This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what

changes have been made to the previous version. Because

it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.

Designation: C1525 − 04 (Reapproved 2013) C1525 − 18

Standard Test Method for

Determination of Thermal Shock Resistance for Advanced
Ceramics by Water Quenching1
This standard is issued under the fixed designation C1525; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope
1.1 This test method describes the determination of the resistance of advanced ceramics to thermal shock by water quenching.
The method builds on the experimental principle of rapid quenching of a test specimen at an elevated temperature in a water bath
at room temperature. The effect of the thermal shock is assessed by measuring the reduction in flexural strength produced by rapid
quenching of test specimens heated across a range of temperatures. For a quantitative measurement of thermal shock resistance,
a critical temperature interval is determined by a reduction in the mean flexural strength of at least 30 %. The test method does
not determine thermal stresses developed as a result of a steady state steady-state temperature differencesdifference within a
ceramic body or of thermal expansion mismatch between joined bodies. The test method is not intended to determine the resistance
of a ceramic material to repeated shocks. Since the determination of the thermal shock resistance is performed by evaluating
retained strength, the method is not suitable for ceramic components; however, test specimens cut from components may be used.
1.2 The test method is intended primarily for dense monolithic ceramics, but may also be applicable to certain composites such
as whisker- or particulate-reinforced ceramic matrix composites that are macroscopically homogeneous.
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1.3 Values expressed in this standard test method are in accordance with the International System of Units (SI) and Standard
IEEE/ASTM SI 10.
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1.4 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 appropriate safety safety, health, and healthenvironmental practices and determine the
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applicability of regulatory limitations prior to use.
1.5 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.
ASTM C1525-18
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2. Referenced Documents
2.1 ASTM Standards:2
C373 Test Methods for Determination of Water Absorption and Associated Properties by Vacuum Method for Pressed Ceramic
Tiles and Glass Tiles and Boil Method for Extruded Ceramic Tiles and Non-tile Fired Ceramic Whiteware Products
C1145 Terminology of Advanced Ceramics
C1161 Test Method for Flexural Strength of Advanced Ceramics at Ambient Temperature
C1239 Practice for Reporting Uniaxial Strength Data and Estimating Weibull Distribution Parameters for Advanced Ceramics
C1322 Practice for Fractography and Characterization of Fracture Origins in Advanced Ceramics
E4 Practices for Force Verification of Testing Machines
E6 Terminology Relating to Methods of Mechanical Testing
E616 Terminology Relating to Fracture Testing (Discontinued 1996) (Withdrawn 1996)3
IEEE/ASTM SI 10 Standard for Use of the International System of Units (SI): The Modern Metric SystemAmerican National
Standard for Metric Practice

1
This test method is under the jurisdiction of ASTM Committee C28 on Advanced Ceramics and is the direct responsibility of Subcommittee C28.01 on Mechanical
Properties and Performance.
Current edition approved Aug. 1, 2013July 1, 2018. Published September 2013July 2018. Originally approved in 2002. Last previous edition approved in 20092013 as
C1525 – 04 (2009).(2013). DOI: 10.1520/C1525-04R13.10.1520/C1525-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 C1525 − 18
2.2 European Standard:4
EN 820-3 Advanced Technical Ceramics—Monolithic Ceramics—Thermomechanical Properties—Part 3: Determination of
Resistance to Thermal Shock by Water Quenching
3. Terminology
3.1 Definitions:
3.1.1 The terms described in Terminologies C1145, E6, and E616 are applicable to this standard test method. Specific terms
relevant to this test method are as follows:
3.1.2 advanced ceramic, n—a highly engineered, high performance, predominately non-metallic, inorganic, ceramic material
having specific functional attributes. C1145
3.1.3 critical temperature difference, ∆Tc, [θ], n—temperature difference between the furnace and the ambient temperature
water bath that will cause a 30 % drop in the average flexural strength.
3.1.4 flexural strength, σf, [FL–2], n—a measure of the ultimate strength of a specified beam specimen in bending, determined
at a given stress rate in a particular environment.
3.1.5 fracture toughness, n—a generic term for measures of resistance to extension of a crack. E616
3.1.6 slow crack growth (SCG), n—subcritical crack growth (extension) which may result from, but is not restricted to, such
mechanisms as environmentally-assisted environmentally assisted stress corrosion or diffusive crack growth. C1145
3.1.7 thermal shock, n—a large and rapid temperature change, resulting in large temperature differences within or across a body.
C1145
3.1.8 thermal shock resistance, n—the capability of material to retain its mechanical properties after exposure to one or more
thermal shocks.
4. Summary of Test Method

