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Abstract
Described in this paper is an apparatus in which bulk samples can easily be mounted on a removable puck for thermal con-
ductivity measurements and then placed in the described measurement system. This rapid mounting and measurement system uses a
standard steady-state absolute thermal conductivity measurement but allows for rapid measurement and excellent thermal stability
coupled with the use of a closed cycle refrigerator. The distinction of this system is rapid mounting and measurement of thermal
conductivity over a broad temperature range without sacrificing accuracy and precision in data acquisition. In addition, this system
allows for versatility in its use. The design of this apparatus, measurement specifications, and thermal conductivity data on several
standard materials measured in this system are presented. Ó 2002 Elsevier Science Ltd. All rights reserved.
radiation losses. For example, in order to minimize essential when designing this system was the ability to
conductive loss a differential thermocouple is utilized so thermally sink the samples to the cold finger. This was
that there will only be two wires available as a heat leak achieved through the use of custom designed compo-
instead of four wires if standard thermocouples were nents at Clemson, coupled with the use of commercial
used. The absolute technique requires fewer thermo- parts (specifically a removable puck and puck recepta-
couples and provides a smaller quantity of places to cle, provided by Quantum Design) and incorporating
make poor thermal contacts than if a comparative these into a commercial cryocooler system. The com-
technique was used. mercial manufactured parts used here are also used in
Radiative loss is also a major concern when using any the Quantum Design physical properties measurement
solid-state technique to measure thermal conductivity. system (PPMS) to thermally sink experiments to the
There are only a few design features that can be incor- cold finger of the PPMS. The sample puck is made of
porated to overcome these losses and corrections to the oxygen-free high-conductivity copper that couples di-
data are typically necessary. Matching of the tempera- rectly to the puck receptacle that houses the thermom-
ture gradient on a radiation shield surrounding the eter. The sample puck is keyed so that it may only be
sample with the temperature gradient of the sample is inserted into the receptacle in the correct orientation [5].
often used as a solution in larger samples. With smaller Another concern alleviated though the use of commer-
samples, several mm in length, this correction shows cial parts was the effect of thermal cycling on the puck/
little reduction of radiative loss. Another method to receptacle junction since this had been adequately tested
combat radiative loss with small samples is to incorpo- previously.
rate a radiation shield that will reflect the heat back on In order to facilitate rapid throughput of samples, the
the sample. This is accomplished through the use of a puck was designed to accommodate two samples, using
highly reflective surface on the inside of the radiation an absolute steady-state technique. The two mounted
shield. Also essential when making measurements is an samples can be measured simultaneously. Samples are
excellent vacuum which will minimize convection and mounted on the dismountable puck and tested for
heat conduction in the system. Convection will lead to readiness (good electrical contact) in a custom designed
heat transfer along the sample not associated with travel test box before they are plugged into the closed cycle
through the sample. A sweep of power verses DT con- refrigerator. A good ‘‘rule of thumb’’ is that excellent
ducted at a stable temperature should be linear. If it is electrical contact as well as mechanical stability is re-
not a straight line, there are losses due to convection flected into excellent thermal contact. Additionally, the
which need to be corrected for or minimized. dismountable puck allows all sample mountings to be
Another issue that must be taken into consideration performed under a microscope and ensures virtually no
when making thermal conductivity measurements is ‘‘down time’’ in the operation of the closed cycle re-
thermal sinking of the sample. In order to make an ac- frigerator.
curate measurement, the sample must be in excellent Components necessary to thermally couple the puck
thermal contact with the cold finger and heater as well as receptacle to the cold finger were machined (see Fig. 1).
with the thermocouple. Kopp and Slack [4] present an A brass piece is screwed into the cold finger of the closed
excellent discussion of thermal contacting problems with
thermocouples. Uncertainties in measurement of sample
dimension can also lead to a 5–10% uncertainty in the
thermal conductivity measurement since the thermal
conductivity depends on the cross-sectional area of the
sample and the length between the thermocouples. With
many systematic errors that must be considered, then a
5–10% uncertainty in the absolute magnitude of the
thermal conductivity is generally considered to consti-
tute a relatively accurate measurement.
