Thermal Conductivity of Plastics by Means of A Transient Line-Source Technique

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5930 − 17

Standard Test Method for


Thermal Conductivity of Plastics by Means of a Transient
Line-Source Technique1
This standard is issued under the fixed designation D5930; 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 (s) indicates an editorial change since the last revision or reapproval.

1. Scope D883 Terminology Relating to Plastics


1.1 This test method covers the determination of the D2717 Test Method for Thermal Conductivity of Liquids
thermal conductivity of plastics over a temperature range from E177 Practice for Use of the Terms Precision and Bias in
–40 to 400°C. It is possible to measure the thermal ASTM Test Methods
conductivity of filled and unfilled thermoplastics, thermosets, E1225 Test Method for Thermal Conductivity of Solids
and rubbers in the range from 0.08 to 2.0 W/m.K. Using the Guarded-Comparative-Longitudinal Heat Flow
1.2 The values stated in SI units shall be regarded as Technique
standard.
3. Terminology
1.3 This standard does not purport to address the safety
concerns, if any, associated with its use. It is the responsibility 3.1 Definitions—Terminology used in this standard is in
of the user of this standard to establish proper safety and accordance with Terminology D883.
health practices and determine the applicability of regulatory 3.2 Definitions of Terms Specific to This Standard:
limitations prior to use. 3.2.1 temperature transient, n—the temperature rise associ-
NOTE 1—There is no known ISO equivalent to this test method. ated with the perturbation of a system, initially at a uniform
1.4 This international standard was developed in accor- temperature. The system does not attain thermal equilibrium
dance with internationally recognized principles on standard- during the transient.
ization established in the Decision on Principles for the 3.2.2 thermal conductivity, n—the time rate of steady heat
Development of International Standards, Guides and Recom- flow/unit area through unit thickness of a homogeneous mate-
mendations issued by the World Trade Organization rial in a direction perpendicular to the surface induced by a
Technical Barriers to Trade (TBT) Committee. unit temperature difference.
3.2.2.1 Discussion—Where other modes of heat transfer are
2. Referenced Documents present in addition to conduction, such as convection and
2.1 ASTM Standards:2 radiation, this property often is referred to as the apparent
C177 Test Method for Steady-State Heat Flux Measure- thermal conductivity, λapp.
ments and Thermal Transmission Properties by Means of 3.2.2.2 Discussion—Thermal conductivity must be associ-
the Guarded-Hot-Plate Apparatus ated with the conditions under which it is measured, such as
C518 Test Method for Steady-State Thermal Transmission temperature and pressure, as well as the compositional varia-
Properties by Means of the Heat Flow Meter Apparatus tion of the material. It is possible that thermal conductivity
C1113 Test Method for Thermal Conductivity of Refracto- will vary with direction and orientation of the specimen since
ries by Hot Wire (Platinum Resistance Thermometer some materials are not isotropic with respect to thermal
Technique) conductivity. In the case of thermoset polymers, it is possible
D618 Practice for Conditioning Plastics for Testing that thermal conductivity will vary with the extent of cure.
3.2.3 thermal diffusivity—a heat-transport property given
1
by the thermal conductivity divided by the thermal mass,
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties. which is a product of the density and the heat capacity.
Current edition approved Aug. 1, 2017. Published August 2017. Originally 3.3 Symbols:
approved in 1997. Last previous edition approved in 2016 as D5930 - 16. DOI:
10.1520/D5930-17. 3.3.1 C—Probe constant.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 3.3.2 λ—Thermal conductivity, W/m.K.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 3.3.3 Q—Heat output per unit length, W/m.
the ASTM website.
3.3.4 T2—The temperature (K) recorded at time t2.

*A Summary of Changes section appears at the end of this standard

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D5930 − 17
this standard.
3.3.5 T1—The temperature (K) recorded at time t1.
3.4 Subscript:
3.4.1 av—average.
3.4.2 app—apparent.
3.4.3 ref—reference.

