Designation: C 1470 – 06

Standard Guide for

Testing the Thermal Properties of Advanced Ceramics1
This standard is issued under the fixed designation C 1470; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents

1.1 This guide covers the thermal property testing of ad- 2.1 ASTM Standards: 2
vanced ceramics, to include monolithic ceramics, particulate/ 2.1.1 Specific Heat:
whisker-reinforced ceramics, and continuous fiber-reinforced C 351 Test Method for Mean Specific Heat of Thermal
ceramic composites. It is intended to provide guidance and Insulation
information to users on the special considerations involved in D 2766 Test Method for Specific Heat of Liquids and Solids
determining the thermal properties of these ceramic materials. E 1269 Test Method for Determining Specific Heat Capac-
1.2 Five thermal properties (specific heat capacity, thermal ity by Differential Scanning Calorimetry
conductivity, thermal diffusivity, thermal expansion, and 2.1.2 Thermal Conductivity:
emittance/emissivity) are presented in terms of their definitions C 177 Test Method for Steady-State Heat Flux Measure-
and general test methods. The relationship between thermal ments and Thermal Transmission Properties by Means of
properties and the composition, microstructure, and processing the Guarded-Hot-Plate Apparatus
of advanced ceramics (monolithic and composite) is briefly C 182 Test Method for Thermal Conductivity of Insulating
outlined, providing guidance on which material and specimen Firebrick
characteristics have to be considered in evaluating the thermal C 201 Test Method for Thermal Conductivity of Refracto-
properties of advanced ceramics. Additional sections describe ries
sampling considerations, test specimen preparation, and report- C 202 Test Method for Thermal Conductivity of Refractory
ing requirements. Brick
1.3 Current ASTM test methods for thermal properties are C 408 Test Method for Thermal Conductivity of Whiteware
tabulated in terms of test method concept, testing range, Ceramics
specimen requirements, standards/reference materials, capa- C 518 Test Method for Steady-State Thermal Transmission
bilities, limitations, precision, and special instructions for Properties by Means of the Heat Flow Meter Apparatus
monolithic and composite ceramics. C 767 Test Method for Thermal Conductivity of Carbon
1.4 This guide is based on the use of current ASTM Refractories
standards for thermal properties where appropriate and on the C 1044 Practice for Using a Guarded-Hot-Plate Apparatus
development of new test standards where necessary. It is not or Thin-Heater Apparatus in the Single-Sided Mode
the intent of this guide to rigidly specify particular thermal test C 1045 Practice for Calculating Thermal Transmission
methods for advanced ceramics. Guidance is provided on how Properties Under Steady-State Conditions
to utilize the most commonly available ASTM thermal test C 1113 Test Method for Thermal Conductivity of Refracto-
methods, considering their capabilities and limitations. ries by Hot Wire (Platinum Resistance Thermometer Tech-
1.5 The values stated in SI units are to be regarded as the nique)
standard per IEEE/ASTM SI 10. C 1114 Test Method for Steady-State Thermal Transmission
1.6 This standard does not purport to address all of the Properties by Means of the Thin-Heater Apparatus
safety concerns, if any, associated with its use. It is the C 1130 Practice for Calibrating Thin Heat Flux Transducers
responsibility of the user of this standard to establish appro- E 1225 Test Method for Thermal Conductivity of Solids by
priate safety and health practices and determine the applica- Means of the Guarded-Comparative-Longitudinal Heat
bility of regulatory limitations prior to use. Flow Technique

1
This guide is under the jurisdiction of ASTM Committee C28 on Advanced
2
Ceramics and is the direct responsibility of Subcommittee C28.03 on Physical For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Properties and Performance. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Current edition approved Jan. 1, 2006. Published February 2006. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 2000. Last previous edition approved in 2000 as C 1470 – 00. the ASTM website.

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

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 C 1470 – 06
E 1530 Test Method for Evaluating the Resistance to Ther- 3.1.3 coeffıcient of linear thermal expansion, a[T -1], n—the
mal Transmission of Materials by the Guarded Heat Flow change in length, relative to the length of the specimen,
Meter Technique accompanying a unit change of temperature, at a specified
2.1.3 Thermal Expansion: temperature. [This property can also be considered the instan-
C 372 Test Method for Linear Thermal Expansion of Por- taneous expansion coefficient or the slope of the tangent to the
celain Enamel and Glaze Frits and Fired Ceramic Whitew- DL/L versus T curve at a given temperature.] (E 1142)
are Products by the Dilatometer Method 3.1.4 continuous fiber-reinforced ceramic composite
C 1300 Test Method for Linear Thermal Expansion of (CFCC), n—a ceramic matrix composite in which the reinforc-
Glaze Frits and Ceramic Whiteware Materials by the ing phase(s) consists of continuous filaments, fibers, yarns, or
Interferometric Method knitted or woven fabric. (C 1145)
E 228 Test Method for Linear Thermal Expansion of Solid 3.1.5 differential scanning calorimetry (DSC), n—a tech-
Materials With a Vitreous Silica Dilatometer3 nique in which the difference in energy inputs into a test
E 289 Test Method for Linear Thermal Expansion of Rigid specimen and a reference material is measured as a function of
Solids with Interferometry temperature while the test specimen and reference material are
E 831 Test Method for Linear Thermal Expansion of Solid subjected to a controlled temperature program. (E 1269)
Materials by Thermomechanical Analysis 3.1.6 discontinuous fiber-reinforced ceramic composite,
2.1.4 Thermal Diffusivity: n—a ceramic matrix composite reinforced by chopped fibers.
C 714 Test Method for Thermal Diffusivity of Carbon and (C 1145)
Graphite by Thermal Pulse Method 3.1.7 emittance (emissivity), e (nd), n—the ratio of the
E 1461 Test Method for Thermal Diffusivity by the Flash radiant flux emitted by a specimen per unit area to the radiant
Method flux emitted by a black body radiator at the same temperature
2.1.5 Emittance/Emissivity: and under the same conditions. Emittance ranges from 0 to 1,
E 408 Test Methods for Total Normal Emittance of Surfaces with a blackbody having an emittance of 1.00. (E 423)
Using Inspection-Meter Techniques 3.1.8 linear thermal expansion, [nd], n—the change in
E 423 Test Method for Normal Spectral Emittance at El- length per unit length resulting from a temperature change.
evated Temperatures of Nonconducting Specimens Linear thermal expansion is symbolically represented by DL/
2.1.6 General Standards: L0, where DL is the observed change in length DL = L2 – L1,
C 373 Test Method for Water Absorption, Bulk Density, and L0, L1, and L2 are the lengths of the specimen at reference
Apparent Porosity, and Apparent Specific Gravity of Fired temperature T0 and test temperatures T1 and T2. (E 228)
Whiteware Products
3.1.9 mean coeffıcient of linear thermal expansion, aL [T -1],
C 1145 Terminology of Advanced Ceramics
n—the change in length, relative to the length of the specimen,
E 122 Practice for Calculating Sample Size to Estimate,
accompanying a unit change of temperature measured across a
With a Specified Tolerable Error, the Average for a
specified temperature range (T1 to T2). (C 372)
Characteristic of a Lot or Process
E 473 Terminology Relating to Thermal Analysis and Rhe- 3.1.10 particulate reinforced ceramic matrix composite,
ology n—a ceramic matrix composite reinforced by ceramic particu-
E 1142 Terminology Relating to Thermophysical Properties lates. (C 1145)
C 1045 Practice for Calculating Thermal Transmission 3.1.11 specific heat (specific heat capacity), C [mL–1T–2u–1],
Properties Under Steady-State Conditions n—the quantity of heat required to provide a unit temperature
IEEE/ASTM SI 10 Standard for Use of the International increase to a unit mass of material. (E 1142)
System of Units (SI) (The Modern Metric System) 3.1.12 thermal conductivity, l [mLT–1u–1], n—the time rate
of heat flow, under steady conditions, through unit area, per
3. Terminology unit temperature gradient in the direction perpendicular to the
3.1 Definitions: area. (E 1142)
2 –1
3.1.1 advanced ceramic, n—a highly engineered, high- 3.1.13 thermal diffusivity, [L T ], n—the property given by
performance, predominantly nonmetallic, inorganic, ceramic the thermal conductivity divided by the product of the bulk
material having specific functional attributes. (C 1145) density and heat capacity per unit mass. (E 1461)
3.1.2 ceramic matrix composite, n—a material consisting of 3.1.14 thermodilatometry, n—a technique in which a di-
two or more materials (insoluble in one another), in which the mension of a test specimen under negligible applied force is
major continuous component (matrix component) is a ceramic, measured as a function of temperature while the test specimen
while the secondary component/s (reinforcing component) may is subjected to a controlled temperature program in a specified
be ceramic, glass-ceramic, glass, metal, or organic in nature. atmosphere. (E 473)
These components are combined on a macroscale to form a 3.2 Units for Thermal Properties:
useful engineering material possessing certain properties or Property SI Units Abbreviation
behavior not possessed by the individual constituents. Specific heat capacity joules/(gram-kelvin) J/(g·K)
Thermal Conductivity watts/(metre-kelvin) W/(m·K)
(C 1145) Thermal diffusivity metre/second2 m/s2
Coefficient of Thermal metre/(metre-kelvin) K–1
Expansion
3
Withdrawn. Emittance/emissivity no dimensions —

