 the duration of steady-state creep

is decreased
hot-isostatically pressed silicon nitride

4% glass reinforced alumina composite

Influence of stress on creep

Comparing creep data
better explained when plotted
as steady state creep rate vs.
either 1/T or log (stress)

e

1/T

e
steady-state creep rate as a function
of temperature for three SSN

log (Stress)
 Effect of single crystal structure on creep

 Creep in single crystal is controlled by the motion of dislocation

 dependent on the slip system of crystal

Highly symmetrical cubic structure (NaCl, MgO)

• 5 independent slip systems; Slip can occur at low temperature
Complex cubic structures (Diamond, rutile, spinel, etc.)
• 5 slip systems operate at high temperature and high applied stress
Hexagonal structure (Graphite, alumina, etc.)
• Only 2 slip systems

 For a measurable creep to occur

 dislocation must be present or created, and then start moving
 increasing T or s reduces the energy required for forming and moving dislocation

 Defects in lattice structure decreases creep by pinning dislocation

 Dislocations oriented across the direction of slip and larger precipitates have the largest
effect on blocking slip motion.
 Solid solutions and point defects have less effect
 Effect of microstructure
 Creep rate in polycrystalline ceramics is controlled by
mechanisms other than those control creep in single crystals.

 dislocation motion is not significant

(because of randomly oriented grain structure and
difficulty for dislocation to move from one grain into another)

 creep is controlled by
diffusion mechanisms or, grain boundary sliding

involves motion of ions, atoms, involves porosity or

or vacancies through crystal compositional difference
structure (bulk diffusion), or to form glassy phase at
along the grain boundary (grain the grain boundary
boundary diffusion)

 Creep mechanism of polycrystalline ceramics varies with

temperature, stress, and grain size.
 Creep rate substantially increased by increased porosity,
due to a decreased cross-sectional area available to resist
creep.

 MgO material with a 12 %

porosity showed 6 times
more creep rate than
another sample with only
2 % porosity

Effect of porosity on creep rate

of Al2O3 polycrystals
 Effect of viscosity

 Creep rate in non-crystalline/amorphous ceramics

is controlled by viscous flow.
 depends on viscosity at the given temperature

 for example, soda-lime-glass (having a low viscosity) creeps

at low temperatures

 Polycrystalline ceramics having a glassy-phase at

the grain boundary also creep by viscous flow.

 Viscosity, and viscous flow creep, strongly dependent

on composition.
 principally due to breaking down of glass-forming network
(e.g., Si-O bond)
 Effect of composition, stoichiometry,
and environment

Composition
 governs bonding and structure, Stoichiometry
and determines baseline creep (all lattice position filled as per formula)
tendencies.
 also controls baseline creep
tendencies.
Environment
 non-stoichiometric compound
 Modifies surface flaw shows diffusional charactersitics.
characteristics (including
crack blunting) TiC – stoichiometeic compound
TiC0.75 – non-stoichiometric compound
NaCl in air – brittle behaviour (TiC with vacancies)
NaCl in water – ductile behaviour (due to
removal of surface defects by dissolving)
– plastic deformation by creep
 Typical Creep Data

NC-132
 Si3N4 hot pressed with MgO
 complex glassy phase along
grain boundary
 grain boundary sliding
 low creep resistance

NCX-34
 Si3N4 hot pressed with Y2O3
 grain boundary phase is
refractory in nature
 improved creep resistance
NC-350
 reaction bonded Si3N4
 no additive used
 no grain boundary phase formed
 greatly improved creep resistance

NC-435
 reaction sintering of SiC and Si
 direct bonding, no glassy phase
formed along grain boundary
 good creep resistance
Sintered a-SiC
 Pressure-less sintering at very
high temperature (>1900 C)
 low additives, no grain boundary
phase
 very good creep resistance

Sintered Si3N4
with BeSiN2 and SiO2
 additives produce a very thin
(~ 10 A) refractory phase along
grain boundary
 very good creep resistance
 Static Fatigue

 Also known as subcritical crack growth (SCG) and stress

rupture, static fatigue refers to the slow growth of a
subcritical flaw as a result of its exposure to the combined
effect of stress and corrosive environment.

 The combination of a reactive atmosphere and a stress

concentration can greatly enhance the rate of crack
propagation.

Example:
 SiO2 dissolves in water at a rate of 10-7 m/s
 the application of stress can cause cracks to grow at speeds greater
than 10-3 m/s
 As the crack tip advances, the material is effectively weakened and
eventually can give away suddenly and catastrophically, after years
of service, according to the Griffith relationship: sf = A(Eg/c)1/2.
Mechanism of static fatigue

 presence of corrosive environments produces localised

corrosion at the crack tip or where stress is concentrated
at a flaw and accelerates static fatigue.

 presence of water and other chemicals accelerated the

process

 This mechanism, commonly known as stress corrosion in metal,

is dominant in glass components and in other polycrystalline
ceramics having a glassy phase in their structures.

 Other factors, those affecting creep, also influence static fatigue:

1. temperature and stress
2. grain size, and
3. presence glassy/secondary phase along the grain boundary.
Experimental determination of static fatigue

 A static load is applied to a specimen at constant temperature

and the time of fracture is recorded.

 Experiment set up is similar to those used to measure creep.

 The results are then plotted in a format identical to the one

shown below for cyclic fatigue, and are referred to as static
fatigue curve or stress/life (S/N) curve.

log s

Schematic of static fatigue curve

Time to failure or stress/life curve
Predicting life of ceramics

 Stress rupture test can be used

 To predict completely the static fatigue life of ceramic materials, and
 To determine life-limiting characteristics that might be improved with
further material development.

 Stress rupture data for ceramics are not easy to interpret

because of the large scatter.
 To characterise completely the static fatigue life of a ceramic requires
many repetitive tests at different stresses and temperatures at
different environments.

 When selecting candidate material for an application,

it is often desirable to obtain a quick determination of
the susceptibility of material to static fatigue.
 This can be done by variable-stressing rate experiments.
 Variable-stressing rate experiment

 Samples are loaded at three or four rates to fracture at

the selected temperature and environment

 The data are plotted as strength versus load rate curves,

as shown in figure.

No slow crack  If strength changes as a

Fracture growth function of load rate, the
stress ceramic is susceptible to slow
Moderate slow crack growth and can probably
crack growth be removed from consideration.
Severe slow  If little or no change in strength
crack growth is detected as a function of load
rate, the material is suitable for
Load Rate (Cross-head Speed) further evaluation by longer-
term static fatigue tests.
Schematic of variable-stressing rate experiment data for
estimating the susceptibility of a ceramic to slow crack growth