4. Summary of Test Method


4.1 Line-Source Technique—This is a transient method for
determining thermal conductivity (1, 2).3 A line source of heat
is located at the center of the specimen being tested. The
apparatus is at a constant initial temperature. During the
course of the measurement, a known amount of heat produced
by the line-source results in a heat wave propagating radially
into the specimen. The rate of heat propagation is related to
the thermal diffusivity of the polymer. The temperature rise of
the line- source varies linearly with the logarithm of time
(3). It is possible to use this relationship to directly calculate
the thermal conductivity of the sample. There are a number of
ways to achieve the line source of heat. In this test method, it
is in the form of a probe as described in 7.2.

5. Significance and Use


5.1 The relative simplicity of the test method makes it
applicable for a wide range of materials (4, 5). The technique
is capable of fast measurements, making it possible to take
data before the materials suffer thermal degradation.
Alternatively, it is possible to study the effect of
compositional changes such as chemical reaction or aging (6).
Short measurement times permit generation of large amounts
of data with little effort. The line-source probe and the
accompanying test specimen are small in size, making it
possible to subject the sample to a wide range of test
conditions. Because this test method does not contain a
numerical precision and bias statement, it shall not be used as
a referee test method in case of dispute.

6. Interferences
6.1 The line-source method produces results of highest
precision with materials where intimate contact with the probe
has been established, thereby eliminating effects of thermal
contact resistance. These materials include viscous fluids and
soft solids.
6.1.1 Thermal-Contact Resistance—In the solid state, it is
possible that a contact resistance is developed due to the
interface between the specimen and the measuring device.
Conventional methods attempt to account for this by introduc-
ing a conductive paste between the specimen and the sensor.
This reduces, but some effect of contact resistance is still
possible. In the line-source method, contact resistance mani-
fests itself as a nonlinearity in the initial portion of the
transient (see Fig. 1). The technique has a method to account
for this phenomenon. By extending the time of the
measurement, it is possible to progress beyond the region of
thermal-contact resistance, achieving a state where the contact
resistance does not contribute to the measured transient (7).
This state typically

