Thermal Conductivity of Solids PDF
Thermal Conductivity of Solids PDF
Thermal Conductivity of Solids PDF
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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This is a highly idealized situation, however, since it must be thoroughly tested. Requirements for qualifying an
assumes no heat exchange between the column and insulation apparatus are outlined in Section 10.
at any position and uniform heat transfer at each meter
bar-specimen interface. The errors caused by these two as- 6. Requirements
sumptions vary widely and are discussed in Section 10.
6.1 Meter Bar Reference Materials:
Because of these two effects, restrictions must be placed on this
test method, if the desired accuracy is to be achieved. 6.1.1 Reference materials or transfer standards with known
thermal conductivities must be used for the meter bars. Since
the minimum measurement error of the method is the uncer-
tainty in lM, it is preferable to use standards available from a
national standards laboratory. Other reference materials are
available because numerous measurements of l have been
made and general acceptance of the values has been obtained.
Table 1 lists the currently available recognized reference
materials including those available from National Institute of
Standards and Technology. Fig. 2 shows the approximate
variation of lM with temperature.
6.1.2 Table 1 is not exhaustive and other materials may be
used as references. The reference material and the source of lM
values shall be stated in the report.
6.1.3 The requirements for any reference material include
stability over the temperature range of operation, compatibility
with other system components, reasonable cost, ease of ther-
mocouple attachment, and an accurately known thermal con-
ductivity. Since heat shunting errors for a specific lI increase as
lM/ls varies from unity, (1) the reference which has a lM
nearest to lS should be used for the meter bars.
6.1.4 If a sample’s thermal conductivity ls is between the
thermal conductivity values of two types of reference materi-
als, the reference material with the higher lM should be used to
reduce the total temperature drop along the column.
6.2 Insulation Materials:
6.2.1 A large variety of powder, particulate, and fiber
materials exists for reducing both radial heat flow in the
column-guard annulus and surrounds, and for heat shunting
along the column. Several factors must be considered during
selection of the most appropriate insulation. The insulation
NOTE 1—The material selected for the meter bars should have a thermal must be stable over the anticipated temperature range, have a
conductivity as near as possible to the thermal conductivity of the low lI, and be easy to handle. In addition, the insulation should
unknown.
not contaminate system components such as the temperature
FIG. 2 Approximate Values for the Thermal Conductivity of
Several Possible Reference Materials for Meter Bars sensors, it must have low toxicity, and it should not conduct
electricity. In general, powders and particulates are used since
they pack readily. However, low density fiber blankets can also
5. Significance and Use be used.
6.2.2 Some candidate insulations are listed in Table 2.
5.1 The comparative method of measurement of thermal
conductivity is especially useful for engineering materials 6.3 Temperature Sensors:
including ceramics, polymers, metals and alloys, refractories, 6.3.1 There shall be a minimum of two temperature sensors
carbons, and graphites including combinations and other com- on each meter bar and two on the specimen. Whenever
posite forms of each. possible, the meter bars and specimen should each contain
5.2 Proper design of a guarded-longitudinal system is diffi- three sensors. The extra sensors are useful in confirming
cult and it is not practical in a method of this type to try to linearity of temperature versus distance along the column, or
establish details of construction and procedures to cover all indicating an error due to a temperature sensor decalibration.
contingencies that might offer difficulties to a person without 6.3.2 The type of temperature sensor depends on the system
technical knowledge concerning theory of heat flow, tempera- size, temperature range, and the system environment as con-
ture measurements, and general testing practices. Standardiza- trolled by the insulation, meter bars, specimen, and gas within
tion of this test method is not intended to restrict in any way the the system. Any sensor possessing adequate accuracy may be
future development by research workers of new or methods or used for temperature measurement (2) and be used in large
improved procedures. However, new or improved techniques systems where heat flow perturbation by the temperature
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TABLE 1 Reference Materials For Use as Meter Bars
Percentage
Material Temperature Range (K) Uncertainty lM(W/m·K) Material Source
in l (6 %)
A
Electrolytic Iron SRM 734 To 1000 2 NISTA
Tungsten SRM 730 4 to 300 2 lM Dependent on TA NISTA
300 to 2000 2 to 5
>2000 5 to 8
Austenitic Stainless SRM 4 to 1200 <5 % lM = 1.22T0.432 T > 200KA NISTA
735
Iron 80 to 1200 2 lM should be calculated from ...
measured valuesBC
Copper 90 to 1250 <2 lM = 416.3 − 0.05904T + 7.087 manufacturer
3107/T3D
EF
Pyroceram Code 9606 90 to 1200 ... manufacturer
Fused SilicaG 1300 <8 lM = (84.7/T) + 1.484 + 4.94 3 10−4 manufacturer
Up to 900 K T + 9.6 3 10−13T4HI
EF
Pyrex 7740 90 to 600 6 manufacturer
A
National Institute of Standards and Technology, Washington, D.C. 20234. See Special Publications 260-52 and 260-46.
