An American National Standard

Designation: D 6744 – 01

Standard Test Method for

Determination of the Thermal Conductivity of Anode
Carbons by the Guarded Heat Flow Meter Technique1
This standard is issued under the fixed designation D 6744; 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 3.1.1 average temperature—the average temperature of a

1.1 This test method covers a steady-state technique for the surface is the area-weighted mean temperature of that surface.
determination of the thermal conductivity of carbon materials 3.1.2 heat flux transducer (HFT)—a device that produces an
in thicknesses of less than 25 mm. The test method is useful for electrical output that is a function of the heat flux, in a
homogeneous materials having a thermal conductivity in the predefined and reproducible manner.
approximate range 1< l < 30 W/(m·K), (thermal resistance in 3.1.3 thermal conductance (C)—the time rate of heat flux
the range from 10 to 400 3 10−4 m2 ·K/W) over the approxi- through a unit area of a body induced by unit temperature
mate temperature range from 150 to 600 K. It can be used difference between the body surfaces.
outside these ranges with reduced accuracy for thicker speci- 3.1.4 thermal conductivity (l), of a solid material—the time
mens and for thermal conductivity values up to 60 W/(m·K). rate of heat flow, under steady conditions, through unit area,
per unit temperature gradient in the direction perpendicular to
NOTE 1—It is not recommended to test graphite cathode materials using the area.
this test method. Graphites usually have a very low thermal resistance, and
3.1.5 thermal resistance (R)—the reciprocal of thermal
the interfaces between the sample to be tested and the instrument become
more significant than the sample itself. conductance.
3.2 Symbols:
1.2 This test method is similar in concept to Test Methods
E 1530 and C 518. Significant attention has been paid to ensure
that the thermal resistance of contacting surfaces is minimized l = thermal conductivity, W/(m·K), Btu·in/(h·ft2·°F)
and reproducible. C = thermal conductance, W/(m2·K), Btu/(h·ft2·°F)
1.3 The values stated in SI units are regarded as standard. R = thermal resistance, m2·K/W, h·ft2·°F/Btu
1.4 This standard does not purport to address all of the Dx = specimen thickness, mm, in
safety concerns, if any, associated with its use. It is the A = specimen cross sectional area, m2, ft2
responsibility of the user of this standard to establish appro- Q = heat flow, W, Btu/h
priate safety and health practices and determine the applica- f = heat flux transducer output, mV
bility of regulatory limitations prior to use. N = heat flux transducer calibration constant,
W/(m2·mV), Btu/(h·ft2·mV)
2. Referenced Documents Nf = heat flux, W/m2, Btu/(h·ft2)
DT = temperature difference,° C, °F
2.1 ASTM Standards: Tg = temperature of guard heater, °C, °F
C 518 Test Method for Steady-State Heat Flux Measure- Tu = temperature of upper heater, °C, °F
ments and Thermal Transmission Properties by Means of Tl = temperature of lower heater, °C, °F
the Heat Flow Meter Apparatus2 T1 = temperature of one surface of the specimen, °C, °F
E 1530 Test Method for Evaluating the Resistance to Ther- T2 = temperature of the other surface of the specimen, °C,
mal Transmission of Thin Specimens of Materials by the °F
Guarded Heat Flow Meter Technique3 Tm = mean temperature of the specimen, °C, °F
s = unknown specimen
3. Terminology r = known calibration or reference specimen
3.1 Definitions of Terms Specific to This Standard: o = contacts
4. Summary of Test Method
1
This test method is under the jurisdiction of ASTM Committee D02 on 4.1 A specimen and a heat flux transducer (HFT) are
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.05.0E on Properties of Fuels, Petroleum Coke and Carbon Materials.
sandwiched between two flat plates controlled at different
Current edition approved Dec. 10, 2001. Published February 2002. temperatures, to produce a heat flow through the test stack. A
2

3
Annual Book of ASTM Standards, Vol 04.06. reproducible load is applied to the test stack by pneumatic or
Annual Book of ASTM Standards, Vol 14.02.

