Thermal Conductivity of Plastics by Means of A Transient Line-Source Technique
Thermal Conductivity of Plastics by Means of A Transient Line-Source Technique
Thermal Conductivity of Plastics by Means of A Transient Line-Source Technique
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5930 − 17
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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.
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
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