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4.1 This test method indicates the ability of an advanced ceramic product to withstand the stress generated by sudden changes
in temperature (thermal shock). The thermal shock resistance is measured by determining the loss of strength (as compared to

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as-received specimens) for ceramic test specimens quickly cooled after a thermal exposure. A series of rectangular or cylindrical
test specimen sets areis heated across a range of different temperatures and then quenched rapidly in a water bath. After quenching,
the test specimens are tested in flexure, and the average retained flexural strength is determined for each set of specimens quenched
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from a given temperature. The “critical temperature difference” for thermal shock is established from the temperature difference
(exposure temperature minus the water quench temperature) that produces a 30 % reduction in flexural strength compared to the
average flexural strength of the as-received test specimens.
5. Significance and Use ASTM C1525-18
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The high temperature capabilities of advanced ceramics are a key performance benefit for many demanding engineering
applications. In many of those applications, advanced ceramics will have to perform across a broad temperature range with
exposure to sudden changes in temperature and heat flux. Thermal shock resistance of the ceramic material is a critical factor in
determining the durability of the component under transient thermal conditions.
5.2 This test method is useful for material development, quality assurance, characterization, and assessment of durability. It has
limited value for design data generation, because of the limitations of the flexural test geometry in determining fundamental tensile
properties.
5.3 Appendix X1 (following EN 820-3) provides an introduction to thermal stresses, thermal shock, and critical material/
geometry factors. The appendix also contains a mathematical analysis of the stresses developed by thermal expansion under steady
state steady-state and transient conditions, as determined by mechanical properties, thermal characteristics, and heat transfer
effects.
6. Interferences
6.1 Time-dependent phenomena such as stress corrosion or slow crack growth may influence the strength tests. This might
especially be a problem if the test specimens are not properly dried before strength testing.
6.2 Surface preparation of test specimens can introduce machining flaws, which may have a pronounced effect on the measured
flexural strength. The surface preparation may also influence the cracking process due to the thermal shock procedure. It is
especially important to consider surface conditions in comparing test specimens and components.
6.3 The results are given in terms of a temperature difference between furnace and quenching bath (∆T). However, it is
important to notice that results may be different for the same ∆T but different absolute temperatures. It is therefore specified in this
test method to quench to room temperature.

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 C1525 − 18
6.4 The formulae presented in this test method apply strictly only to materials that do not exhibit RR-curve-curve behavior, but
have a single-valued fracture toughness. If the test material exhibits a strong R-curve behavior, that is, increase in fracture
toughness with increasing crack length, caution must be taken in interpreting the results.
6.5 Test data for specimens of different geometries are not directly comparable because of the effect of geometry on heat transfer
and stress gradients. Quantitative comparisons of thermal shock resistance for different ceramic compositions should be done with
equivalent test specimen geometries.