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 C 1470 – 06
4. Summary of Guide 7. Thermal Properties and Their Measurement
4.1 Five thermal properties (specific heat capacity, thermal 7.1 Specific Heat Capacity:
conductivity, thermal diffusivity, thermal expansion, and 7.1.1 Specific heat capacity is the amount of energy required
emittance/emissivity) are presented in terms of their definitions to increase the temperature by one unit for a unit mass of
and general test methods. The relationship between thermal material. It is a fundamental thermal property for engineers and
properties and the composition, microstructure, and processing scientists in determining the temperature response of materials
of advanced ceramics is briefly outlined, providing guidance to changes in heat flux and thermal conditions. The SI units for
on which material characteristics have to be considered in specific heat capacity are joules/(gram·K). Since the specific
evaluating the thermal properties. Additional sections describe heat capacity changes with temperature, a specific heat capac-
sampling considerations, test specimen preparation, and report- ity value must always be associated with a specific test
ing requirements. temperature or temperature range.
4.2 Current ASTM test methods for thermal properties are 7.1.2 Specific heat capacity is commonly measured by
tabulated in terms of test method concept, testing range, calorimetry in which changes in thermal energy are measured
specimen requirements, standards/reference materials, capa- against changes in temperature. The two common calorimetry
bilities, limitations, precision, and special instructions for methods are differential scanning calorimetry and drop calo-
monoliths and composites. rimetry.
5. Significance and Use 7.1.3 Differential scanning calorimetry heats the test mate-
rial at a controlled rate in a controlled atmosphere through the
5.1 The high-temperature capabilities of advanced ceramics temperature region of interest. The heat flow into the test
are a key performance benefit for many demanding engineering material is compared to the heat flow into a reference material
applications. In many of those applications, advanced ceramics to determine the energy changes in the test material as a
will have to perform across a broad temperature range. The function of temperature.
thermal expansion, thermal diffusivity/conductivity, specific
7.1.4 In drop calorimetry, the test sample is heated to the
heat, and emittance/emissivity are crucial engineering factors
desired temperature and then immersed in an instrumented,
in integrating ceramic components into aerospace, automotive,
liquid-filled container (calorimeter), which reaches thermal
and industrial systems
equilibrium. The increase in temperature of the calorimeter
5.2 This guide is intended to serve as a reference and
liquid/container is a measure of the amount of heat in the test
information source for testing the thermal properties of ad-
specimen.
vanced ceramics, based on an understanding of the relation-
7.1.5 In any calorimetry test, the experimenter must recog-
ships between the composition and microstructure of these
nize that phase changes and other thermo-physical transforma-
materials and their thermal properties.
tions in the material will produce exothermic and endothermic
5.3 The use of this guide assists the testing community in
events which will be captured in the test data. The thermal
correctly applying the ASTM thermal test methods to advanced
events must be properly identified and understood within the
ceramics to ensure that the thermal test results are properly
context of the material properties, chemistry, and phase com-
measured, interpreted, and understood. This guide also assists
position across the temperature range of interest.
the user in selecting the appropriate thermal test method to
evaluate the particular thermal properties of the advanced 7.2 Thermal Conductivity:
ceramic of interest. 7.2.1 Thermal conductivity is a measurement of the rate of
5.4 The thermal properties of advanced ceramics are critical heat flow through a material for a given temperature gradient.
data in the development of ceramic components for aerospace, It is normalized for thickness and cross-sectional area to give
automotive, and industrial applications. In addition, the effect a material specific value. The thermal conductivity of a ceramic
of environmental exposure on thermal properties of the ad- is used in determining the effectiveness of a ceramic either as
vanced ceramics must also be assessed. a thermal insulator or as a thermal conductor. The SI units for
thermal conductivity are watts/(metre·kelvin). As with other
6. Procedure thermal properties, thermal conductivity changes with tem-
6.1 Review Sections 7-10 to become familiar with thermal perature, so that a thermal conductivity value for a material
property concepts and thermal testing issues for advanced must be associated with a specific test temperature.
ceramics, specimen preparation guidance, and reporting rec- 7.2.2 In electrically nonconductive ceramics, thermal con-
ommendations. ductivity occurs by lattice vibration (phonon) conductivity and
6.2 Review the test method text and tables in Section 11 for by radiation (photon) at higher temperatures (>500°C). Ther-
the property you need to determine. Use the text and tables to mal conductivity decreases when the mean free path of the
help select the most appropriate ASTM test method for phonons and photons decreases. Lattice imperfections, differ-
evaluating the thermal property of interest for the specific ences in atomic weight between anions and cations, non-
advanced ceramic. stoichiometric compositions, solid solutions, amorphous
6.3 Perform the thermal property test in accordance with the atomic structures, porosity, and grain boundaries all act as
selected ASTM test method, but refer back to the guide for scattering sites for phonons and reduce the thermal conductiv-
directions and recommendations on material characterization, ity of the material.
sampling procedures, test specimen preparation, and reporting 7.2.3 Thermal conductivity is commonly measured by
results. steady-state methods, that is, cut bar comparative techniques,

