Standard Test Method for Determination of Slow Crack Growth Parameters of Advanced Ceramics by Constant Stress-Rate Flexural Testing at Elevated Temperatures

SIGNIFICANCE AND USE
4.1 For many structural ceramic components in service, their use is often limited by lifetimes that are controlled by a process of slow crack growth. This test method provides the empirical parameters for appraising the relative slow crack growth susceptibility of ceramic materials under specified environments at elevated temperatures. This test method is similar to Test Method C1368 with the exception that provisions for testing at elevated temperatures are given. Furthermore, this test method may establish the influences of processing variables and composition on slow crack growth as well as on strength behavior of newly developed or existing materials, thus allowing tailoring and optimizing material processing for further modification. In summary, this test method may be used for material development, quality control, characterization, and limited design data generation purposes.
Note 3: Data generated by this test method do not necessarily correspond to crack velocities that may be encountered in service conditions. The use of data generated by this test method for design purposes may entail considerable extrapolation and loss of accuracy.  
4.2 In this test method, the flexural stress computation is based on simple beam theory, with the assumptions that the material is isotropic and homogeneous, the moduli of elasticity in tension and compression are identical, and the material is linearly elastic. The average grain size should be no greater than one fiftieth (1/50) of the beam thickness.  
4.3 In this test method, the test specimen sizes and test fixtures were chosen in accordance with Test Method C1211, which provides a balance between practical configurations and resulting errors, as discussed in Refs (5, 6). Only the four-point test configuration is used in this test method.  
4.4 In this test method, the slow crack growth parameters (n and D) are determined based on the mathematical relationship between flexural strength and applied stress rate, log σ...
SCOPE
1.1 This test method covers the determination of slow crack growth (SCG) parameters of advanced ceramics by using constant stress-rate flexural testing in which flexural strength is determined as a function of applied stress rate in a given environment at elevated temperatures. The strength degradation exhibited with decreasing applied stress rate in a specified environment is the basis of this test method which enables the evaluation of slow crack growth parameters of a material.
Note 1: This test method is frequently referred to as “dynamic fatigue” testing (1-3)2 in which the term “fatigue” is used interchangeably with the term “slow crack growth.” To avoid possible confusion with the “fatigue” phenomenon of a material which occurs exclusively under cyclic loading, as defined in Terminology E1823, this test method uses the term “constant stress-rate testing” rather than “dynamic fatigue” testing.
Note 2: In glass and ceramics technology, static tests of considerable duration are called “static fatigue” tests, a type of test designated as stress-rupture (Terminology E1823).  
1.2 This test method is intended primarily to be used for negligible creep of test specimens, with specific limits on creep imposed in this test method.  
1.3 This test method applies primarily to advanced ceramics that are macroscopically homogeneous and isotropic. This test method may also be applied to certain whisker- or particle-reinforced ceramics that exhibit macroscopically homogeneous behavior.  
1.4 This test method is intended for use with various test environments such as air, vacuum, inert, and any other gaseous environments.  
1.5 Values expressed in this standard test are in accordance with the International System of Units (SI) and IEEE/ASTM SI 10.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish a...

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ASTM C1465-08(2019) - Standard Test Method for Determination of Slow Crack Growth Parameters of Advanced Ceramics by Constant Stress-Rate Flexural Testing at Elevated Temperatures
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1465 − 08 (Reapproved 2019)
Standard Test Method for
Determination of Slow Crack Growth Parameters of
Advanced Ceramics by Constant Stress-Rate Flexural
Testing at Elevated Temperatures
This standard is issued under the fixed designation C1465; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 Thistestmethodcoversthedeterminationofslowcrack
responsibility of the user of this standard to establish appro-
growth (SCG) parameters of advanced ceramics by using
priate safety, health, and environmental practices and deter-
constantstress-rateflexuraltestinginwhichflexuralstrengthis
mine the applicability of regulatory limitations prior to use.