7. Apparatus
7.1 Test Apparatus:
7.1.1 The test method requires a thermal exposure/quenching system (consisting of a furnace, specimen handling equipment,
and a quench bath) and a testing apparatus suitable for measuring the flexural strength of the test specimens.
7.1.2 The test method requires a furnace capable of heating and maintaining a set of test specimens at the required temperature
to 6 5 K (6 5°C). 65 K (65 °C). The temperature shall be measured with suitable thermocouples located no more than 2 mm
2 mm from the midpoint of the specimen(s) in the furnace. Furnaces will usually have an open atmosphere, because air exposure
is common during the transfer to the quench bath.
NOTE 1—If air exposure is detrimental, a special furnace-quench system can be set up in which both the furnace and the quench unit are contained
within an inert atmosphere container. A common design for such a system consists of a tube furnace positioned vertically above the quench tank, so that
the test specimen drops directly into the tank from the furnace.
7.1.3 The method requires a test specimen handling equipment designed so that the test specimen can be transferred from the
furnace to the quenching bath within 5 s.
7.1.4 A water bath controlled to 293 6 2 K (20°C(20 6 2°C)2 °C) is required. The water bath must have sufficient volume to
prevent the temperature in the bath from rising more than 5 K (5°C)(5 °C) after test specimen quenching. It is recommended that
the bath be large enough for the test specimens to have cooled sufficiently before reaching the bottom of the bath, or contain a
screen near the bottom to prevent the test specimens from resting directly on the bottom of the bath.
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7.1.5 The universal test machine used for strength testing in this test method shall conform to the requirements of
PracticePractices E4. Specimens may be loaded in any suitable test machine, provided that uniform test rates, either rates using
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either load-controlled or displacement-controlled mode,mode can be maintained. The loads used in determining flexural strength
shall be accurate to within 61.0 % at any load within the selected load rate and load range of the test machine as defined in

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PracticePractices E4.
7.1.6 The configuration and mechanical properties of the test fixtures shall be in accordance with Test Method C1161 for use
with the standard four-point flexure specimens. If larger test pieces (sizes(size A or C below) are employed, the test fixture shall
be scaled accordingly. There are currently no standard fixtures for testing cylindrical rods in flexure; however, the fixtures to be
ASTM
used shall have the appropriate articulation. Test fixtures C1525-18
without appropriate articulation shall not be permitted; the articulation
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fixture shall meet the requirements specified in Test Method C1161.
7.1.7 The method requires a 393 K (120°C)(120 °C) drying oven to remove moisture from test specimens before (if needed)
and after quench testing.
7.1.8 A micrometer with a resolution of 0.002 mm (or 0.0001 in.) or smaller should be used to measure the test piece
dimensions. The micrometer shall have flat anvil faces. The micrometer shall not have a ball tip or sharp tip, since these might
damage the test piece if the specimen dimensions are measured prior to fracture. Alternative dimension measuring instruments may
be used, provided that they have a resolution of 0.002 mm (or 0.0001 in.) or finer and do no harm to the specimen.

8. Test Specimens
8.1 The ceramic test specimens shall be pieces specifically prepared for this purpose from bulk material or cut from components.
8.1.1 Specimen Size—Three specimen geometries are defined for use in this test method:
8.1.1.1 Type A—Rods 10 6 0.13 mm in diameter, 120 mm long.
8.1.1.2 Type B—Bars 3 6 0.13 mm × 4 6 0.13 mm in cross section, minimum 45 mm long with chamfered edges, in accordance
with typeType B in Test Method C1161.
8.1.1.3 Type C—Bars 10 6 0.13 mm × 10 6 0.13 mm in cross section, 120 mm long, with chamfered edges.
NOTE 2—The test specimens of Types A and C type are intended to be large enough to produce a materials ranking that is basically independent of
specimen size and appropriate for larger test specimens (1, 2)).5. Test specimens of Type B type may require greater quenching temperature differences
in order to produce strength reduction. These test specimens may not correctly rank the relative behavior of larger components. Only Type B coincides
with Type B in Test Method C1161.
NOTE 3—Under some circumstances, the edges of prismatic test specimens or the ends of cylindrical test specimens may be damaged by spallation
during the quench test. These specimens should be discarded from the batch used for strength testing if the damage will interfere with the strength test.
In any case, such spallation must be noted in the report. Spallation problems can be alleviated by chamfering sharp edges.
NOTE 4—The parallelism tolerances on the four longitudinal faces are 0.015 mm for B and C and the cylindricity for A is 0.015 mm.