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 C 1470 – 06
heat flow meter techniques, guarded hot-plate/heater/hot-wire coefficient of thermal expansion, which is the tangent slope at
techniques, and calorimetry techniques. It can also be deter- a specific temperature for the expansion-temperature curve of
mined by transient techniques (hot wire and flash diffusivity). the sample.
7.2.4 In cut bar comparative heat flow techniques, the test 7.3.6 Thermal expansion is commonly measured by ther-
specimen is subjected to a known heat flow and the tempera- modilatometry, a technique in which a known dimension of a
ture differential/s are measured across the dimension/s of test specimen under negligible applied force is measured as a
interest. The entire test system with the test specimen is function of temperature while the specimen is subjected to a
configured with insulation and heaters to minimize heat flow controlled-temperature program in a specified atmosphere. The
perpendicular to the direction of interest. In the heat flowmeter measurement of the dimensional change can be done by direct
technique, the heat flow in the test is measured by a calibrated mechanical measurement or by optical techniques (interferom-
heat flux transducer without the use of direct reference mate- etry and optical lever)
rials in the test system. In both techniques, the thermal
7.3.7 Different crystalline phases in ceramics have different
conductivity of the material is then calculated as follows:
thermal expansion characteristics. Major phase changes in
l 5 q D L/ ~D T! (1) ceramics can give abrupt or progressive changes in length with
where: increasing or decreasing temperature and may cause confusion
l = thermal conductivity, when included in overall expansion measurements. In a similar
q = heat flow/unit area, manner, crystallization and changes in amorphous, glassy
DL = distance across which the temperature difference is phases in ceramics can produce marked changes in the thermal
measured, and expansion over specific temperature regimes.
D T = measured temperature difference. 7.3.8 Thermal expansion measurements for ceramics often
Thermal conductivity can be calculated from thermal diffu- show heating/cooling hysteresis when microcracking or minor
sivity measurements, using the specific heat capacity and the phase changes occur. There are also irreversible thermal
material density as follows: expansion effects, based on annealing, heating rate, creep,
l 5 thermal diffusivity * specific heat capacity * density (2) crystallization, or microcracking. Thermal expansion tests
done only on heating can be misleading, and thermal expansion
7.3 Thermal Expansion (Thermodilatometry):
measurements should be done under both heating and cooling
7.3.1 All materials expand or contract with changes in conditions.
temperature, with most materials expanding with increasing
7.4 Thermal Diffusivity:
temperature. Thermal expansion is often very important in
engineering applications, because differences in thermal ex- 7.4.1 Thermal diffusivity is a measurement of the rate of
pansion between fitted or bonded components can produce temperature change in a material measured under transient
thermal stresses, leading to component failure. conditions. It is defined as the ratio of the thermal conductivity
7.3.2 The thermal expansion for a given ceramic composi- to the “specific heat capacity per unit volume” (which is the
tion and phase is a function of crystal structure and of atomic specific heat capacity divided by the bulk density), as follows:
bond strength. In ceramics with anisotropic crystal structures, Diffusivity 5 l / ~Cp / r! (4)
the thermal expansion is different along the different crystal
axes. (This is of particular concern for single crystal specimens where:
and for specimens with oriented grain structures). For some l = thermal conductivity,
Cp = specific heat capacity, and
specific ceramics (cordierite, aluminum titanate, and zirconium
r = the bulk density,
phosphate), the thermal expansion may be zero or negative in
all at the specific temperature of measurement.
certain crystal axes in specific temperature regimes.
7.3.3 The quantitative determination of the change in di- The units of thermal diffusivity are metre/second2.
mension as a function of temperature is defined as the mean 7.4.2 Thermal diffusivity is important in characterizing the
coefficient of linear thermal expansion – the ratio of a given transient thermal response of ceramics that are used in heat
change in length per unit length for a specimen for a specific transfer applications, either as insulators or as thermal conduc-
change in temperature as follows: tion paths. As with the other thermal properties that change
with temperature, a specific thermal diffusivity value must be
a 5 [~L2 – L1!/~T2 – T1!#/L1 (3)
defined for a specific temperature or a temperature range.
where: 7.4.3 Thermal diffusivity is experimentally determined by
L1 and L2 = lengths of the test specimen at test tempera- measuring the temperature-time response of a material to a
tures T1 and T2, respectively, where T2 > T1. thermal event. The current method of choice is flash diffusivity,
7.3.4 The units for mean coefficient of linear thermal in which one side of a specimen of known thickness and
expansion are metres/(metre · K). The mean coefficient of temperature is subjected to a short duration thermal pulse. The
linear thermal expansion for a material has to be defined for a energy of the pulse is absorbed on the front surface of the
given temperature range, for example, 7 3 10–6 m/(m·K) for 25 specimen and the resulting rear face temperature rise is
to 500°C. measured. Thermal diffusivity is calculated from the specimen
7.3.5 The mean coefficient of linear thermal expansion thickness and the time required for the rear face temperature to
across a temperature range is different than the instantaneous reach a specified percentage of its maximum value.

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 C 1470 – 06
TABLE 1 Nominal Thermal Properties for Monolithic Ceramics at Room Temperature
NOTE 1—Thermal property data obtained from reference books and producer specifications. Values are approximate for a given class of material and
are provided for the sake of general comparison. Actual values in specific test specimens will depend on composition, microstructure, porosity, and other
factors. Emittance/emissivity data from—Thermal Radiative Properties, Nonmetallic Solids, Touloukian, Y. S. and DeWitt, D.P., I.F. I. Plenum, 1972.
Alumina, Silicon Silicon Aluminum Boron
Property at Room Temperature Zirconia Mullite Beryllia Cordierite
99.5 % Nitride Carbide Nitride Nitride
3
Density, g/cm 3.85 3.31 3.10 3.25 2.10 6.02 2.80 2.90 2.30
Specific heat capacity, [J/(g·K)] 0.92 0.69 0.67 0.78 0.79 0.45 0.77 1.04 0.74
Thermal conductivity, [W/(m·K)] 35.6 15 110 115 32.8 2.2 3.5 250 3.0
Thermal diffusivity, m2/s 3 10-6 10.0 6.6 53.0 45.4 19.8 0.8 1.6 82.9 1.8
Coefficient of linear thermal expan- 8.0 3.0 4,4 5.7 10 10.3 5.3 8.7 1.7
sion, 10-6/K (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C) (25–1000°C)
Emittance/Emissivity, 1000°C 0.1-0.3 0.7-0.9 0.7-0.9 0.7-0.9 0.7-0.9 0.1-0.3 0.4 '0.3 NA

7.4.4 All of the microstructural variables that have an roughness, radiation wavelength, and observation angle. The
impact on thermal conductivity will have a similar effect on the relative radiant flux of a given material can be characterized by
thermal diffusivity. the term emittance (also called emissivity). Emittance is the
7.5 Emittance/Emissivity: ratio of the radiant flux emitted by a specimen per unit area to
7.5.1 All objects radiate energy depending on their tempera- the radiant flux emitted by blackbody radiator at the same
ture and their radiative characteristics. This radiation is called temperature and under the same conditions.
thermal radiation, because it is strongly dependent on tempera- 7.5.6 Emittance is determined by measuring the emitted
ture. A perfect emitter (a blackbody) emits radiation across a thermal radiation at a given temperature and then comparing it
range of wavelengths according to its surface temperature to a reference standard of known emittance or by direct
through the Planck radiation equation. The amount of hemi- comparison to an experimental “blackbody” at the same
spherical radiated energy per unit surface area at a given temperature.
temperature for a blackbody is calculated through the Stefan-
Boltzmann’s law as follows: 8. Test Specimen Characterization
Eb,total 5 5.670 3 10–8 * T4@W/~m2 · K4!# (5)
8.1 Introduction:
8.1.1 Advanced ceramics, both monolithic and composite,
where: offer a wide range of thermal properties, from thermal insula-
T = specimen temperature for hemispherical emittance tors to thermal conductors. Nominal thermal property values
7.5.2 At high temperatures, the emittance of radiation by a for a range of advanced monolithic ceramics are given in Table
material has significant impact on its thermal condition, based 1. Note the range of thermal properties listed in the table.
on how the thermal radiation is emitted, absorbed, and re- Advanced ceramics such as aluminum nitride and beryllia with
flected. For advanced ceramics operating at high temperatures their high thermal conductivity are often used as thermal
(>600°C) where radiation is a major mode of heat transfer, the conductors.
emittance properties of the ceramic are necessary to model the 8.1.2 Table 2 provides nominal thermal properties for dif-
thermal conditions and to determine the heat transfer rates ferent types of ceramic fibers used in continuous fiber-
under heating and cooling conditions. reinforced ceramic matrix composites. When these different
7.5.3 The measurement of emittance has a directional com- ceramic fibers are combined with different ceramic matrices,
ponent based on the observation angle to the plane of the the resulting composites can contain constituents whose ther-
sample. Directional emittance is measured at a specific obser- mal properties are widely different.
vation angle. Normal emittance is a special case of directional 8.1.3 The range of thermal properties for advanced ceramics
emittance, measured normal to the plane of the sample. and the complexity inherent in ceramic composites require a
Hemispherical emittance is measured by integration over the detailed understanding of the relationships between composi-
entire range of solid observation angles. tion, processing, microstructure, and thermal properties in
7.5.4 Emittance can also be characterized as either “total” or those ceramics. With that understanding, test operators will
“spectral.” Total emittance is a measurement of the radiant ensure that thermal test results for advanced ceramics are valid,
energy across the entire range of thermal wavelengths and is useful, and reproducible.
commonly utilized for total radiation pyrometry and radiant 8.2 Material Characteristics and Thermal Properties:
heat transfer analysis. Spectral emittance is a measurement of 8.2.1 Advanced ceramics cover a broad range of composi-
the radiant energy at/across a particular portion of the tions, microstructures, and physical properties. It is not pos-
wavelength/frequency spectrum. The emittance at a particular sible to give specific guidance for every current or future
frequency is important in temperature measuring equipment, advanced ceramic material, but general guidelines and infor-
such as optical pyrometers. mation are provided on the effects of composition, microstruc-
7.5.5 Most materials are not perfect emitters. The emission ture, and processing on the thermal properties of advanced
of radiation from a surface depends on many factors: tempera- ceramics and on thermal property measurement.
ture, bulk composition, surface composition (impurities, coat- 8.2.2 The thermal properties of an advanced ceramic
ings, and oxidation), optical transparency, surface profile/ (monolithic or composite) are a function of the material