3
The boldface numbers in parentheses refer to the list of references at the end of
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D5930 − 17
6.2 Measurements in viscid fluids are subject to the devel-
opment of convection currents, which have been known to
affect the measurement. Because of the transient nature of the
measurement, these effects are not as pronounced. They
cannot be eliminated, however.
6.3 Although the technique is not limited by temperature, at
measurements above 500°C, a significant amount of heat
transfer occurs due to radiation so that it is possible to measure
only a λapp.
7. Apparatus
7.1 The apparatus consists of a line-source probe imbedded
in a specimen contained in a constant-temperature environ-
ment. During the measurement, the line-source probe produces
a precise amount of heat. The resulting temperature transient
is recorded, preferably, on a computer data-acquisition system,
FIG. 1 Line-Source Transient as specified in 7.4. This transient is analyzed to obtain the
thermal conductivity.
7.2 Line-Source Probe—The line-source probe contains a
heater that runs the length of the probe (3). The length-to-
diameter ratio of the probe must be greater than 20. The
resistance of the line-source temperature rises are
heater must be known to between 2 and 10°C over the
within duration of the measurement.
60.1 %. The probe also The frequency of data
contains a temperature acquisition must be at least
sensor to measure the once every second.
temperature transient. A 7.5 Specimen
typical sensor for the line- Environment—A constant-
source probe is a high- temperature envi- ronment
sensitivity J-type must be maintained through
thermocouple used because the duration of the test so as
of its large Seebeck to provide a temperature
coefficient. The housing stability in the specimen of
sheath of the probe must be within 60.1°C. Failure to
robust enough to ensure that
attain this criterion will on
the probe does not bend or
occasions compromise the
deform under the adverse
linearity of the transient,
conditions it is subject to
is achieved after about 10 to 20 s in the measurement. The thereby affecting the test
during measurements.
larger the contact resistance, the greater is this time. It is, result. The environment shall
therefore, important to make a sufficiently long measurement 7.3 Heater Power be free from excessive
to exclude the portion of the transient that shows the effect of Source—The power input vibration.
the contact resistance. The duration of measurement, to the line- source heater 7.5.1 Ambient—For
however, must not be too long, because the possibility of the comes from a DC voltage measurements close to
heat wave striking a sample boundary exists, thereby source. The precision of the ambient temperature, use of
violating the theo- retical requirements of the measurement. voltage source must be a stirred water bath is one
6.1.2 Shrinkage Upon Solidification—Plastics tend to within 60.25 % over the method to be used to maintain
shrink significantly upon solidification. This shrinkage is entire duration of the test. the test temperature.
especially so for the semi-crystalline materials, which 7.4 Recording Device— Alternatively, placing the
experience a signifi- cant change in specific volume upon The temperature transient specimen, adequately
crystallization. The probability exists that this crystallization from the line-source probe is shielded to protect it from
will result in large gaps being developed between the recorded for the duration of convection, is a possible
specimen and the sensing device. To account for shrinkage, the test. A temperature alternative.
and possibly permit the line-source probe to move downward measurement device with a 7.5.2 Cryogenic
to take up the slack a simple compression scheme as resolution of 0.1°C is Temperatures—Placing a
described in 9.5 has been used successfully. Steps also must required. Data are acquired specimen ad- equately
be taken to minimize specimen volume so as to reduce the for 30 to 120 s depending on shielded from convection in
extent of shrinkage. the type of material. Typical a controlled cryogenic bath
or chamber is acceptable.
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D5930 − 17
7.5.3 Elevated The specimen-preparation to drill a pilot hole that is contain the specimen. For
smaller than the probe thermally unstable materials,
diameter to aid in insertion. follow material
manufacturers’
9.4 Thermoplastics in the
recommendations on
Melt—Preheat the sample
temperature exposure limits.
cell to the lowest melt
processing temperature of 9.5 Solid Thermoplastics
the thermoplastic. Loading —Load the sample in the
specimens at a low same manner as in 9.4. The
temperature is desirable to following precautionary
ensure an air-free specimen. steps are needed to account
Pour a charge of the for shrinkage of the
specimen, typically in pellet specimen as it solidifies. The
or powder form, into the cell probe shall be fitted with a
and compress into a dynamic sealing system
homogeneous mass. Several permitting it to move with
charges, tamped well, are the shrinking specimen.
often needed to fill the Static loads placed on the
sample cell. When the probe to help maintain
specimen is well molten, contact as the plastic shrinks
insert the probe so as to be are acceptable and
near the axial center of the recommended. These loads
Temperatures—At method depends on the type specimen. Sealing systems optimally will apply a
temperatures above of material being tested. If are sometimes employed to pressure of 1 to 7 MPa on
ambient, a special heated the material is believed to the specimen.
cell is required. This be anisotropic, at least three
consists of a vertical specimens must be tested. 9.6 Thermosets and such that a calibration is
cylindrical heated chamber, Specimens must be longer Rubber—Preheat the sample necessary to account for such
fitted with a removable plug than the line-source probe cell to a loading temperature, effects as the thermal mass
at the bottom. The specimen and large enough in radius above the glass transition, of the probe and the fact that
is loaded from the top and is to have at least 4 mm of where the specimen is fluid the precise length of the line-
discharged through the material surrounding the enough to be molded but will source cannot be determined.
bottom, once the test is probe, so that the expanding not undergo significant A probe constant must be
complete (see Fig. 2). heat wave will not strike a reaction (6). If the sample obtained by calibrating the
boundary during the cell is to be reused, wipe the probe against a material of
8. Conditioning measurement. walls of the cell with a thin known thermal conductivity.
layer of a release agent such The constant depends on the
8.1 Many thermoplastic 9.2 Viscous Liquids— as silicone oil to prevent the probe characteristics and has
materials must be dried These include pastes and cured specimen from no significant temperature
because moisture has been semisolids. Pour or extrude bonding to the cell. Charge sensi- tivity. The ideal value
shown to affect the the specimen into a test tube or pour the uncured of the probe constant is 1.0.
properties. Moisture causes or similar cylindrical specimen in the same Typical values range from
molten polymer samples to container. The container manner as in 9.4. For best 0.8 to 0.9.
foam, which will affect the must be filled with suffi- results, do not coat the probe 10.2 Reference Material—
measured thermal cient quantity of fluid such with release agents since this An ideal reference material is
conductivity. Conditioning that the probe is immersed might affect the test results. a well-characterized, viscous
is generally not a completely.
10. Calibration liquid. Such a system will not
requirement of this test; if 9.3 Soft Solids—Insert be subject to thermal contact
conditioning is necessary, the line-source probe 10.1 The actual probe and
resistance effects. Because of
see the applicable material directly into the specimen, sample cell differ in many
the high viscosity, convection
specification or Practice taking care to see that it ways from the theoretical
effects are not present. A
D618. does not bend during situation, which assumes an
polydim- ethylsiloxane fluid4
insertion. A specimen of any infinitely long probe in an
is in common use as a
9. Preparation of Test size or shape as long as it is infinite specimen. Judicious
reference material. This
Specimen larger than the minimum design of the probe and
material has a thermal
specified in 9.1 is sample cell will often
9.1 The test specimen conductivity of 0.16 W/m.K
acceptable. In the case minimize some of the non-
prepared from plastic at room temperature (8, 9).
where the specimen cannot idealities. Practical
pellets, liquids, foams, or 10.3 Probe Calibration—
be penetrated without being limitations in probe
soft solids is acceptable. In the equations in 12.2, the
destroyed, it is permissible construction, however, are
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D5930 − 17
λ5
probe constant is set to 1.0. fume removal. The probe
The line-source probe is input to the line-source tempera- ture must be
heater is dependent on the 4π
immersed in the reference monitored so that it does not Slop
material of known thermal character- istics of the exceed permissible limits.
conductivity λref, which is at material being tested. A Remove all adhering
e
the reference temperature. high-thermal-diffusivity materials. Do not scratch, where:
At least five measurements material dissipates heat at a mar, or bend the probe
must be performed as faster rate so that a larger during cleaning. T
outlined in Section 11. The amount of heat is needed.
Conversely, low-thermal- 11.8 Inspect the 2