determined as a function of applied stress rate in a given
1.7 This international standard was developed in accor-
environment at elevated temperatures. The strength degrada-
dance with internationally recognized principles on standard-
tion exhibited with decreasing applied stress rate in a specified
ization established in the Decision on Principles for the
environment is the basis of this test method which enables the
Development of International Standards, Guides and Recom-
evaluation of slow crack growth parameters of a material.
mendations issued by the World Trade Organization Technical
NOTE 1—This test method is frequently referred to as “dynamic
Barriers to Trade (TBT) Committee.
fatigue”testing (1-3) inwhichtheterm“fatigue”isusedinterchangeably
with the term “slow crack growth.” To avoid possible confusion with the
2. Referenced Documents
“fatigue”phenomenonofamaterialwhichoccursexclusivelyundercyclic
loading, as defined in Terminology E1823, this test method uses the term
2.1 ASTM Standards:
“constant stress-rate testing” rather than “dynamic fatigue” testing.
C1145Terminology of Advanced Ceramics
NOTE 2—In glass and ceramics technology, static tests of considerable
C1211Test Method for Flexural Strength of Advanced
duration are called “static fatigue” tests, a type of test designated as
Ceramics at Elevated Temperatures
stress-rupture (Terminology E1823).
C1239Practice for Reporting Uniaxial Strength Data and
1.2 This test method is intended primarily to be used for
Estimating Weibull Distribution Parameters forAdvanced
negligiblecreepoftestspecimens,withspecificlimitsoncreep
Ceramics
imposed in this test method.
C1322Practice for Fractography and Characterization of
1.3 Thistestmethodappliesprimarilytoadvancedceramics
Fracture Origins in Advanced Ceramics
that are macroscopically homogeneous and isotropic. This test
C1368 Test Method for Determination of Slow Crack
method may also be applied to certain whisker- or particle-
Growth Parameters of Advanced Ceramics by Constant
reinforcedceramicsthatexhibitmacroscopicallyhomogeneous
Stress Rate Strength Testing at Ambient Temperature
behavior.
D1239Test Method for Resistance of Plastic Films to
Extraction by Chemicals
1.4 This test method is intended for use with various test
E4Practices for Force Verification of Testing Machines
environmentssuchasair,vacuum,inert,andanyothergaseous
E6Terminology Relating to Methods of Mechanical Testing
environments.
E220Test Method for Calibration of Thermocouples By
1.5 Values expressed in this standard test are in accordance
Comparison Techniques
with the International System of Units (SI) and IEEE/
E230Specification for Temperature-Electromotive Force
ASTMSI10.
(emf) Tables for Standardized Thermocouples
E337Test Method for Measuring Humidity with a Psy-
chrometer (the Measurement of Wet- and Dry-Bulb Tem-
This test method is under the jurisdiction of ASTM Committee C28 on
peratures)
Advanced Ceramics and is the direct responsibility of Subcommittee C28.01 on
Mechanical Properties and Performance.
CurrenteditionapprovedJuly1,2019.PublishedJuly2019.Originallyapproved
ɛ1
in 2000. Last previous edition approved in 2014 as C1465–08 (2013) . DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/C1465-08R19. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1465 − 08 (2019)
E616Terminology Relating to Fracture Testing (Discontin- 3.1.11 slow crack growth (SCG),n—subcritical crack
ued 1996) (Withdrawn 1996) growth (extension) which may result from, but is not restricted
E1150Definitions of Terms Relating to Fatigue (Withdrawn to, such mechanisms as environmentally assisted stress corro-
1996) sion or diffusive crack growth.
−3/2
E1823TerminologyRelatingtoFatigueandFractureTesting
3.1.12 stress intensity factor, K [FL ],n—the magnitude
I
IEEE/ASTMSI10American National Standard for Metric
of the ideal-crack-tip stress field (stress-field singularly) sub-
Practice
jectedtoModeIloadinginahomogeneous,linearelasticbody.