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 C 1470 – 06
TABLE 2 Nominal Thermal Properties of Ceramic Fibers at Room Temperature
NOTE 1—Thermal property data obtained from reference books and producer specifications. Values are approximate and are provided for the sake of
general comparison. Actual values in specific test specimens will depend on composition, microstructure, porosity, architecture, and other factors.
T-300 P-120
Property at Room Temperature Nicalon CGA Hi-NicalonA Hi-Nicalon SA Sylramic SiCA Nextel 312B Nextel 610B Nextel 720B
CarbonC CarbonC
Nominal composition Silicon Silicon Silicon Silicon Alumino- Alumina Alumina- Carbon Graphite
Carbide Carbide Carbide Carbide borosilicate Mullite
Density, g/cm3 2.55 2.74 3.10 3.20 2.70 3.88 3.40 1.76 2.17
Specific Heat, [J/(g·K)] 1.14 .067 NA 0.61 '0.7 '0.9 '0.85 '0.70 '0.70
Thermal conductivity, [W/(m·K)] 2.97 7.77 18.4 40-45 '3(est) '30 (est) '10 (est) 8.5 640
Coefficient of Linear Thermal Ex- 4.0 3.5 NA 5.4 3.0 7.9 6.0 –1.4 at –1.45 at
pansion, 10–6/K (0–900°C) (0–500°C) (20–1320°C) (100–1100°C) (100–1100°C) (100–1100°C) (23°C) (23°C)
A
CDI Ceramics, Inc., San Diego, CA.
B
3M Corp., St. Paul, MN.
C
Amoco Performance Products, Alpharetta, GA.

composition and constituents, its microstructure, its processing temperature or if oxidation reactions (surface or bulk) occur at
history, and its environmental exposure. For example, porosity elevated temperatures. Oxidation-sensitive materials should be
has a very strong effect on thermal conductivity and diffusivity. tested in inert atmospheres. Accelerated heating rates can also
In a similar manner, composites containing high thermal produce test anomalies, because of nonuniform temperatures
conductivity components can be tailored to specific thermal within a test specimen. Thermal tests should always be done
property targets by changing the amount and the architecture of with the test specimen in relative steady-state thermal equilib-
the reinforcing component. The advanced ceramic must be rium, unless transient properties are specifically desired.
adequately characterized in terms of composition, constituents, 8.3 Monolithic Ceramics—Material Variables:
microstructure, processing methods, and exposure history. 8.3.1 For monolithic ceramics, the following material char-
8.2.3 The sensitivity of the thermal properties of ceramics to acteristics should be carefully considered in terms of their
such variations requires that the composition and constituents expected and actual effect on the thermal properties. Evalua-
in advanced ceramics be sufficiently determined and docu- tion of the material characteristics may be recommended, if the
mented to avoid misinterpretation of results and to permit thermal properties are sufficiently impacted by the pertinent
adequate characterization of the test material. This character- characteristics.
ization may be simple and straightforward for monolithic 8.3.2 Porosity has a major effect on thermal conductivity/
ceramics, but may require extensive microstructural, chemical, diffusivity. From one viewpoint, porosity can be considered an
and physical analysis for complex systems such as whisker or additional, low thermal conductivity/capacity phase in the test
fiber-reinforced composites. The degree of characterization specimen in which the pore volume fraction, the porosity size
required depends on the variation in the thermal properties (mean and distribution), and its geometric distribution can all
produced by changes in composition, constituents, and micro- have variable effects on the thermal properties, especially the
structure. Spatial variations must be considered and adequately thermal transport properties. The porosity in the test specimens
evaluated, particularly for whisker- and particle-reinforced should be adequately defined and characterized with regard to
composites, in which reinforcement concentrations may vary its effect on thermal conductivity/diffusivity.
spatially through the test specimen. 8.3.3 Variations in stoichiometry, impurities, grain size, and
8.2.4 For advanced ceramic composites (whisker, chopped- grain boundary phases can have a large effect on the thermal
fiber, and continuous-fiber reinforced) and for monolithics with conductivity and thermal diffusivity for ceramics with high
oriented or textured grain growth, anisotropy effects must be intrinsic thermal conductivity (aluminum nitride, beryllia,
carefully evaluated and characterized. Directional effects are silicon carbide, and so forth). The effect of such composition
pronounced in thermal conductivity/diffusivity and thermal variations and phase distributions should be carefully consid-
expansion measurements. The character and degree of anisot- ered and evaluated (if feasible) in thermal tests of high thermal
ropy in such composites must be adequately characterized and conductivity ceramics.
understood. 8.3.4 Phase changes and devitrification of amorphous
8.2.5 In a similar manner, the exposure history of a compo- phases may occur during thermal tests, producing anomalies in
nent can also affect the thermal properties through oxidation, the various thermal properties. Test operators should be in-
phase changes, grain growth, high-temperature reactions, cor- formed of the potential for such transformations in specimens
rosion, and slow crack growth. Exposure history (time, tem- submitted for testing.
perature, and atmosphere) for test specimens has to be well- 8.3.5 Thermal expansion measurements for ceramics often
documented. show heating/cooling hysteresis when microcracking or minor
8.2.6 Exposure and thermal effects can also occur during the phase changes occur. Irreversible thermal expansion effects
thermal testing, changing the composition and microstructure. may also occur in certain materials, based on annealing, rapid
It is imperative that the test operator be aware of potential heating rates, creep, crystallization, or microcracking. Thermal
reactions, oxidation, phase changes, and other thermal events expansion tests done only on heating can be misleading, and
that could occur across the test temperature range. This can thermal expansion measurements should be done under both
occur if the test temperature exceeds the maximum processing heating and cooling conditions.