resulting values of thermal specimen for voids. If 2


conductivity are calculated diffusivity materials, such
as foams and insulations specimen has been
based on 12.2, for each case subjected to conditions T
and the results averaged require a small amount of 1
heat input. where it might have Slope 5
yielding λav. undergone degradation, 2 ln~t /t
11.4 Allow the system to K
C note and report such
5 attain temperature stability, evidence. 12.3 Test Conditions—
λref as defined in the criteria in The temperature at which
/λav 7.5. Supply the heat input to 12. Calculation the thermal conductivity is
the line-source. 12.1 Plot the temperature to be reported is the
It is recommended that Simultaneously, record the rise against log time. Obtain equilibrium temperature of
calibration be verified at temperature and time for the slope of the linear the specimen prior to the
least once a month. the duration of the portion of the curve. start of the measurement,
measurement. Neglect initial reported to the nearest whole
11. Procedure nonlinearities, which occur number. If the time of the
11.5 It is acceptable to
11.1 Before beginning make multiple because of the heat wave measurement is to be
experiments, examine the measurements if desired at propa- gating through the recorded, report the time at
line-source probe. The probe these same conditions, walls of the probe and also the start of the measurement.
must be straight and its provided that the system is due to contact resistance, Report any other conditions
surface free of residues, oil, permitted to stabilize prior where the phenomenon that are unique to the
or water. Nonresidue to each measurement. exists (7). measure- ment.
solvents and copper gauze 12.2 Perform the
11.6 Change the sample 13. Report
are recommended for calculations using the
environment conditions for 13.1 Report the following
cleaning. The sample cell following equation:
the next measurement. information:
must be clean and free of
Continue the process until C 13.1.1 Description of the
residues. Q
the desired range of test 1 material and test
11.2 Prepare the conditions have been specimen.
specimen and insert the covered. Where a change of
probe as applicable for the physical state occurs over 13.1.2 Description of the
TABLE 1 Repeatability Data for
appropriate sample type, as the range of conditions apparatus. Thermal
described in Section 9. tested, acquire at least two 13.1.3 Reference material Conductivity
Ensure that the probe is measurements in each state. used for calibration (W/m·K) of
secure and the system is not including its thermal Polypropylene
11.7 Clean up the system and
subject to any form of conductivity value.
by extracting the probe Polycarbonate
vibration or temperature under the same conditions Test
fluctuation. M Tem r Average S
as those under which it was 13.1.4 Details of the a pera A