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The boldface numbers in parentheses refer to a list of references at the end of this standard.

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 C1525 − 18
8.2 Test Specimen Preparation—Depending on the intended application of the thermal shock data, one of the four test specimen
preparation methods described in Test Method C1161 may be used: As-Fabricated, Application-Matched Machining, Customary
Procedures, or Standard Procedures.as-fabricated, application-matched machining, customary procedures, or standard procedures.
8.3 Handling Precautions—Care shall be exercised in storing and handling of test specimens to avoid the introduction of
random and severe flaws, such as might occur if test specimens were allowed to impact or scratch each other.
8.4 Number of Test Specimens—A minimum of 10ten specimens shall be used to determine as-received strength at room
temperature. A minimum of 30 is required if estimates regarding the form of the strength distribution isare to be determined (for
example, a Weibull modulus). A minimum of 5five specimens shall be used at each thermal shock temperature. It is recommended
that as ∆Tc is established, an additional 5five specimens be tested at this as well as the adjacent temperature intervals. This will
allow for determination of the mean and standard deviation. If estimates regarding the form of the strength distribution at the ∆Tc
and adjoining temperature intervals are desired (for example, Weibull analysis) additional specimens must be tested at these
temperature intervals. See Practice C1239 for guidance on estimating Weibull parameters.

9. Procedure
9.1 Test Exposure Temperatures:
9.1.1 The maximum exposure target temperature of the furnace for the thermal shock test of a given advanced ceramic will be
determined from the maximum performance temperature required for a specific application, specified in a comparative thermal
shock test, or cited in test literature.
9.1.2 The initial exposure temperature can be determined from literature values, prior test experience, or from a 50 % value of
the maximum exposure temperature. Follow-on exposure/quench tests shall be performed such that the critical temperature
difference is determined within a 50 K (50°C)(50 °C) interval.
9.1.3 An efficient “bracketing” search technique for ∆Tc can be employed wherein the initial exposure temperature is chosen
high enough that a definitive strength drop (>30 % of as-received strength, see Fig. 1) is expected and observed. (If the strength
drop is not observed, repeat the test with a higher initial temperature.) The second exposure temperature is chosen at the midpoint
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of the first exposure temperature and room temperature. Each subsequent exposure temperature is selected at the midpoint between
the lowest temperature producing a >30 % strength drop and the highest temperature to produce a <30 % strength drop. (See Figs.
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2 and 3.) Continue the iteration until the temperature interval is between iterations is less than 100°C.100 °C. This search procedure
minimizes the number of iterations needed to identify the ∆Tc, as compared to a stepwise fixed increment search procedure.

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9.2 Clean the test specimens in water or alternate fluid to remove any cutting solutions or other contaminants. A final rinse in
or ethanol is recommended. Determine the thickness and width of each test specimen
in accordance with Test Method C1161. Determine the mass of each test specimen to an accuracy of 0.1%0.1 % or better. Calculate
the bulk density for each specimen (Bulk density = mass / (length x× width x× thickness)
ASTM C1525-18
NOTE 5—If the calculated bulk density varies significantly (<3%)(<3 %) between specimens or if the mean of the density for all the specimens is 95
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% or less of the theoretical density of the test material, specimen porosity may be a critical experimental factor in thermal shock. If the porosity in
specimens is of concern, the apparent porosity and apparent specific gravity of selected specimens may be measured prior to thermal shock testing using

FIG. 1 Typical Plot of Average Strength Versusversus Quenching Temperature Difference (Not for a Specific Material)

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FIG. 2 Example of a Temperature Sequence Using the (Bracketing( Technique for a Material Withwith a Low Thermal Shock Resis-
tance.Resistance