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8.3.6 Oriented or textured grain structures in monolithic 8.5.2.4 The composition and morphology (thickness, poros-
ceramics can introduce anisotropic effects in the thermal ity, and grain structure) of any surface coatings on the
properties. Such grain structures are commonly developed composite component, used for surface sealing, oxidation/
during processing. If the thermal effects of such anisotropy are corrosion protection, or wear/abrasion resistance. Surface coat-
significant, the grain structure should be characterized by ings may be considered as monolithic layers on the surface of
optical or SEM microscopy or by X-ray diffraction. the composite.
8.4 Particulate and Whisker-Reinforced Ceramic 8.5.3 The matrix in the composite must also be adequately
Composite—Material Variables: characterized in terms of composition, constituents, morphol-
8.4.1 Particulate and whisker reinforcement of advanced ogy, and grain structure. Porosity in the composite should also
ceramics adds an additional degree of complexity to the be characterized, considering volume fraction, pore size, shape
composition and microstructure of the test specimen. It is factors, and distribution of porosity.
critical that the particulate or whisker additions be adequately 8.5.4 Fiber-reinforced ceramic composites often have strong
characterized in terms of composition, phase and crystal anisotropic properties, determined by the reinforcement archi-
structure, particle/whisker morphology, and size distribution. It tecture with higher fiber volume loadings in specific directions.
is also useful to have nominal thermal properties, that is, It is essential that the geometry and orientation of the rein-
specific heat, thermal conductivity, and thermal expansion, for forcement are fully documented and correlated with the ther-
the reinforcement across the temperature range of interest. mal test results.
Those thermal property data will assist in interpreting the 8.5.5 In many thermal tests (such as thermal dilatometery,
composite thermal test results. diffusivity, and specific heat), the test specimens may have one
8.4.2 As part of the composite specimen, the particulate/ or more dimensions which are small in comparison to the
whisker reinforcement must be adequately defined in terms of weave repeat elements. Experimenters should carefully con-
the volume fraction, spatial distribution, and orientation/ sider the size of the test specimens for a specific test to ensure
anisotropy/texture. For example, reinforcements with high that an adequate number of weave repeat elements are included
thermal conductivity relative to the matrix will have markedly in the specimen. Specimens of insufficient size may not be
different effects on the composite thermal properties, depend- representative of the properties of the larger piece or may have
ing on how the reinforcements are distributed and oriented. For exaggerated end or edge effects.
example, whiskers in a laminated, planar orientation will
produce anisotropic thermal conductivity in the composite. The 9. Test Specimen Sampling and Preparation
bulk thermal conductivity will markedly change if the particu- 9.1 Test Specimen Sources—Test specimens for thermal
late packing factor is high enough to produce significant evaluation can be taken from engineering components or
particle-to-particle contact. fabricated test panels/billets. The selection of a particular
8.4.3 If there is a large difference in thermal expansion source depends on the required test specimen geometry and the
between the reinforcement and the matrix in the composite, suitability of the test component for test specimen preparation.
residual stresses or microcracks, or both, can develop during The primary objective is to select test specimens that are
processing. Such residual stresses and microcracks can pro- representative of the composition, processing, and properties of
duce anomalies in thermal expansion measurements. Microc- the final functional part.
racking can also have a direct effect on thermal conductivity/ 9.2 Specimen Sampling to Assess Variability:
diffusivity. 9.2.1 Depending on the degree of process control, variabil-
8.5 Continuous Fiber-Reinforced Ceramic Composites— ity may occur among test specimens within a batch and
Material Variables: between different batches of test specimens. The variation may
occur in the composition, microstructure, and porosity of
8.5.1 The use of continuous fiber reinforcement in ceramic
advanced ceramics. The degree of variation will depend on the
composites provides the ceramic engineer the greatest range of
homogeneity within the batch and on reproducibility between
property control and tailoring, but also introduces the highest
batches from the producer. The test operator should select/
level of complexity into the composition and microstructure of
prepare sufficient test specimens to provide a representative
advanced ceramics.
sample of the entire batch of specimens submitted for testing.
8.5.2 It is essential that the composition and architecture of In addition, batch/lot identification should be carefully noted
the fiber reinforcement in the composite be adequately char- for documentation purposes.
acterized and documented, to include the following:
9.2.2 Practice E 122 provides guidance on calculating the
8.5.2.1 Fiber composition, filament morphology (diameter number of units required for testing to obtain an estimate of
and length), and fiber volume fraction. certain precision for a given property.
8.5.2.2 Filament counts in tows, comprehensive description 9.3 Orientation and Anisotropy Effects—If the test material
of the reinforcement architecture [one-dimensional (tows), has significant anisotropy or orientation effects, it is imperative
two-dimensional (woven fabrics), and three-dimensional that test specimens be selected to adequately sample the
(weaves and braid)] to include tow count and repeat units. anisotropy in the major directions of interest. A minimum of
8.5.2.3 The composition and morphology of any interface two directions should be selected for test specimens. The
coatings on the fibers, used for process protection of the fibers orientations should be selected to produce the maximum and
or for development of crack deflection modes in the composite. minimum material properties. Each test specimen should be

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 C 1470 – 06
marked and identified so that its orientation in the original not pertinent, the following machining procedures are recom-
part/test piece can be identified. mended as a method commonly used for ceramic test speci-
9.4 Location and Identification: mens for mechanical testing.
9.4.1 Given the variability which may occur in developmen- (1) Perform all grinding or cutting with ample supply of
tal advanced ceramics and the anisotropy which may be an appropriate filtered coolant to keep the specimen and grinding
engineered characteristic of composite components, test speci- wheel constantly flooded and particles flushed. Grinding can be
men locations should be documented by drawing or photo- done in two stages, ranging from coarse to fine rates of material
graph. Test specimens should be identified so that their location removal. All cutting can be done in one stage appropriate for
can be traced on the original part. Special identification should the depth of cut.
be used for test specimens taken from plate edges or from areas (2) The stock removal rate shall not exceed 0.03 mm per
with local anomalies. pass to the last 0.06 mm of material removed. Final finishing
9.4.2 Nondestructive evaluation (NDE) methods may be of shall use diamond tools between 320 and 500 grit. No less than
value in characterizing test plates prior to specimen prepara- 0.06 mm shall be removed during the final finishing stage, and
tion, particularly for fiber-reinforced ceramic composites. The at a rate less than 0.002 mm per pass. Remove equal stock from
NDE results will assist in locating material anomalies, such as opposite faces.
excessive porosity or delaminations. (3) Grinding is followed by either annealing or lapping, as
9.5 Specimen Count and Repeat Tests—Follow the instruc- deemed appropriate for a particular material and test. For
tions of the specific test method to determine the specimen silicon based ceramics (for example, silicon carbide or silicon
count and repeat tests needed for the required precision and nitride) or oxide ceramics containing a glassy phase (for
confidence. example, aluminas with second phases) annealing at ;1200°C
9.6 Surface Effects on Thermal Property Measurements— for ;2 h is generally sufficient to heal the grinding damage
Surface finish requirements are commonly detailed in thermal introduced during specimen preparation.
test methods to provide for minimal thermal resistance at 9.7.4 Specimens may require environmental or thermal
contact surfaces or to ensure flat, smooth, and accurate surfaces conditioning, prior to testing, if there is a need to determine
for measurement. Surface finish can have a strong effect on changes in thermal properties after such environmental or
radiation absorption/emission with a direct effect on emittance thermal exposure. Any conditioning procedures should be fully
measurements and on thermal diffusivity measurements by documented with careful measurements of dimensions,
flash. Surface finish measurements may be advisable to ensure weights, and appearance before and after conditioning.
reproducibility and proper interpretation of specific thermal 9.7.5 Record dimensions and weights of all samples to the
test results. required tolerances or 61 %, whichever is more restrictive.
9.7 Test Specimen Preparation: Dimensions and weights are important in calculating specimen
densities. However, bulk density and apparent porosity should
9.7.1 Careful machining of specimens is critical in all
be calculated using Archimedes immersion (Test Method
thermal measurements, primarily for accurate measurement of
C 373) where necessary, especially for composites with sig-
critical dimensions and for accurate fit of specimens into
nificant porosity or surface roughness.
fixtures. Machining procedures should be sufficiently docu-
9.8 Post Test Inspection—In any thermal test involving
mented for reproducibility.
high-temperature exposure, post-test examination of the tested
9.7.2 Per Test Method C 372, test specimens for mechanical
specimen is of value in determining thermally induced
dilatometry should have ends that are cut/ground flat and
changes, such as melting, sintering, phase changes, oxidation,
perpendicular to the specimen axis. Dilatometer fixtures are
or corrosion. Visual inspection should be done as a minimum.
commonly designed to provide point contact with specimens
Dimensional inspection or microstructural and compositional
and to prevent sideways levering. For thermal expansion
analysis, or both, may be necessary if such thermal changes are
measurements using optical test methods, specimen ends need
suspected.
to be flat and parallel to a quite high precision to ensure
9.9 Health and Safety—Proper handling and safety proce-
stability and to define light paths.
dures should be used for all ceramic materials in monolithic or
9.7.3 There is no standard method for machining and composite forms. Refer to the Material Safety Data Sheets for
finishing ceramic specimens for thermal testing. There are the test materials for inhalation, handling, ingestion, reaction,
three general categories of machining which can be applied fire, environmental, and disposal hazards.
both to monolithic and composites ceramics
9.7.3.1 Application-Matched Machining—The machined 10. Report
surfaces of the thermal test specimen will have the same 10.1 Follow all of the normal reporting requirements of the
surface/edge preparation as that given to a service component. standard used for testing.
9.7.3.2 Customary Practices—In instances where a custom- 10.2 The accurate description of the advanced ceramic test
ary machining procedure has been developed that is completely specimens is essential for proper interpretation of the thermal
satisfactory for a class of materials (that is, it induces no test results. All ceramic test specimens should be described to
unwanted surface/subsurface damage or residual stresses), this the fullest extent possible, providing documentation (as
procedure may be used to produce the thermal specimens. applicable/available) on:
9.7.3.3 Recommended Procedure—In instances where 10.2.1 Material composition, chemistry, phase, and micro-
Application-Matched Machining and Customary Practices are structure,

