The specific heat of Cry-Con grease, a copper loaded electrically insulating grease, was
measured between 0.5 and 20 K. The low specific heat and high thermal conductivity of
Cry-Con grease render it a useful thermal bonding material for calorimetric measurements
on samples with low thermal conductivity.
Low temperature specific heat of Cry-Con
grease
M.S. Torikachvili, K.N. Yang, R. Calvo, O.R. Nascimento and M.B. Maple
Key words: cryogenics, insulation,grease, thermal conductivity
Frequently, measurement of the specific heat (69 at low
temperatures with the conventional heat pulse technique is
cumbersome because of the poor thermal conductivity of
the sample. The heat pulse is generally produced with a
resistance heater in good thermal contact with the addenda
of the calorimeter. The change in temperature (T) is
measured with a thermometer that is also in good thermal
contact with the calorimeter addenda.
Our experiments are performed with a semiadiabatic calor-
meter, ~ one in which the temperature, in the equilibrium
situation, drifts slowly and approximately linearly with
time. The temperature is continuously recorded on a strip-
chart recorder; the change in temperoture due to the heat
pulse is inferred from linear extrapolations of T vs time,
both before and after the pulse, to the time at which half
of the pulse has elapsed. The duration of a heat pulse lasts
from 10 to 30 s. After the heat pulse is applied, the tempera-
tures of the sample and the addenda relax to the same value
approximately exponentially with time; ie, as ~ exp (-t/r),
where ~" is the relaxation time constant. This relaxation
time r is an inverse function of the thermal diffusivity of
the sample, and the accuracy of the method depends on
how fast thermal equilibrium is reached, since the semi-
adiabatic condition does not prevail indefinitely.
An alternative way of making specific heat measurements
on a sample with poor thermal conductivity is to grind the
sample and mix it with a medium of good thermal diffusi-
vity and then subtract the contribution of the medium from
the results. Two greases, Apiezon T 2 and Apiezon N 3 , have
been successfully used for this purpose. Cry-Con 4 is a
copper bearing electrically insulating grease, and its low
temperature thermal conductivity was found to be substan-
tially higher than that of silicone-based vacuum greases, s
which makes it an attractive candidate for a thermal con-
tact agent in calorimetry.
We frequently measure the specific heat of magnetic
materials at very low temperatures (0.5 - 20 K range) and
sometimes encounter a sample whose thermal conductivity
at these temperatures is very small, especially if it orders
The authors are with the Institute for Pure and Applied
Physical Sciences and the Department of Physics at the University
of California, San Diego, La Jolla, CA 92093, USA. The research
was supported by the US Department of Energy under contract
No. DE-AT03-76ERT0227. MST is on leave from UNICAMP
(Brazil) and is also supported by FAPESP. RC is on sabbatical
leave from IVIC, Caracas (Venezuela). ORN is on leave from USP,
Sao Carlos (Brazil) and is also supported by CNPq. Paper received
10 May 1982.
magnetically. In such cases, the elapsed time for reaching
thermal equilibrium, after a heat pulse is applied, may be
very long. In a recent experiment, we attempted to
measure the specific heat below 1.5 K of a powdered
specimen of Ni(NH2CO2CH2):2HzO that had been pressed
into a copper sample holder and observed relaxation times
of over 1 h, which considerably limited the accuracy of
the results and made data acquisition an extremely long
and tedious process. Subsequently, we ground the sample
into a rme powder and mixed it with Cry-Con grease
(sample: Cry-Con mass ratio of approximately 40:60)
after which it was again pressed into the copper sample
holder. This procedure reduced the relaxation times to less
than 1 min and greatly facilitated the specific heat
measurement .6
The purpose of this paper is to present an accurate charac-
terization of the specific heat of Cry-Con grease between
0.5 and 20 K, so that its contribution can be estimated
when it is used as a thermal bonding material in calorimetry.
We also compare the specific heat and thermal diffusivity of
Cry-Con grease to Apiezon T 1 and Apiezon N 2 greases.
The experiment was performed in a He3 refrigerated semi-
adiabatic calorimeter, in which the temperature sensor was
a germanium resistor. A 0.430 g amount of Cry-Con grease
was placed in a 4.536 g copper sample holder whose specific
heat has been measured previously. At 0.6 K, the heat
capacity due to the Cry-Con grease was ~ 3.6% of the total
(Cry-Con + copper sample holder + addenda of the calori.
30
'7
v
?
i-
.-
Cry - con //
0'06 t ./~ /2
0"041 /'/ /'/"
~""¢P': /°
0 Or5 I0 r5 20 ..."/'"
,,d-
. j-*'-
,o.,,
I ~ J ~ n ~ in4 i 8 [
0 2 4 6 8 I0 12 16 I
Temperature, K
Fig. 1 Specific heat vs temperature for Cry-Con grease between
0.5 and 20 K. The solid line is a least squares fit of the data with a
5th-order polynomial
20
52
0011-2275/83/001052-03 $03.00 © 1983 Butterworth & Co (Publishers) Ltd.
CRYOGENICS. JANUARY 1983