RESEARCHAND TECHNICALNOTES

This paper reports on the measurement o f the specific heat o f Wakefield thermal
c o m p o u n d from 2 - 4 0 K

Specific heat of Wakefield thermal compound

from 2 to 40 K
J. Scott Payson and L.E. Wenger

K e y words: specific heat; Wakefield thermal c o m p o u n d ; thermal grease

0.8

Thermal greases are extensively used in this and other

laboratories to thermally anchor samples to substrates.
Using the same substrate repeatedly and knowing the heat
capacity of both the substrate and grease allows for
corrections to the measured heat capacity.
The specific heat of one type of thermal grease, Wakefield
thermal compound, 1 has been previously reported by
Bachmann, et al. 2 and Schwall 3 in the temperature range
of 1 to 10 K. More recently Cort and Naugle 4 have reported
on measurements from 20 to 100 K. In order to close the
gap between 10 and 20 K of these previous measurements,
we have measured the heat capacity of the Wakefield grease
between 2 and 40 K using an adiabatic heat-pulse method, s
An argon annealed copper (OFHC) cup was used as a
sample holder for the grease. The heat capacity of the
empty copper cup and substrate was first measured, then

iO-I

i i ( X IKo

eX o X X

o OX= oXQ tXe

eeeS

10-2

This work

Schwall
Bachmann etal

x Cort and Nougle

O0

10-4

10-5
0

I
I0

I
20

1
30

I
40

Temperoture, K

Fig. 1
40 K

Specific heat of Wakefield

thermal

compound from 2 to

The authors are at the Department of Physics Wayne State

University Detroit, MI 48202 USA. This research is supported in
part by the National Science Foundation (DMR 7921298) and the
Alfred P. Sloan Research Foundation. Paper received 23 July 1981.

44

0.6

S"

/.

3E

0.4

X
&

This work
V Schwall
Bachmonnetol

y
0.2

&

C = 00146 T 3

/
o
0

I
I0

I
20

I
30

I
40

I
50

[
60

70

Temperature 2 , K2
Fig. 2 Specific heat of Wakefield thermal compound from 2 to
7 K plotted as C/T vs T 2

i00

10-3

remeasured after adding 2 g of grease. Thus the difference in these two measurements is due to the heat
capacity of the grease. The specific heat results for the
Wakefield grease are shown in Figs 1 and 2 as well as the
previously reported results. An overall accuracy of 1% is
estimated at the lowest temperatures increasing to 2% at
the highest temperatures. The heat capacity of the grease
represents 40% of the total heat capacity at 4 K and 20%
of the total at 40 K.
In comparison to the prior results on the Wakefield thermal
compound, our results are ~ 10% above Bachmann, et al
and ~ 10% below those of Schwall, who suggests that this
difference may arise from different amounts of binder. 6
Above 25 K, our results are in excellent agreement with
those of Cort and Naugle although below 25 K these latest
results are slightly higher and outside the experimental
error. Note also at the lowest temperatures in Fig. 2 that
the specific heat still follows a T 3 temperature dependence
with no observable linear temperature dependence as is
typical of most amorphous systems at very low temperatures. 7

CRYOGENICS

. JANUARY

1982

The present data between 2 and 40 K have been represented

by least squares fitting the following polynomial,

Cp = Z

a n t n, mJ g-1 K-X,

References
1

Wakefield Engineering Co., Wakefield, Mass. 01880. The

thermal grease is part No. 120-2

Baehmann, R., DiSalvo, F.J. Jr., Geballe, T.H., Greene, R.L.,

Howard, R.E., King, C.N., Kirseh, H.C., Lee, K.N., Sehwall,
R.E., Thomas, H.U., Zubeek, R.B. Rev Sei [nstr 43 (1972)

?1=3

where a3 = 6.70640 x 10 -3 , a4 = 5.15072 x 10 -3,

as = - 1.09745 x 10-3,a6 = 1.01187 x 10 -4 ,
a 7 = - 5.13233 x 10-6,a8 = 1.49078 x 10 -7,
a 9 = - - 2.37950 x i 0 -9, alo = 1.69294 x 10 -11 . The
average deviation is approximately 1.3%, well within the
experimental error.