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 C 1470 – 06

FIG. 4 Schematic of Hot Wire Thermal Conductivity Technique

FIG. 1 Schematic of Test Stack and Guard System for Cut Bar
Comparative Heat Flow Technique

FIG. 5 Schematic of Calorimetry Technique

FIG. 2 Schematic of Guarded Heat Flow Meter Apparatus

FIG. 6 Schematic of Drop Calorimetry Technique

10.2.5 Sampling method and identification,

10.2.6 Specimen preparation, conditioning, and geometry,
and
10.2.7 Equipment and test procedure description.
FIG. 3 Schematic of Guarded Hot Plate Apparatus
11. Test Method Comparison
11.1 Thermal Conductivity Test Methods—There are five
10.2.2 Composite composition and architecture, general types of ASTM test standards for thermal conductivity:
10.2.3 Processing and fabrication method and exposure Cut Bar Comparative Heat Flow, Guarded Heat Flow Meter,
history, Guarded-Hot-Plate, Hot Wire, and Calorimetry Method for
10.2.4 Part description, Refractories.

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TABLE 3 Thermal Conductivity—Cut Bar Comparative and Guarded Heat Flow Meter Methods
ASTM Test Method E 1225 C 408 C 518 E 1530
Measurement technique Cut Bar Comparative Cut Bar Comparative Guarded Heat Flow Meter Guarded Heat Flow Meter

Thermal conductivity range, l 0.2-200 W/(m·K) depending on 0.2-200 W/(m·K) 0.01-0.5 W/(m·K) depending 0.01-30 W/(m·K) depending on
reference materials and on instrument configuration instrument configuration and
instrument configuration and meter range meter range

Test temperature range –150 to 1000°C, depending on 40 to 150°C –150 to 300°C, depending on –150 to 300°C, depending on
fixture material and thermal flux meter limit and thermal flux meter limit and thermal
control range. control range control range.

Specimen environment air, inert/reducing gas, vacuum vacuum air air

depending on system design

Specimen size and preparation thin flat disk or rectangle—25- thin flat disk or rectangle— thick flat slab—100-300 mm in thin flat disk or rectangle
50-mm diameter and 10-40 mm 6.5-13-mm diameter with length by 10-50 mm thick,
thick depending on instrument thickness = diameter depending on instrument recommended—50-mm diameter
design configuration by 0.5-12.7 mm thick, dependent
flat and parallel surfaces to on instrument configuration.
flat and parallel surfaces to 615 min and metallized and
610 min and polished to 32 then soldered to the copper flat and parallel faces with
rms thermode references thickness 60.025 mm

Reference/standard materials two reference specimens copper reference specimens one or more calibration one or more calibration
standards required standards required

Benefits and advantages small sample size, high- small sample size suitable for low thermal Versatile, broad thermal
temperature range, direct conductivity (<0.1 W/m·K) conductivity range
measurement against reference materials
standards

Test limitations and requires one or more reference limited temperature range requires calibration with one or requires calibration with one or
requirements materials with suitable l and more reference standards of more reference standards of
stability at the test temperatures contact resistance should be similar l similar l.
minimized, especially for high l
contact resistance should be materials. see Practice C 1130 see Practice C 1130.
minimized, especially for high l
materials. contact resistance should be
minimized, especially for high l
materials.

Precision Data 67 % for 0-600°C 63 % for 0-150°C 62 % 62 %

Comments for advanced — — not suitable for high l materials —

ceramic Monoliths

Comments for advanced specimen dimensions should be 203 the dimensions of a “unit cell” or laminate thickness
ceramics composites

controlled at different temperatures to establish the desired

thermal gradient along the length of the test assembly. The test
assembly is designed (with heaters or insulation) to eliminate/
minimize radial/lateral heat losses. The temperature gradient is
measured by thermocouples at six known locations in the test
assembly: two locations in the upper reference specimen, two
locations in the test specimen, and two locations in the lower
reference specimen. Once thermal equilibrium is reached, the
heat flux in the test assembly is calculated in the two reference
specimens based on the known thermal conductivity and the
temperature gradients in the two references. Knowing the heat
FIG. 7 Schematic of Differential Scanning Calorimeter
flux from the reference specimens and the thermal gradient in
the test specimens, the thermal conductivity of the test speci-
11.1.1 Cut Bar Comparative Heat Flow Technique—A test men is calculated. (See Test Methods E 1225 and C 408.) See
specimen of measured cross section and thickness is sand- Fig. 1.
wiched between two identical reference specimens of a mate- 11.1.2 Guarded Heat Flow Meter Technique—The heat
rial with known thermal conductivity. The test assembly flow meter apparatus establishes a steady-state unidirectional
(reference specimen/test specimen/reference specimen) is heat flux through a test specimen between two parallel plates at
placed with an applied force between two heating elements constant but different temperatures. The heat flux is measured

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TABLE 4 Thermal Conductivity—Guarded Hot Plate, Hot Wire, and Calorimeter Methods
ASTM Test Method C 177 and C 1044 C 1114 C 1113 C 182, C 201, C 202, C 767
Measurement technique Guarded Hot Plate Thin Heater Hot Wire Calorimeter

Thermal conductivity range, l 0.01-2 W/(m·K) 0.01-2 W/(m·K) 0.5-15 W/(m·K) <28 W/(m·K)

Test temperature range –150 to 1000°C, depending on –150 to 1000°C, depending on 40 to 1500°C, depending on 40 to 1500°C, depending on
instrument configuration and instrument configuration and instrument configuration and instrument configuration and
thermal control range thermal control range thermal control range and furnace range
insulation range of test material

Specimen environment commonly air, but inert/reducing gas, vacuum depending on system design air

Specimen size and preparation flat slab, generally 200-600-mm flat slab, generally 200-600-mm two bricks (230 by 115 by 75 six flat bricks – 228 by 64 by 57
width and 10-150 mm thick width and 10-150 mm thick mm) with a groove for the wire mm
depending on system depending on system
configuration configuration flat and parallel to 60.3 mm

Reference/standard materials none required none required none required none required

Benefits and advantages absolute measurement of absolute measurement of absolute measurement of absolute measurement of
thermal conductivity with no thermal conductivity with no thermal conductivity with no thermal conductivity with no
reference specimens reference specimens reference specimens reference specimens

Test limitations and most suitable for low l [<5-W/ most suitable for low l [<5-W/ not applicable for electrically designed for refractory bricks
requirements (m·K)] insulators (m·K)] insulators conductive ceramics and requires large specimens,
not commonly used for
advanced ceramic

Precision data 62 % 62 % 62 % NA

Comments for advanced limited application because of large sample size — very limited application because
ceramic monoliths of large sample size