B
Fulkerson W., et al., Physics Review 167, p. 765, (1968).
C
Lucks C. F., Journal of Testing and Evaluation, ASTM 1 (5), 422 (1973).
D
Moore, J. P., Graves, R. S. and McElroy, D. L., Canadian Journal of Physics, 45, 3849 (1967).
E
“Thermal Conductivity of Selected Materials,” Report NSRDS-NBS 8, National Bureau of Standards, 1966.
F
L. C. Hulstrom, R. P. Tye, and S. E. Smith, Thermal Conductivity 19, Ed. D. W. Yarbrough, Plenum Press, New York, In Course of Publication (see also High
Temperature-High Pressures, 17, 707, 1985.
G
Hust J. G., Cryogenics Division; NBS, Boulder, Colorado 80302.
H
Above 700 K a large fraction of heat conduction in fused silica will be by radiation and the actual effective values may depend on the emittances of bounding surfaces
and meter bar size.
I
Recommended values from Table 3017 A-R-2 of the Thermophysical Properties Research Center Data Book, Vol. 3, “Nonmetallic Elements, Compounds, and
Mixtures,” Purdue University, Lafayette, Indiana.
TABLE 2 Suitable Thermal Insulation Materials 6.3.5 In Fig. 3b, the thermocouple resides in a radial slot,
Typical Thermal Conductivity (W/(m·K)) and in Fig. 3c the thermocouple is pulled through a radial hole
MaterialA
300K 800K 1300K in the material. When a sheathed thermocouple or a thermo-
Poured Powders couple with both thermoelements in a two-hole electrical
Diatomaceous Earth 0.053 0.10 0.154 insulator is used, the thermocouple attachment shown in Fig.
Bubbled Alumina 0.21 0.37 0.41 3d can be used. In the latter three cases, the thermocouple
Bubbled Zirconia 0.19 0.33 0.37
Vermiculite 0.07 0.16 ... should be thermally connected to the solid surface using a
Perlite 0.050 0.17 ... suitable glue or high temperature cement. All four of the
Blankets and Felts procedures shown in Fig. 3 should include wire tempering on
Aluminosilicate 60–120 kg/m3 0.044 0.13 0.33
Zirconia 60–90 kg/m3 0.039 0.09 0.25 the surfaces, wire loops in isothermal zones, thermal wire
A
All materials listed can be used up to the 1300 K limit of the comparative
grounds on the guard, or a combination of all three (5).
longitudinal except where noted. 6.3.6 Since uncertainty in temperature sensor location leads
to large errors, special care must be taken to determine the
correct distance between sensors and to calculate the possible
sensors would be negligible. Thermocouples are normally error resulting from any uncertainty.
employed. Their small size and the ease of attachment are 6.4 Reduction of Contact Resistance:
distinct advantages. 6.4.1 This test method requires uniform heat transfer at the
6.3.3 When thermocouples are employed, they should be meter bar to specimen interfaces whenever the temperature
fabricated from wires which are 0.1 mm diameter or less. A sensors are within a distance equal to rA from an interface (6).
constant temperature reference shall always be provided for all This requirement necessitates a uniform contact resistance
cold junctions. This reference can be an ice-cold slurry (3), a across the adjoining areas of meter bars and specimens. This is
constant temperature zone box, or an electronic ice point normally attained by use of an applied axial load in conjunction
reference. All thermocouples shall be fabricated from either with a conducting medium at the interfaces. Measurements in
calibrated thermocouple wire (4) or from wire that has been a vacuum environment are not recommended, unless the
certified by the supplier to be within the limits of error vacuum is required for protection purposes.
specified in Table 1 of Standard E 230. 6.4.2 For the relatively thin specimens normally used for
6.3.4 Thermocouple attachment is important to this tech- materials having a low thermal conductivity, the temperature
nique in order to ensure that reliable temperature measure- sensors must be mounted close to the surface and in conse-
ments are made at specific points. The various techniques are quence the uniformity of contact resistance is critical. In such
illustrated in Fig. 3. Intrinsic junctions can be obtained with cases, a very thin layer of a compatible highly conductive fluid,
metals and alloys by welding individual thermo-elements to the paste, soft metal foil, or screen shall be introduced at the
surfaces (Fig. 3a). Butt or bead welded thermocouples junc- interfaces.