(E616)
3. Terminology
3.1.13 R-curve, n—a plot of crack-extension resistance as a
3.1 Definitions:
function of stable crack extension. (E616)
3.1.1 The terms described inTerminologies C1145, E6, and
3.2 Definitions of Terms Specific to This Standard:
E1823 are applicable to this test method. Specific terms
relevant to this test method are as follows: 3.2.1 slow crack growth parameters, n and D, n—the
parameters estimated as constants in the flexural strength (in
3.1.2 advanced ceramic, n—a highly engineered, high-
megapascals)-stressrate(inmegapascalspersecond)equation,
performance, predominately nonmetallic, inorganic, ceramic
material having specific functional attributes. (C1145) which represent a measure of susceptibility to slow crack
−2 −1 growthofamaterial(seeAppendixX1).Fortheunitsof D,see
3.1.3 constant stress rate, σ˙[FL t ],n—a constant rate of
9.3.1.
increase of maximum flexural stress applied to a specified
beam by using either a constant load or constant displacement
4. Significance and Use
rate of a testing machine.
4.1 For many structural ceramic components in service,
3.1.4 environment, n—the aggregate of chemical species
their use is often limited by lifetimes that are controlled by a
and energy that surrounds a test specimen. (E1150)
process of slow crack growth. This test method provides the
3.1.5 environmental chamber, n—a container surrounding
empirical parameters for appraising the relative slow crack
the test specimen and capable of providing controlled local
growth susceptibility of ceramic materials under specified
environmental condition.
environments at elevated temperatures. This test method is
−2
3.1.6 flexural strength, σ [FL ],n—a measure of the similar to Test Method C1368 with the exception that provi-
f
ultimate strength of a specified beam specimen in bending sions for testing at elevated temperatures are given.
determined at a given stress rate in a particular environment. Furthermore, this test method may establish the influences of
processing variables and composition on slow crack growth as
3.1.7 flexural strength-stress rate curve—a curve fitted to
well as on strength behavior of newly developed or existing
the values of flexural strength at each of several stress rates,
materials, thus allowing tailoring and optimizing material
based on the relationship between flexural strength and stress
processing for further modification. In summary, this test
rate:
methodmaybeusedformaterialdevelopment,qualitycontrol,
log σ = [1/(n + 1)] log σ˙ + log D (see Appendix X1)
f
characterization, and limited design data generation purposes.
3.1.7.1 Discussion—In the ceramics literature, this is often
called a “dynamic fatigue” curve.
NOTE 3—Data generated by this test method do not necessarily
correspond to crack velocities that may be encountered in service
3.1.8 flexural strength-stress rate diagram—a plot of flex-
conditions. The use of data generated by this test method for design
ural strength as a function of stress rate. Flexural strength and
purposes may entail considerable extrapolation and loss of accuracy.
stress rate are both plotted on logarithmic scales.
4.2 In this test method, the flexural stress computation is
−3/2
3.1.9 fracture toughness, K [FL ],n—agenerictermfor
IC
based on simple beam theory, with the assumptions that the
measures of resistance to extension of a crack. (E616)
materialisisotropicandhomogeneous,themoduliofelasticity
−2
3.1.10 inert flexural strength [FL ],n—a measure of the
in tension and compression are identical, and the material is
strength of a specified beam specimen in bending as deter-
linearly elastic. The average grain size should be no greater
minedinanappropriateinertconditionwherebynoslowcrack
than one fiftieth (1/50) of the beam thickness.
growth occurs.
4.3 In this test method, the test specimen sizes and test
3.1.10.1 Discussion—An inert condition at near room tem-
fixtures were chosen in accordance with Test Method C1211,
perature may be obtained by using vacuum, low temperatures,
which provides a balance between practical configurations and
very fast test rates, or any inert media. However, at elevated
resultingerrors,asdiscussedinRefs (5, 6).Onlythefour-point
temperatures, the definition or concept of an inert condition is
test configuration is used in this test method.
unclear since temperature itself acts as a degrading environ-
4.4 Inthistestmethod,theslowcrackgrowthparameters(n
ment. It has been shown that for some ceramics, one approach
and D) are determined based on the mathematical relationship
to obtain an inert condition (thus, inert strength) at elevated
between flexural strength and applied stress rate, log σ = [1/(n
temperatures is to use very fast (ultra-fast) test rates ≥3×10 f
+ 1)] log σ˙ + log D, together with the measured experimental
MPa/s, where the time for slow crack growth would be
data.Thebasicunderlyingassumptiononthederivationofthis
minimized or eliminated (4).
relationship is that slow crack growth is governed by an
n
empirical power-law crack velocity, v= A[K /K ] (see
The last approved version of this historical standard is referenced on I IC
www.astm.org. Appendix X1).