Comments for advanced — — not recommended for very limited application because
ceramics composites anisotropic materials of large sample size

thermal equilibrium. The hot-plate technique can be used in

either a two-sided or a one-sided mode. The Thin-Heater
Method is a geometrical variation of the guarded hot plate
technique. (See Test Method C 177, Practice C 1044, and Test
Method C 1114.) See Fig. 3.
11.1.4 Hot Wire Technique—In the hot-wire technique, a
resistance heated platinum wire is sandwiched between two
blocks of the test material in a temperature controlled chamber.
A constant electrical current is applied to the wire. The rate at
which the wire heats is dependent on how rapidly heat flows
from the wire into the constant temperature mass of the test
blocks. The rate of temperature increase of the wire is
accurately determined by measuring its increase in resistance
FIG. 8 Schematic of Flash Diffusivity Apparatus in the same way a platinum resistance thermocouple is used. A
Fourier equation is used to calculate the thermal conductivity
by a heat flux transducer (output voltage changes with heat based on the rate of temperature increase of the hot wire and
flow through the sensor) in the instrument, which is calibrated the power input. (See Test Method C 1113.) See Fig. 4.
with one or more reference materials of known thermal 11.1.5 Calorimetry Technique for Refractories—A refrac-
conductivity. At thermal equilibrium the measured heat flux, tory insulation specimen of known thickness is positioned in an
the temperature drop between the top and bottom faces of the electrically heated furnace with the back side of the specimen
specimen, and the specimen thickness are used to calculate the positioned against a water-cooled calorimeter (a copper plate
thermal conductivity of the test specimen. (See Test Methods with flowing water). The inner and outer face of the refractory
C 518 and E 1530.) See Fig. 2. specimen are instrumented with thermocouples. The refractory
11.1.3 Guarded-Hot-Plate Technique—Test specimens of test specimen is fixtured with insulating guard bricks to reduce
fixed thickness are placed between a main heat source operat- lateral heat flow. With the furnace at the desired temperature
ing at a known power level and an auxiliary heater operating at and the calorimeter showing a steady-state heat flow, the heat
a fixed temperature. Additional guard heaters are positioned to flux flowing through the test specimen is determined from the
minimize lateral heat flow. Thermocouples measure the tem- measured heat flow and the specimen cross-sectional area. The
perature differential across the test specimen thickness at thermal conductivity is then calculated from the heat flux and

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TABLE 5 Specific Heat—Scanning Differential and Drop Calorimetry Methods
ASTM Test Method E 1269 D 2766 C 351
Measurement technique Scanning Differential Calorimetry Drop Calorimetry Drop Calorimetry

Specific heat capacity, Cp, Range no limit no limit no limit

Test temperature range 0 to 1000°C dependent on furnace 0 to 250°C depending on the furnace 0 to 150°C depending on the boiling
range and specimen holder capability and specimen capsule limits point of the calorimeter fluid and the
temperature limit furnace capability

Specimen environment air, inert/reducing gas, vacuum air air

depending on system design

Specimen size and preparation 1-500 mg, dependent on specimen dependent on instrument configuration nominal—50 by 25 by 3 mm
holder volume and specimen capsule size
dependent on instrument configuration
samples must be dry, especially for and test conditions
powdered samples

Reference/standard materials reference specimen recommended one or more calibration standards one or more calibration standards
required, copper or aluminum required, copper or aluminum

Benefits and advantages rapid testing with data across a broad convenient sample size for convenient sample size for
temperature range; easily identifies inhomogeneous materials inhomogeneous materials
thermal transformations

Test limitations and requirements small samples have to be limited temperature range; determines limited temperature range; determines
homogeneous and linear mean value for Cp and requires linear mean value for Cp and requires
representative multiple tests to determine Cp at multiple tests to determine Cp at
different temperatures different temperatures

difficult to identify thermal difficult to identify thermal

transformations transformations

Precision data 62 % NA 610 %

Comments for advanced ceramic monitor samples for phase transformations and glass transitions
monoliths

Comments for advanced ceramics small samples have to be homogeneous

composites and representative

give comparative information on the different ASTM test

methods for thermal conductivity.
11.2 Specific Heat Capacity Test Methods—Specific heat
capacity is measured in two ways in accordance with ASTM
methods: drop calorimetry and scanning differential calorim-
etry.
11.2.1 Drop Calorimetry—A test specimen is heated to a
specified temperature in a furnace and then rapidly inserted
into an adiabatic calorimeter at a known temperature. When
thermal equilibrium is reached between the test specimen and
the calorimeter, the increase in thermal energy in the calorim-
eter is measured based on the temperature increase and the
specific heat capacity of the calorimeter. The specific heat
FIG. 9 Schematic of Thermodilatometry Method capacity of the sample is then calculated by dividing the
measured increase in thermal energy of the calorimeter by the
specimen temperature difference (initial specimen temperature
the temperature gradient across the specimen thickness. (See – final specimen temperature) and the mass of the test
Test Methods C 182, C 201, C 202, and C 767.) See Fig. 5. specimen. (See Test Methods D 2766 and C 351.) See Fig. 6.
NOTE 1—The calorimetry technique has been superceded by simpler, 11.2.2 Differential Scanning Calorimetry—The test speci-
less complex conductivity methods and is not commonly used for men is heated at a controlled rate in a controlled atmosphere
advanced ceramics, because of the large sample size and the mass and the through the temperature regime of interest. The heat flow into
cost of the test equipment. the test specimen is measured with a heat flux transducer and
11.1.6 General requirements and guidelines for determining compared to the heat flow into a reference material or blank run
the thermal transmission properties based upon heat flux concurrently. The difference in heat flow is continually moni-
measurements are given in Practice C 1045. Tables 3 and 4 tored and recorded as the test specimen is heated. The

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TABLE 6 Thermal Diffusivity by the Flash/Thermal Pulse Method
ASTM Test Method E 1461 C 714
Measurement technique Flash Method Flash/Thermal Pulse Method

Thermal diffusivity range, m2/s 1 3 10-7 – 1 3 10-3 m2/s 4 3 10-8 – 2 3 10-6 m2/s

Test temperature range –200 to 2500°C, depending on test chamber 20 to 500°C

capability

Specimen environment air, inert/reducing gas, vacuum depending on system air, inert or vacuum, depending on test chamber
design capability

Specimen size and preparation thin circular disk, typically 6-18 mm in diameter with thin circular disk, typically 6-12 mm in diameter with a
a thickness of 1.5-4 mm, depending on thermal thickness of 2-4 mm,
properties of specimen
thickness must be uniform to 60.01 mm
thickness must be uniform to 0.5 %

Reference/standard materials reference standards available, but not required for operation

Benefits and advantages small sample size and rapid testing across a range of temperatures

Test limitations and requirements small samples have to be representative.

Accurate thickness measurements are critical; surface finish may affect the absorption of the thermal radiation
on the incident face.

Calculation of thermal conductivity from thermal diffusivity requires specific heat and density at all the
experimental temperatures.

Translucency to laser radiation in the ceramic material will require a coating on one or both specimen surfaces
with a calculation and adjustment for the effects of the coating on radiation absorption and thermal diffusivity.

Precision data 63 % 63 %

Comments for advanced ceramics monoliths Translucency to laser radiation in the ceramic material will require a coating on one or both specimen surfaces
with a calculation and adjustment for the effects of the coating on radiation absorption and thermal diffusivity.

Comments for advanced ceramics composites Anisotropy effects must be carefully considered and analyzed to avoid misinterpretation of results.

Surface skin effects (density and surface texture) may complicate the measurements.