11.3 In general, low loaded. The only exception probe, including t


e
ture,
°C
power
ength, outputs
and power are output.
desirable to this rule is in the case of probe constant,
Polypropylene 200
r
0.164 i 0.0019
rB
0.0053
to 13.1.5prevent excessive atthermosets
Thermal conductivity where
the relevant test the
conditions, l Polycarbonate 280
a
0.263 l 0.0058 0.0162
perturbation of the system. specimen has solidified
The amount of power around the probe. Cutting such as temperature or time. a single laboratory. The
rubbers away from the materials used were unfilled
4
Polydimethylsiloxane, probe using a sharp razor 13.2 Report if the
trimethylsiloxyteminated, 60,000 CS, specimen has undergone any polypropyl- ene and
from Huls America, Bristol, PA
has been found to be polycarbonate resins.
successful. It is possible to physical or chemical change
19007.
during testing. Measurements were
remove rigid thermosets by performed by a single
thermal decomposition technician on a single day.
using a Bunsen burner. This 14. Precision and Bias
Each test result is an
procedure must be 14.1 Table 1 is based on a individual determination.
performed with adequate repeatability study involving Five measurements were
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D5930 − 17
obtained for each material. A
Sr = within-laboratory standard deviation mentioned in this standard. Users of this
of the average. standard are expressly advised that
14.2 Attempts to develop B
r = within-laboratory repeatability limit determination of the validity of any such
= 2.8 × Sr. patent rights, and the risk of infringement of
a full precision and bias such rights, are entirely their own
statement for this test responsibility.
method have not been shall not be used as a
successful. Because this test referee test method in case This standard is subject to revision at any
time by the responsible technical committee
method does not contain of dispute. It is requested and must be reviewed every five years and
round-robin based precision that anyone wishing to if not revised, either reapproved or
data, it withdrawn. Your comments are invited either
participate in the develop- for revision of this standard or for additional
ment of precision and bias standards and should be addressed to
ASTM International Headquarters. Your
data should contact the comments will receive careful consideration
Chairman, Subcommittee at a meeting of the responsible technical
D20.30 (Section committee, which you may attend. If you
feel that your comments have not received a
D20.30.07), ASTM, 100 fair hearing you should make your views
Barr Harbor Drive, PO Box known to the ASTM Committee on
C700, West Conshohocken, Standards, at the address shown below.
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This standard is copyrighted by ASTM
14.3 There are no International, 100 Barr Harbor Drive, PO Box
recognized standards on C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or
which to base an estimate of multiple copies) of this standard may be
bias for this test method. obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-
15. Keywords 832-9555 (fax), or service@astm.org (e-
mail); or through the ASTM website
15.1 line-source probe; (www.astm.org). Permission rights to
line-source technique; photocopy the standard may also be
secured from the Copyright Clearance
plastics; rub- ber; thermal Center, 222 Rosewood Drive, Danvers, MA
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thermoplastics; thermosets http://www.copyright.com/

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(1) Hooper, F. C., and Lepper, F.


Chem. Eng. Prog. Sym.
R.,Trans. Am. Soc. Heat.
Series, Vol 56, No. 30, 1960,
Vent. Engrs., Vol 56, 1950,
p. 261.
p. 309.
(2) Eustachio, D., and (6) Lobo, H., SPE Technical
Papers, Vol XXXVIII, 1991,
Schreiner, R. E., Trans.
p. 1281.
Am. Soc. Heat. Vent.
Engrs., Vol 58, 1952, p. 331. (7) Tye, R. P., ed., “Thermal
(3) Lobo, H., and Cohen, C., Conductivity,” Vol 2, p. 377.
Polym. Eng. Sci., Vol 30, (8) Bates, O. K., Ind. Eng.
1990, p. 65. Chem., Vol 41, No. 9 , 1949, p.
(4) Haugh, C. H., and Sweat, V. 1966.
E., Trans. ASAE, Vol 56, (9) “Silicon Compounds
1974. Register and Review,”
(5) McTaggart, R. B., and Petrarch Systems, Inc.,
Underwood, W. M., “Heat 1984, p. 190.
Transfer (Storrs),”

ASTM International takes no position


respecting the validity of any patent rights
asserted in connection with any item
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