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

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 D 6744
hydraulic means, to ensure that there is a reproducible contact spring loaded mechanism. In either case, means must be
resistance between the specimen and plate surfaces. A cylin- provided to ensure that the loading can be varied and set to
drical guard surrounds the test stack and is maintained at a certain values reproducibility.
uniform mean temperature of the two plates, in order to 6.2.2 The loading force must be transmitted to the stack
minimize lateral heat flow to and from the stack. At steady- through a gimball joint (2) that allows up to 5° swivel in the
state, the difference in temperature between the surfaces plane perpendicular to the axis of the stack.
contacting the specimen is measured with temperature sensors 6.2.3 Suitable insulator plate (3) separates the gimball joint
embedded in the surfaces, together with the electrical output of from the top plate (4).
the HFT. This output (voltage) is proportional to the heat flow
6.2.4 The top plate (assumed to be the hot plate for the
through the specimen, the HFT and the interfaces between the
purposes of this description) is equipped with a heater (5) and
specimen and the apparatus. The proportionality is obtained
control thermocouple (6) adjacent to the heater, to maintain a
through prior calibration of the system with specimens of
certain desired temperature. (Other means of producing and
known thermal resistance measured under the same conditions,
maintaining temperature may also be used as long as the
such that contact resistance at the surface is made reproducible.
requirements under 6.3 are met.) The construction of the top
5. Significance and Use plate is such as to ensure uniform heat distribution across its
face contacting the sample (8). Attached to this face (or
5.1 This test method is designed to measure and compare
embedded in close proximity to it), in a fashion that does not
thermal properties of materials under controlled conditions and
interfere with the sample/plate interface, is a temperature
their ability to maintain required thermal conductance levels.
sensor (7) (typically a thermocouple, thermistor) that defines
6. Apparatus the temperature of the interface on the plate side.
6.1 A schematic rendering of a typical apparatus is shown in 6.2.5 The sample (8) is in direct contact with the top plate
Fig. 1. The relative position of the HFT to sample is not on one side and an intermediate plate (9) on the other side.
important (it may be on the hot or cold side) as the test method 6.2.6 The intermediate plate (9) is an optional item. Its
is based on maintaining axial heat flow with minimal heat purpose is to provide a highly conductive environment to the
losses or gains radially. It is also up to the designer whether to second temperature sensor (10), to obtain an average tempera-
choose heat flow upward or downward or horizontally, al- ture of the surface. If the temperature sensor (10) is embedded
though downward heat flow in a vertical stack is the most into the face of the HFT, or other means are provided to define
common one. the temperature of the surface facing the sample, the use of the
6.2 Key Components of a Typical Device: intermediate plate is not mandatory.
6.2.1 The compressive force for the stack is to be provided 6.2.7 Heat flux transducer (HFT) is a device that will
by either a regulated pneumatic or hydraulic cylinder (1) or a generate an electrical signal in proportion to the heat flux