C1465 − 08 (2019)
NOTE 4—There are various other forms of crack velocity laws which
inaccurate strength data and SCG parameters, especially for
are usually more complex or less convenient mathematically, or both, but
materials that are sensitive to the environment.
maybephysicallymorerealistic (7).Themathematicalanalysisinthistest
method does not cover such alternative crack velocity formulations. 5.2 Significant creep at both higher temperatures and lower
testratesresultsinnonlinearityinstress-strainrelationsaswell
4.5 In this test method, the mathematical relationship be-
as accumulated tensile damage in flexure (9). This, depending
tweenflexuralstrengthandstressratewasderivedbasedonthe
on the degree of nonlinearity, may limit the applicability of
assumption that the slow crack growth parameter is at least n
linear elastic fracture mechanics (LEFM), since the resulting
≥ 5 (1, 8). Therefore, if a material exhibits a very high
relationship between strength and stress rate derived under
susceptibility to slow crack growth, that is, n < 5, special care
constant stress-rate testing condition is based on an LEFM
should be taken when interpreting the results.
approach with negligible creep (creep strain less than 0.1%).
4.6 The mathematical analysis of test results according to
Therefore, creep should be kept as minimal as possible, as
the method in 4.4 assumes that the material displays no rising
compared to the total strain at failure (see 8.11.2).
R-curve behavior, that is, no increasing fracture resistance (or
5.3 Depending on the degree of SCG susceptibility of a
crack-extension resistance) with increasing crack length. It
material, the linear relationship between log (flexural strength)
should be noted that the existence of such behavior cannot be
and log (applied stress rate) (see Appendix X1) may start to
determinedfromthistestmethod.Theanalysisfurtherassumes
deviateatacertainhighstressrate,atwhichslowcrackgrowth
that the same flaw types control strength over the entire test
diminishes or is minimized due to the extremely short test
range. That is, no new flaws are created, and the flaws that
duration. Strengths obtained at higher stress rates (>1000
control the strength at the highest stress rate control the
MPa/s) may remain unchanged so that a plateau is observed in
strength at the lowest stress rate.
the plot of strength versus stress rate; see Fig. 1a (4).Ifthe
4.7 Slow crack growth behavior of ceramic materials can
strength data determined in this plateau region are included in
vary as a function of mechanical, material, thermal, and
the analysis, a misleading estimate of the SCG parameters will
environmental variables. Therefore, it is essential that test
beobtained.Therefore,thestrengthdataintheplateaushallbe
results accurately reflect the effects of specific variables under
excluded as data points in estimating the SCG parameters of
study. Only then can data be compared from one investigation
the material. This test method addresses this issue by recom-
to another on a valid basis, or serve as a valid basis for
mending that the highest stress rate be ≤1000 MPa/s.
characterizing materials and assessing structural behavior.
5.4 Aconsiderable strength degradation may be observed at
4.8 The strength of advanced ceramics is probabilistic in
lower stress rates and higher temperatures for some materials.
nature. Therefore, slow crack growth that is determined from
In these cases, excessive creep damage in the form of creep
the flexural strengths of a ceramic material is also a probabi-
cavities,micro-ormacro-cracks,orboth,developinthetensile
listic phenomenon. Hence, a proper range and number of test
surface (10-13). This results in a nonlinearity in the relation-
rates in conjunction with an appropriate number of specimens
ship between log (flexural strength) and log (applied stress
at each test rate are required for statistical reproducibility and
rate); see Fig. 1b. It has been reported that the strength
design (2). Guidance is provided in this test method.
degradat
...

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