5. Data acquisition
(b)
With corrections made for radiative loss and conduction cut from the same boule. These samples were all
along the wires we conclude that our data is accurate to mounted for thermal conductivity measurements, di-
within 6% of the NIST data. However, the temperature mensions were ascertained, and thermal conductivity
dependence is identical. Much of the difference in mag- recorded. In Fig. 6(a), thermal conductivity of the four
nitude is due to uncertainty in the measurement of the samples is shown. The data are all within 10% of one
sample dimensions as well as conductive and convective another. This variability is probably due to dimensional
losses, which may be estimated and corrected for. Low uncertainties as well as possible slight variation in
thermal conductivity samples will give off a smaller sample composition between the samples measured. If
signal, so care must be taken to get a very low noise level the data are normalized (Fig. 6(b)), it is seen that the
from the thermocouples. curves lie on top of one another. The slight deviation at
The thermal conductivity measurement is found to be higher temperatures is most likely due to differences in
very accurate, with essentially the same temperature sample size leading to different amounts of radiation
dependence and magnitude of the stainless steel stan- contributions. This data shows that our system has very
dard. However, precision and reproducibility of the good precision and reproducibility. In addition, our
measurement are also very important. In order to check quasicrystalline data show an excellent agreement with
these issues, four AlCuFe quasicrystalline samples were the values in the literature [6].
7. Conclusions
(a)
In conclusion, a custom designed measurement sys-
tem in which thermal conductivity can be measured
accurately and precisely using a dismountable mounting
system has been developed. This system utilizes an ab-
solute thermal conductivity technique, but has the ad-
vantage that two samples are mounted on a puck that is
easily introduced into a closed cycle refrigerator. This
system offers enhanced throughput of samples and ease
of mounting. One added advantage to this system is its
versatility in the type of measurement to be executed on
the dismountable puck. For example, a system has also
been developed to measure thermal conductivity of very
thin fibers (A 0:0001 to 0:01 mm2 ) using a modifica-
tion of this design and incorporating with an extensive
(b) data acquisition program [7]. This parallel thermal
conductivity (PTC) technique measures a background
thermal conductance of the wire heaters and platform
and then the sample is placed in parallel with the
background and measured again. By subtracting the
background the thermal conductance of the sample may
be determined.
Acknowledgements
to thank Quantum Design for providing the parts and [3] Pope AL, Littleton IV RT, Tritt TM. Apparatus for the rapid
support necessary to design this system. We acknowledge measurement of electrical transport properties for both ‘‘needle-
like’’ and bulk materials. Rev Sci Instrum 2001;72:3129.
support from ONR, ARO, DARPA (ONR No. N00014- [4] Kopp J, Slack GA. Thermal contact problems in low temperature
98-0271, ONR/DARPA No. N00014-98-0444, and thermocouple thermometry. Cryogenics February, 1971.
ARO/DARPA No. DAAG55-97-0-0267) and from re- [5] Physical Properties Measurement System: Hardware and Opera-
search funds provided (TMT) from Clemson University. tion Manual. Quantum Design Corporate Headquarters, 11578
Sorrento Valley Road, San Diego, CA 92121, USA.
[6] Perrot A, Duboise JM, Cassart M, Issi JP. In: Proceeding of the 6th
International Conference on Quasicrystals, 1997. p. 588.
References [7] Zawilski BM, Littleton IV RT, Tritt TM. Rev Sci Instrum
2001;72:1770.
[1] Cahill DG. Rev Sci Instrum 1990;61:802. [8] Uher C. private communication.
[2] Parrott JE, Stuckes AD. Thermal conductivity of solids. London:
Pion; 1975.