3
4
5
6
7

2O5
SchwaB,R.E. Ph.D. thesis (Stanford, 1973)) ), unpublished
Cort, B., Naugle, D.G. Cryogenics 21 (1981) 313
Payson, J.S., M.S. thesis (Wayne State, 1981), unpublished
In the present investigation, thermal compound used directly
from container with no binder
Zeller, R.C., Pohl, R.O. Phys Rev B 4 (1971) 2029; Stephens,
R.B.,Phys Rev B 8 (1973) 2896

The presence o f a few tenths mol % hefium in hydrogen causes anomalous vapour pressures
as high as 10 kPa. This effect is caused by the combination o f a small cold cell, a single,
long fill tube, and the insolubility o f helium in liquid hydrogen. This effect is important
in the handling of deuterium-tritium, as radioactive decay produces He 3.

Anomalous vapour pressure over liquid D-T

P. Clark Souers, E.M. Fearon, R.K. Stump and R.T. Tsugawa

Key words: cryogenic; deuterium - tritium; vapour pressure

Cryogenic deuterium-tritinm (D-T) is of interest as a

possible fuel for magnetic or inertial confinement fusion.
Cryogenic D-T work :is bedeviled by liquid vapour pressures
that are higher than expected from the sensor temperatures.
This is attributed to either temperature gradients or to
excess He 3, the daughter formed by tritium d e c a y ) This is
accompanied by a He 3 blocking effect, which impedes the
loading o f the cryogenic cell with D-T. 2
The apparatus consists of a room temperature gas storage
vessel and a cold cell connected b y a long, thin tube. The
storage vessel has a volume of about 1700/~m 3 and its
temperature T t is 296 to 299K, -+ 0.5K in any given run.
A baratron is mounted next to the vessel to measure the
system pressure. The sample cell is small, with a volume
Vc of 0.371/~m 3. A germanium sensor, mounted inside
the copper wall of the sample cell, measures the temperature Te, which is set between 19 and 21K, + 0.05K. The
connecting tube has an average internal cross sectional
area of 1.2 x 10 -s m s, and its length varies from 1.7 to
4.5 m. Calibration with He 3 shows that the cold temperature extends about 35 mm up the connecting tube. The
apparatus is all stainless steel except for the sample cell,
which is copper and Kovar, with sapphire viewing ports.
The temperature and pressure calibration have been
previously described. 2 The H2 and D2 samples have known
quantities of He 3 a d d e d ; t h e D-T is stored until the desired
amount o f He 3 is present (production rate 0.015 tool %
The authors are with the Lawrence Livermore National Laboratory,
Livermore, California 94550, USA. This work was performed under
the auspices of the US Department of Energy under contract
W-7405-Eng-48. Paper received 31 July 1981.

CRYOGENICS

. JANUARY

1982

(day mol T)-I). After each run, the mixture is analyzed

with a high resolution magnetic sector mass spectrometer.
The gas mixture is admitted at 40 Pa and the pressure
measured by the spectrometer. The hydrogen is then
removed by a titanium sublimation pump to about 0.1 Pa.
The pressure of the remaining He 3 is measured by the mass
spectrometer, which has been calibrated with a He 3
standard. 3 We estimate the accuracy in determining the
amount of He 3 to be -+ 10%.
The sample gas is loaded into the storage vessel with the
valve closed, and the rest o f the system is cooled and
evacuated. The amount of sample gas is set so that, at
eventual equilibrium, the cell will be filled to the top
with liquid hydrogen. The appropriate liquid densities 1
and saturation vapour pressures 4 are required, and room
temperature chemical equilibrium is assumed.
At time zero, the valve is either fully or slightly opened.
The gas flows to the cell and liquefies. With the valve fully
open at time zero, the sensor temperature rises 0.3 to
0.8 K as the heat o f liquefaction is released. It stabilizes
exponentially with a time constant o f about 0.8 s. When
the valve is barely opened, the observed temperature rise
is 0.07 to 0.14 K.
The results of several He3-D2 runs are shown in Fig. 1. The
excess pressure is the pressure above the expected 20 K
saturation value. The pure D2 pressure (0% He 3) drops as
quickly as the cryostat can remove the heat of liquefaction.
The pressures of the other samples level off at higher
pressures which are proportional to the amount of He 3
initially present. We extrapolate each pressure plateau back
to time zero to obtain the pressure Pex. This plateau

45