11.3.1 Flash Diffusivity—Thermal diffusivity is experimen-

tally determined by measuring the temperature time response
of a test specimen to a thermal event. The current method of
choice is flash diffusivity, in which one side of a specimen of
known thickness and temperature is subjected to a high-
intensity short-duration thermal pulse. (The thermal pulse is
introduced by a laser or flash lamps). The energy of the pulse
is absorbed on the front surface of the specimen and the
resulting rear face temperature rise is measured by a direct
contact thermocouple or a noncontact pyrometer. The ambient
temperature of the specimen is controlled by a furnace or
crysostat.
11.3.2 Thermal diffusivity is calculated from the specimen
thickness and the time required for the rear face temperature to
reach a specified percentage of its maximum value. (See Test
Methods C 714 and E 1461.) See Fig. 8.
11.3.3 Table 6 gives comparative information on the differ-
FIG. 10 Schematic of Reflectance and Emittance Methods ent ASTM test methods for thermal diffusivity.
11.4 Thermal Expansion Test Methods:
measured difference in heat flow across the temperature range 11.4.1 Thermal expansion is commonly measured by ther-
of interest is used to calculate the specific heat capacity of the modilatometry, a technique in which a specific, precisely
test specimen. (See Test Method E 1269.) See Fig. 7. measured dimension of a test specimen under negligible
11.2.3 Table 5 gives comparative information on the differ- applied force is measured as a function of temperature while
ent ASTM test methods for specific heat capacity. the test specimen is subjected to a controlled-temperature
11.3 Thermal Diffusivity Test Methods: program in a specified atmosphere. The measurement of the

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TABLE 7 Thermal Expansion by Thermodilatometry (Mechanical and Interferometry)
ASTM Test Method E 228 and C 372 E 289 and C 1300 E 831
Measurement technique Dilatometer Interferometry Dilatometer - Thermomechanical
Analyzer

Mean coefficient of thermal expansion 0.1 to 100 10–6/K depending on 0.05 to 5 10–6/K depending on 5 to 100 10–6/K depending on instrument
range, aL instrument sensitivity, specimen instrument sensitivity and specimen sensitivity and specimen dimensions
dimensions, and test temperature dimensions
range

Test temperature range –180 to 900°C for silica fixture; up to –150 to 1000°C depending on fixture –120 to 600°C depending on fixture
2500°C for other fixture materials and materials and thermal chamber range materials and thermal chamber range.
depending on thermal chamber range

Specimen environment air, inert/reducing gas, vacuum vacuum or low-pressure inert to avoid air, inert/reducing gas, vacuum
depending on system design optical drift depending on system design

Specimen size and preparation 2-50 mm long cylinder or rod de- E 289—5-20-mm long cylinder or rod 2-10-mm long cylinder or rod depending
pending on instrument sensitivity, with 5-12-mm diameter with rounded on instrument sensitivity and specimen
furnace uniformity, and specimen ends. thermal expansion
thermal expansion.
C 1300—cones at least 6 mm high with maximum diameter dependent on fixture
maximum diameter dependent on a 3-mm base. size
fixture size
ends flat and parallel to 625 µm
ends should have surface finish of 10
rms

length measured to an accuracy of

60.002 %

Reference/standard materials Calibration/reference standard required Calibration/reference standard required Calibration/reference standard required

Benefits and advantages small sample size and direct extra precision for specimens with very smaller sample size than Test Method
measurement low thermal expansions. E 228

Test limitations limited sensitivity for small specimens not suitable for large specimens or limited high-temperature range; limited to
with aL<2 10–6/K) materials with larger aL(>5 10–6/K) specimens with aL greater than 5 ppm/K

Specimens ends need to be precisely

machined and flat.

Precision 61 % NA 62 % for aL>20 10–6/K

615 % for aL<5 10–6/K

Comments for advanced ceramic monitor samples for microcracking hysteresis, sintering, creep, and phase transformations.
monoliths

Comments for advanced ceramics anisotropy effects must be carefully considered and analyzed to avoid misinterpretation of results.
composites

dimensional change can be done by direct mechanical mea-

surement or by optical measurement, using interferometers.
See Fig. 9.
11.4.2 In mechanical measurement dilatometers, the speci-
men is positioned in a fixture with one end in contact with a
rigid, spring-loaded push rod. The fixture and the push rod are
made of materials with high-temperature stability and known
thermal expansion. The opposite end of the push rod is fixtured
into the position transducer (digital or linear variable differen-
tial transformer) which converts the linear motion of the push
rod into a voltage signal. As the specimen in the fixture is
heated in a controlled manner, the change in dimension of the
sample is translated to the push rod and measured by the
FIG. 11 Schematic of Spectrophotometer Emittance Method

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 C 1470 – 06
TABLE 8 Thermal Emittance/Emissivity
ASTM Test Method E 408 E 423
Measurement technique Test Method A—Reflected radiation measured by spectrophotometer with high-temperature furnace and
infrared detector and compared to a standard integral blackbody radiator

Test Method B—Emitted radiation measured by

infrared detector and compared to a standard

Emittance/emissivity range 0.05-1 0.05-1

Test temperature range ambient temperature 1000 to 1800K depending on furnace capabilities

Specimen environment ambient atmosphere; vacuum or inert atmosphere inert and air atmospheres, vacuum, depending on
with special detector head and fittings to an sample chamber
atmosphere chamber

Specimen size and preparation minimum size depends on the “spot size” of the hollow cylinder 25 mm high and 25 mm in diameter
optical system. No sample preparation required. with wall thickness sufficient to be opaque

Reference/standard materials required for both reflection and emission methods Blackbody standard is part of the test system.

Benefits and advantages rapid testing; no special sample preparation full-range capabilities across temperature and
wavelength spectrum

Test limitations limited temperature capability complex furnace and measurement equipment

Precision 61 % 61 %

Comments for advanced ceramic monoliths Surface texture may have a significant effect on Surface texture may have a significant effect on
emittance. emittance.
Cylindrical test specimen is difficult to fabricate.

Comments for advanced ceramics composites same as monoliths same as monoliths

transducer as a function of time/temperature. A thermocouple 11.5 Emittance/Emissivity Test Methods:

is positioned close to the specimen to measure the specimen 11.5.1 There are two ASTM test methods used in the
temperature. measurement of emittance of ceramics, E 408 and E 423. Both
11.4.3 Single-rod dilatometers require calibration against a test methods measure the normal emittance, not the hemi-
standard specimen to account for the thermal expansion of the spherical emittance.
fixture. Dual-rod extensometers have two test positions; one 11.5.2 Test Methods E 408 describes two commercial sys-
position contains a known reference sample which acts as a
tems for measuring radiant energy. Test Method A measures
direct standard for comparison to the specimen in the second
radiant energy reflected by the specimen from a radiant source
position. Dilatometers can be designed with controlled atmo-
in the test equipment. Test Method B measures radiant energy
sphere test chambers to operate under vacuum or inert gas
emitted by the specimen. The two systems are suitable for
atmospheres. (See Test Methods E 228, E 831, and C 372.)
specimens at ambient temperatures and operate in the infrared
11.4.4 With interferometric techniques, thermal expansion
wavelength region of 4 to 50 µm, depending on the specific
is measured by the use of laser or monochromatic light and a
capabilities of the infrared detectors. Both systems require
dual mirror system in which the specimen is positioned. The
calibration against standards of known reflectance and emit-
mirror system is designed so that fringe patterns are produced
tance. See Fig. 10
on a sensor by constructive interference of the light. Changes
in the length of the specimen shorten or lengthen the light path 11.5.3 Test Method E 423 describes a test method for
and shift the fringe pattern. Fringe shifts are produced by measuring the emittance of ceramic specimens in a heated
sample dimension changes on the order of the wave length of furnace across a range of temperatures with direct comparison
light (200 to 400 nm), depending on the specific wavelength of to a blackbody reference at the same temperature. Special
the light used. The specimen-mirror system is placed on a efforts are made to maintain the ceramic test specimen and the
temperature-controlled furnace for high-temperature measure- blackbody reference at the identical controlled and uniform
ments. It is recommended that tests be done under vacuum or temperature. Radiant flux is measured with a spectrophotom-
low-pressure helium to reduce atmospheric distortion along the eter across the desired spectral range from 1 to 35 µm). See Fig.
light path. (See Test Methods C 1300 and E 289.) 11.
11.4.5 Table 7 gives comparative information on the differ- 11.5.4 Table 8 gives comparative information on the differ-
ent ASTM test methods for thermal expansion ent ASTM test methods for thermal emittance.

15
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 C 1470 – 06
12. Keywords
12.1 advanced ceramic; ceramic composite; emissivity;
emittance; specific heat capacity; thermal conductivity; thermal
diffusivity; thermal expansion; thermal properties

Bibliography

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(3) M. McLean, Physical and Elastic Characterization— hocken, PA, 1985
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Industrial Applications, V. 7, Netzsch-Geratebau Gmbh, 1997 many, 1987

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