FIG. 1 Key Components of a Typical Device

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 D 6744
across it. The level of output required (sensitivity) greatly the specimen DT is not less than 3 °C. Adjust the guard heater
depends on the rest of the instrumentation used to read it. The temperature (Tg) such that it is at approximately the average of
overall performance of the HFT and its readout instrumentation Tu and Tl.
shall be such as to meet the requirements in Section 13. 9.2 Select at least two calibration specimens having thermal
6.2.8 The lower plate (12) is constructed similarly to the resistance values that bracket the range expected for the test
upper plate (4), except it is positioned as a mirror image. specimens at the temperature conditions required.
6.2.9 An insulator plate (16) separates the lower plate (12) 9.3 Table 1 contains a list of several available materials
from the heat sink (17). In case of using circulating fluid in commonly used for calibration, together with corresponding
place of a heater/thermocouple arrangement in the upper and/or thermal resistance (Rs) values for a given thickness. This
lower plates, the heat sink may or may not be present. information is provided to assist the user in selecting optimum
6.2.10 The entire stack is surrounded by a cylindrical guard specimen thickness for testing a material and in deciding which
(18) equipped with a heater (19) and a control thermocouple calibration specimens to use.
(20) to maintain it at the mean temperature between the upper 9.4 The range of thermal conductivity for which this test
and lower plates. A small, generally unfilled gap separates the method is most suitable is such that the optimum thermal
guard from the stack. For instruments limited to operate in the resistance range is from 10 3 10−4 to 400 3 10−4 m−2·K/W.
ambient region, no guard is required. A draft shield is recom- The most commonly used calibration materials are the Pyrex
mended in place of it. 7740, Pyroceram 9606, and stainless steel.
NOTE 2—It is permissible to use thin layers of high conductivity grease 9.5 Measure the thickness of the specimen to 25 µm.
or elastomeric material on the two surfaces of the sample to reduce the 9.6 Coat both surfaces of a calibration specimen with a very
thermal resistance of the interface and promote uniform thermal contact thin layer of a compatible heat sink compound or place a thin
across the interface area. layer of elastomeric heat transfer medium on it to help
NOTE 3—The cross sectional area of the sample may be any, however,
minimize the thermal resistance at the interfaces of adjacent
most commonly circular and rectangular cross sections are used. Mini-
mum size is dictated by the magnitude of the disturbance caused by contacting surfaces.
thermal sensors in relation to the overall flux distribution. The most 9.7 Insert the calibration specimen into the test chamber.
common sizes are 25 mm round or square to 50 mm round. Exercise care to ensure that all surfaces are free of any foreign
6.3 Requirements: matter.
6.3.1 Temperature control of upper and lower plate is to be 9.8 Close the test chamber and clamp the calibration speci-
6 0.1 °C (6 0.18 °F) or better. men in position between the plates at the recommended
6.3.2 Reproducible load of 0.28 MPa (40 psi) has been compressive load of 0.28 MPa.
found to be satisfactory for solid samples. Minimum load shall 9.9 Wait for thermal equilibrium to be attained. This should
not be below 0.07 MPa (10 psi). be seen when all the temperatures measured do not drift more
6.3.3 Temperature sensors are usually fine gage or small than 0.1° C in 1 min. Read and record all temperatures and the
diameter sheath thermocouples, however, ultraminiature resis- output of the heat flux transducer.
tance thermometers and linear thermistors may also be used. NOTE 4—The time to attain thermal equilibrium is dependent upon the
6.3.4 Operating range of a device using a mean temperature thickness of the specimen and its thermal properties. Experience shows
guard shall be limited to − 100 °C to 300 °C, when using that approximately 1 h is needed for thermal equilibrium to be attained,
thermocouples as temperature sensors, and − 180 °C to 300 °C when testing a sample with the thermal conductivity within the optimum
with platinum resistance thermometers. operating range of the instrument.
9.10 Repeat the procedure in 9.5 to 9.9 with one or more
7. Test Specimen
calibration specimens, having different thermal resistance val-
7.1 The specimen to be tested shall be representative for the ues covering the expected range for the test specimen.
sample material. The recommended specimen configuration is
a 50.8 6 0.25 mm (2 6 0.010 in.) diameter disk, having
smooth flat and parallel faces, 6 0.025 mm (6 0.001 in.), such TABLE 1 Typical Thermal Resistance Values of Specimens of
that a uniform thickness within 0.025 mm (6 0.001 in.) is Different Materials
attained in the range from 12.7 to 25.4 mm (0.5 to 1.0 in.) Material Approximate Thickness, Approximate
Thermal mm Thermal
8. Sampling and Conditioning Conductivity, Resistance,
W/(m·K) at 10 m2·K/W at
−4

8.1 Cut representative test specimens from larger pieces of 30°C 30 °C

the sample material or body. Pyroceram 9606A 4 20 50
8.2 Condition the cut specimens in accordance with the Pyroceram 9606A 4 10 25
requirements of the appropriate material specifications, if any. Pyrex 7740A Glass 1 20 200
Pyrex 7740A Glass 1 10 100
Pyrex 7740A Glass 1 1 10
9. Calibration 304 Stainless Steel 14 20 14
304 Stainless Steel 14 10 7
9.1 Select the mean temperature and load conditions re- VespelB 0.4 2 50
quired. Adjust the upper heater temperature (Tu) and lower A
Pyrex 7740 and Pyroceram 9606 are products and trademarks of Corning
heater temperature (Tl) such that the temperature difference at Glass Co., Corning, WV.
the required mean temperature is no less than 30 to 35 °C and B
Vespel is a product of DuPont Co.