tions can be rigidly attached by peening, cementing, or welding 6.4.3 Means shall be provided for imposing a reproducible
in fine grooves or small holes (Fig. 3b, 3c, and 3d). and constant load along the column with the primary purpose
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3a 3b
Intrinsic weld with separate temperature elements welded to specimen or meter Radial slots on the flat surfaces to hold a bare wire or ceramic insulated
bars so that signal is through the material. thermocouple sensor the may be bonded into slot.
3c 3d
Small radial hole drilled through the specimen or meter bar and non-insulated Small Radial hole drilled part way through the specimen or meter bar and a
(permitted if the material is an electrical insulator) or insulated thermocouple pulled thermocouple pushed into the hole.
through the hole.
NOTE 1—In all cases the thermoelements should be thermally tempered and/or thermally grounded on the guard to minimize temperature measurement
errors due to heat flow into or out of the hot junction.
FIG. 3 Thermocouple Attachments
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sensor attachment to be far enough away from the interfaces to ensure that the system should be pumped and purged, and the operating
heat flow was uniform. The specimen length should be selected based on gas and pressure established. The predetermined force required
considerations of radius and thermal conductivity. When lM is higher than for reducing the effects of non-uniform interfacial resistance
the thermal conductivity of SRM 735 (stainless steel), long specimens
with length / rA>>1 can be used. These long specimens permit the use of
should be applied to the load column.
large distances between temperature sensors and this reduces the percent- 9.2 Heaters at either end of the column should be energized
age error derived from the uncertainty in sensor position. When l M is (see Note 4) and adjusted until the temperature differences
lower than the thermal conductivity of SRM 735, the sample’s length must between positions Z1 and Z2, Z3 and Z4, and Z5 and Z6 are
be reduced because uncertainty due to the heat shunting becomes too between 200 times the imprecision of the DT measurements
large. and 30 K, and the specimen is at the average temperature
7.2 Sampling and Conditioning—Unless specifically re- desired for the measurement. Although the exact temperature
quired or prescribed, one representative specimen shall be profile along the guard is not important for rB/rA $ 3, the power
prepared from the sample and no preconditioning has to be to the guard heaters should be adjusted until the temperature
undertaken. profile along the guard, Tg (z), is constant with respect to time
to within 60.1 K and either:
8. Calibration and Verification 9.2.1 Approximately linear so that Tg (z) coincides with the
8.1 There are many situations that call for equipment temperature along the sample column at a minimum of three
verifications before operations on unknown materials can be places including the temperature at the top sensor on the top
successfully accomplished. These include the following: meter bar, the bottom sensor on the bottom bar, and the
8.1.1 After initial equipment construction, specimen midplane; or
8.1.2 When the ratio of lM to lS is less than 0.3 or greater 9.2.2 Constant with respect to z to within 65 K and
than 3 and it is not possible to match thermal conductance matched to the average temperature of the test specimen.
values,
NOTE 4—These heaters can either be attached to the ends of the meter
8.1.3 When the specimen shape is complex or the specimen bars or to a structure adjacent to the meter bar. The heaters can be powered
is unusually small, with A.C. or D.C. Several different heater configurations are acceptable.
8.1.4 When changes have been made in the system geom- The power to these heaters shall be steady enough to maintain short term
etry, temperature fluctuations less than 60.03 K on the meter bar thermocouple
8.1.5 When meter bar or insulation material other than those nearest the heater. These two heaters, in conjunction with the guard shell
listed in 5.1 and 5.2 are considered for use, and heater and the system coolant shall maintain long term temperature drift
less than 60.05 K/h.
8.1.6 When the apparatus has been previously operated to a
high enough temperature to change the properties of a compo- 9.3 After the system has reached steady state (T drift <0.05
nent such as thermocouples’ sensitivity. K/h), measure the output of all temperature sensors.