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ASTM C1525-18
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FIG. 3 Example of a Temperature Sequence Using the (Bracketing( Technique for a Material Withwith a High Thermal Shock Resis-
tance.Resistance

an Archimedes density measurement (Test MethodMethods C373) and reported. Specimens that have been measured by Test MethodMethods C373
should be thoroughly dried out per paragraph9.3.
9.3 Dry the test specimens in an oven at 393 6 10 K (120 6 10°C)10 °C) for 2 h. Allow the specimens to cool to room
temperature in a dessicator. Select the specimens for quench testing and store in the dessicator until furnace exposure.
9.4 Perform the initial flexural strength test on at least 10ten test specimens in accordance with Test Method C1161, using the
appropriate test machine and fixture.
9.5 Determine the mean and standard deviation of the strength of the as-received specimens.
9.6 Place the first set (minimum five test specimens) of quench test specimens in the cold furnace and heat slowly
[minimum(minimum 30 min to temperatures up to 873 K (600°C);(600 °C); minimum 60 min to temperature greater than 873 K
(600°C)](600 °C)) to the initial exposure temperature. Equilibrate at the exposure temperature for a period of 15 min and
check/record the exposure temperature. After equilibration, remove the test specimens singly from the furnace, and transfer each
of them to the quench bath as quickly as possible, but in no more than 5 s. 5 s. A specific orientation of the specimens during this
operation is not required.

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 C1525 − 18
9.7 After quenching, dry the test specimens in the drying oven and store, if necessary, in a dessicator per 9.3, before strength
testing at room temperature.
9.8 Conduct strength tests on the quenched and dried test specimens in flexure at room temperature in accordance with Test
Method C1161.
9.9 Calculate flexural strength according to Section 10, and compare the average flexural strength for the quenched test
specimens to the strength of the as-received test specimens. A 30 % decrease in flexural strength for a given ∆T will meet the
critical ∆T requirement,requirement; see Figs. 2 and 3.
9.10 Once the exposure temperature for the ∆T is determined, repeat the test exposure/quench/strength test for the critical
temperature as well as for one 50 K (50°C)(50 °C) temperature interval above and one below this ∆T. Calculate average flexural
strength and standard deviation for the three sets of test specimens and compare those values with those obtained for the
as-received test specimens. Often an increase in the standard deviation is observed for the sets tested around ∆Tc (43), and this may
help in determining the critical temperature interval. An example of a typical graph of average strength versus temperature interval
is given in Fig. 1.
9.11 If desired, expose and test additional test sets to determine the strength reduction across the entire temperature regime of
interest.
9.12 Performing fractographic analysis according to Practice C1322 is recommended for the as-received test specimens as well
as for the test specimens tested at ∆Tc. Fractography could be helpful in determining the location and source of critical fracture
flaws in the as-received test specimens and assessing if thermal shock produces a change in the critical flaw population with a
corresponding strength drop.

10. Calculation

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10.1 Evaluate flexural strength of the prismatic test specimens according to the formula for four-point flexure (see Test Method
C1161):

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~ !
S5
3 P Lo 2 Li
2b d 2
(1)

where:
S = flexural strength, Pa,
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P = measured fracture load, N,
Lo and Li = outer and inner spans, respectively, m, ASTM C1525-18
b = test specimen width, m, and
d https://standards.iteh.ai/catalog/standards/sist/9df619ba-77f0-44ac-9116-11697d15e7cc/astm-c1525-18
= test specimen height, m.
Evaluate the strength of cylindrical test specimens as follows:
P ~ L o 2 L i!
S5 (2)
π r3

where:
r = radius of the test specimen cylinder.
10.2 Evaluate the mean, S¯, and standard deviation, SD, according toto:
n

H
(S 1
S5 (3)
n

!
n

( ~ S 2 HS !
2

1
SD 5 (4)
~n 2 1!
10.3 Calculate the ∆T for each exposure/quench test, where:
∆T 5 T x 2 T 0 (5)

where:
Tx = exposure test temperature, K or °C, and
T0 = quench bath temperature, K or °C.
10.4 Plot the mean flexural strength and the standard deviations for each test set versus the ∆T, , as shown in Fig. 1.