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 D 6744
10. Thermal Conductivity of an Unknown Specimen number in practical units of 10−4 m2·K/W and derive values of
10.1 Tests shall only be conducted at a temperature in a thermal conductivity to the second significant figure level of
range and under applied load conditions for which valid precision.
calibration data exists. 11.2.1 Graphical Method—At each set of conditions, Eq 1
10.1.1 When automatic control of temperature of the heaters is represented by a straight line on a graph of Rs versus (T1 −
is involved, the controller settings should be checked to ensure T2)/Q. Plot the test result of the calibration specimens on the
that they are the same as those for the desired temperature level graph, and draw a best-fit straight line through the data points
for the calibration. as illustrated in Fig. 2. When measuring the thermal conduc-
10.2 Measure the thickness of the specimen to 25 µm. tivity of a test specimen, obtain Rs by drawing a vertical line at
10.3 Apply a thin layer of heat sink compound or place a the appropriate value of (T1 − T2)/Q to intersect the calibration
thin layer of elastomeric heat transfer medium on the surfaces line. Obtain values of Cs and ls from Eq 2 and Eq 3.
of the test specimen. 11.2.2 Analytical Method—At each set of conditions, solve
Eq 1 mathematically for N and R0 after measuring a pair of
NOTE 5—Exercise care to ensure that any material applied to the reference specimens to yield two sets of data for Rs and (T1 −
surfaces of the specimen does not change its thermal properties by soaking
into it.
T2)/Q. Eq 1 can be used subsequently to determine Rs of the
test specimen following measurement of T1, T2, and Q provid-
10.4 Repeat the procedure in 9.7 to 9.9 using the test ing the calculated Rs falls within the calibration range corre-
specimen. sponding to the particular pair of reference specimens in
NOTE 6—Experience has indicated that for reliable measurements on a accordance with 9.2. By calibrating with additional reference
single specimen, the minimum thickness (mm) is given by Dx $ 3l specimens of different thermal resistances, several linear equa-
(W/(m·K)). tions can be generated, each covering a part of the overall
10.5 Automated Systems—Computerized or otherwise auto- range.
mated systems may require different operating steps, and may 11.2.3 Computer-Aided Analysis:
or may not provide intermediate readings described in 9.9. For 11.2.3.1 At each set of conditions, solve Eq 1 mathemati-
these devices, follow the operating and calibrating procedures cally for N and R0, using a linear regression analysis of the
prescribed by the manufacturer. results for several sets of data for Rs and (T1 − T2)/Q produced
as a result of testing several calibration specimens. A similar
NOTE 7—For an automated system to meet the requirements of this test series of tests carried out at the different temperatures provides
method, the calibrating, testing, and calculational methods built into it
shall at minimum include the steps or principles set forth in Section 10,
new values of N and R0.
and all applicable guidelines given in Section 6, 9, 12 and 13. 11.2.3.2 Determine a polynomial relationship between N
and temperature, and between R0 and temperature, so that Eq 1
11. Calculation becomes:
11.1 At equilibrium, the Fourier heat flow equation applied T1 2 T 2
Rs 5 f1 ~T!· Q 2 f2 ~ T ! (4)
to the system becomes as follows:
N ~ T1 2 T2 ! where:
Rs 5 Q 2 R0 (1)
f1(T) = temperature dependent value of N,
and: f2(T) = temperature dependent value of R0, and
1 T = test temperature.
Cs 5 R (2) 11.2.3.3 R2 and l of the test specimen are calculated
s
automatically, once T1, T2, and Q have been measured. Results
11.1.1 For homogeneous materials:
are accurate provided that the test temperatures fall within the
Dx limits used during calibration, and that Rs does not fall outside
Rs 5 l (3)
the calibration range obtained with the reference specimens.
11.1.2 In Eq 1, N and R0 are temperature-and load-
dependent parameters obtained by calibration at each particular 12. Report
set of conditions. Once obtained, they should remain fixed for 12.1 Report the following information:
the particular settings used to attain the conditions. 12.1.1 Complete identification and description of material
NOTE 8—Since N is also determined by the particular HFT utilized, the and specimen including any conditioning procedure;
calibration should be checked occasionally to ensure that continuous 12.1.2 Details of reference specimen materials used for
heating/cycling does not affect the HFT. calibration;
NOTE 9—The parameter R0 depends on the parallelism of the two 12.1.3 Details of temperatures of appropriate surfaces,
surface plates and should be reproducible unless the test section is altered guard and ambient, °C (°F);
mechanically in any way. If this occurs, recalibration is necessary. 12.1.4 Applied load, Pa (psi);
11.2 There are three methods of data analysis to determine 12.1.5 Specimen thickness, mm (in.);
Rs, Cs, and l. In each case, utilize relevant input parameters 12.1.6 Mean temperature, °C (°F);
determined to the stated precision levels and use all available 12.1.7 Measured thermal resistance to the nearest whole
decimal places through the calculation stages to the final result. number in practical units, 10−4 m2·K/W (h·ft2·°F/Btu) and
Calculate the thermal resistance Rs to the nearest whole derived thermal conductivity to the second significant figure in

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D 6744

FIG. 2 Thermal Resistance Versus (T1–T2) / Q

 D 6744
W/(m·K) (Btu·in./(h·ft2·°F)); include details of the calculation 13. Precision and Bias
method used (for manual instruments, omit for automated
13.1 A round robin program is in progress.
systems);
12.1.8 The sample’s mean temperature and the direction
14. Keywords
and orientation of thermal transmission through the sample,
since some bodies are not isotropic with respect to thermal 14.1 heat flow meter; heat flux transducer; thermal conduc-
conductivity; and tance; thermal conductivity; thermal resistance
12.1.9 Designation of model/make in case a commercial
device is used.

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