8.2 These verification tests shall be run by comparing at
least two reference materials in the following manner: 10. Calculation
8.2.1 A reference material which has the closest thermal 10.1 Approximate Specimen Thermal Conductivity:
conductivity to the estimated thermal conductivity of the 10.1.1 The outputs from the temperature sensors shall be
unknown sample should be machined according to 6.1, and converted to temperature, and the apparent heat flow per unit
8.2.2 The thermal conductivity l of the specimen fabricated area, q8, in the meter bars shall be calculated using the
from a reference material shall then be measured as described following:
in Section 9, using meter bars fabricated from another refer- T2 2 T1
ence material which has the closest l to that of the specimen. q8T 5 lM · Z 2 Z
2 1
For example, verification tests might be performed on a top bar (2)
Pyroceramy 9606 specimen using meter bars fabricated from T6 2 T 5
SRM 735 stainless steel. If the measured thermal conductivity q8B 5 lM · Z 2 Z
6 5
of the specimen disagrees with the value from Table 1 after bottom bar (3)
applying the corrections for heat exchange, additional effort is In each of these equations, the lM value (see Note 5) to be
required to find the error source(s). inserted shall be obtained from the information of 6.1 for the
9. Procedure average meter bar temperature. Although these two values, q8
T and q8B, should agree with each other to within about 610 %
9.1 Where possible and practical, select the reference speci-
when heat exchange with the insulation is small, good agree-
mens (meter bars) such that the thermal conductance is of the
ment is not a sufficient condition (nor always a necessary
same order of magnitude as that expected for the test specimen.
condition) for low heat shunting error.
After instrumenting and installing the proper meter bars, the
10.1.2 A value for the specimen thermal conductivity at
specimen should be instrumented similarly. It should then be
temperature (T3 + T4)/2, as uncorrected for heat exchange with
inserted into the test stack such that it is at aligned between the
the insulation, can then be calculated using the following:
meter bars with at least 99 % of each specimen surface in
contact with the adjacent meter bar. Soft foil or other contact- ~q8T 1 q8B! ~Z4 2 Z 3!
l8S 5 (4)
ing medium may be used to reduce interfacial resistance. If the 2 ~ T4 2 T 3 !
system must be protected from oxidation during the test or if NOTE 5—This type of calculation procedure actually requires only two
operation requires a particular gas or gas pressure to control lI, temperature sensors on each column section. In this case, the third sensor
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on each section serves as a test for consistency of the other two. Some since all such specimens should have the same size as the
calculation procedures require more than the two sensors to obtain more specimen with an unknown thermal conductivity and have the
knowledge about dT/dZ. same surface finish.
10.2 Corrections for Extraneous Heat Flow:
10.2.1 Calculation of the specimen thermal conductivity by 11. Report
a simple comparison of temperature gradients in the meter bars 11.1 The report of the test results shall include the follow-
to that in the specimen is less valid when the specimen or meter ing:
bars, or both, have low thermal conductivities relative to that of 11.1.1 Complete specimen identification including shape
the insulation. The apparatus should be designed to minimize and size,
these errors. The deviation from uniform heat flow has been 11.1.2 Complete identification of insulation and source of lI
expressed as follows (1) : values, gas, and gas pressure,
g 5 F g Fl (5) 11.1.3 Statements of thermocouple type, size, and attach-
where Fg is a function of system dimensions, and Fl is a ment procedure,
function of lM, lI, and lS (1). The Fg term has a value between 11.1.4 Complete listing of the geometrical dimensions of
2 and 3 for the ratio of guard radius to column radius specified the system including rA, rB, specimen height, meter bar height,
for this system. The Fl term is shown in Fig. 4 as a function of and distances between temperature sensors,
l/lI for various values of lM/lI for a linear guard. At high 11.1.5 Column force,
ratios of lM/lI and lS/lI, corrections would not be necessary 11.1.6 Meter bar material and source of lM values if other
since the departure from ideal heat flow would be small. For than those listed in Table 1,
example, the product of Fl and Fg would be less than 0.10 11.1.7 Reference to the use of this test method shall include
(10 %) for all measurements where l M/lI and lS/lI are greater a statement of the percentage variation of the qualification
than 30. If the value of FgFl is to be kept below 10 %, the results about the true value. For example, “thermal conductiv-
ratios lM/lI and ls/lI must be within the boundaries on Fig. 4. ity results on Pyroceramy 9606 using SRM 735 meter bars
10.2.2 Measurements on materials where the ratios of lM/lI were within 64 % of the accepted values for Pyroceramy over
and lS/lI do not fall within these boundaries shall be accom- the temperature range from 250 to 900 K,”
panied with corrections for extraneous heat flow. These cor- 11.1.8 Variations, if any, from this test method. If results are
rections can be determined in the following three different to be reported as having been obtained by this method, then all
ways: requirements prescribed by this method shall be met. Where
10.2.2.1 Use of analytical techniques as described by such conditions are not met, the phrase, “All requirements of
Didion (1) and Flynn (8), this method have been met with the exception of ...” shall be
10.2.2.2 Using calculations from finite-difference or finite- added and a complete list of the exceptions included;
element heat conduction codes, and 11.1.9 Measured values of temperature and specimen ther-
10.2.2.3 Determined experimentally by using several refer- mal conductivity.
ence materials or transfer standards of different thermal con-
ductance as specimens. The procedure must be used cautiously 12. Precision and Bias
12.1 Example of Error Estimation:
12.1.1 Assumptions for a system where both meter bars and
the specimen are of equal length is that the sensor spacings are
all 13 mm and lM' l S:
U dll U 5 ? 0.003 ?
M
M
(6)
Z2 2 Z1 ; Z4 2 Z 3 ; Z6 2 Z5 5 13 mm;
T2 2 T 1 ; T4 2 T3 ; T 6 2 T5 5 10 K;
d~Z2 2 Z 1! ; d~Z4 2 Z3! ; d~Z 6 2 Z5! 5 0.2 mm; and
d~T2 2 T 1! ; d~T4 2 T3! ; d~T 6 2 T5! 5 0.04 K.
12.1.2 The maximum value of d(Z2 − Z 1) etc. was approxi-
mated by assuming an uncertainty of 60.5 (sensor diameter) at
each temperature measurement position. Therefore, if the
diameter of each sensor is 0.2 mm, the uncertainty in the
difference would be 60.2 mm. The number for d(T2 − T1) etc.
was calculated based on the sensor absolute accuracy.
12.1.3 With these values the fractional uncertainty in l8S
will be |0.069| or 66.9 %.
ls/li 12.2 Indeterminate Errors:
FIG. 4 Fractional Heat Exchange Between the Meter Bar-
12.2.1 There are at least three other errors that can contrib-
Specimen Column and Surrounding Insulation as a Function of ute to total system error and these are (1) non-uniform
lm/l i for Several Values of ls/li interfacial resistance, (2) heat exchange between the column
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and the guard, and (3) heat shunting through the insulation 12.3 Overall—An international, inter-laboratory round
around the column. These three errors must be minimized or robin study also involving absolute methods (9) has shown that
appropriate corrections applied to the data if the desired a precision of 66.8 % can be attained over the temperature
accuracy is to be obtained. range 300 to 600 K. Although no definite bias could be
12.2.2 The contributions from the last two errors can be established these are indications that the values were on the
determined approximately using results from appropriate ex- order of 2 % lower than those obtained by absolute methods.
periments carried out at different levels of guard temperature to This cited paper is on file at ASTM as a research report.
specimen stack temperature out of balance.
REFERENCES
(1) Didion, D. A., “An Analysis and Design of a Linear Guarded Cut-Bar (6) Fried, E., Thermal Conductivity, Vol 2, Tye, R. P. (ed.), Academic
Apparatus for Thermal Conductivity Measurements,” AD-665789, Press, New York (1969).
January, 1968, available from the National Technical Information (7) Morgan, M. T., and West, G. A., “Thermal Conductivity of the Rocks
Service, Springfield, VA. in the Bureau of Mines Standard Rock Site,” Thermal Conductivity,
(2) Finch, D. I., “General Principles of Thermoelastic Thermometry,” in 16, Larsen, D. C., ed., Plenum Press, NY, NY, 1983, pp 79–90.
Temperature, It’s Measurement and Control in Science and Industry, (8) Flynn, D. R., “Thermal Conductivity of Ceramics,” Mechanical and
Vol. 3, Part 2, Section 1, Reinhold Publishing Corporation. Thermal Properties of Ceramics, Special Publication 303, National
(3) Caldwell, F. R., “Temperatures of Thermocouple Reference Junctions Bureau of Standards, 1969.
in an Ice Bar,” J. Res. Nat. Bur. Std., 69C (2) (1965). (9) Hulstrom, L. C., Tye, R. P., and Smith, S. E., “Round-Robin Testing of
(4) ASME: PTC 19.3, Temperature Measurement, Part 3, p. 1232, 1974. Thermal Conductivity Reference Materials,” Thermal Conductivity,
(5) Anderson, R. L., and Kollie, T. G., “Problems in High Temperature 19, Yarbrough, D. W., ed., Plenum Press, New York. (See also
Thermometry,” July, 1976, pp. 171–221. High-Temp-High Pressures, Vol 17, p. 707, 1985).
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