Charcoalpumped 3He cryostats for storage Dewars

E. T. Swartz

Citation: Review of Scientific Instruments 58, 881 (1987); doi: 10.1063/1.1139596

View online: http://dx.doi.org/10.1063/1.1139596
View Table of Contents: http://scitation.aip.org/content/aip/journal/rsi/58/5?ver=pdfcov
Published by the AIP Publishing

Articles you may be interested in

Initial stages of Cu growth on ordered Al2O3 ultrathin films
J. Vac. Sci. Technol. A 14, 1662 (1996); 10.1116/1.580315

Interdiffusion and interfacial reaction between an YBa2Cu3O x thin film and substrates
Appl. Phys. Lett. 53, 1437 (1988); 10.1063/1.100460

Efficient 4He cryostats for storage Dewars

Rev. Sci. Instrum. 57, 2848 (1986); 10.1063/1.1139213

A Compact 3He Cryostat Using Activated Charcoal

Rev. Sci. Instrum. 42, 1265 (1971); 10.1063/1.1685364

Probe Cryostat to Fit He Supply Dewar

Rev. Sci. Instrum. 37, 640 (1966); 10.1063/1.1720271

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
 Charcoa.l .. pumped 3He cryostats for storage Dewa.rs
E. T. Swartz
Laboratory ofAtomic and Soltd State Physics. Cornell University, Ithaca, New York 14853-250]
(Received 30 October 1986; accepted for publication 26 January 1987)

We have designed a 3He cryostat which can be inserted into a storage Dewar. This cryostat
requires no external gas-handling system and has the advantages of extremely low (and
recoverable) helium consumption, fast cooldown and warm-up times, excellent temperature
range and stability, and low vibrational and electrical noise. The freedom from an external gas-
handling system allows for portability and flexibility in its uses. Design and construction of the
cryostat are presented, and operation and performance are discussed in some detail. To
demonstrate performance of the cryostat, we present thermal boundary resistance
measurements between 0.4 and 170 K for a solid-solid interface (Rh:Fe/sapphire).

INTRODUCTION and used. This allows the use of a small charge of 'He (about
1 STP liter). By permanently sealing the lHe system, the
Conventional 4He cryostats typically are permanently
chances of accidental leakage are very smaH, and the ]He can
mounted, require long times to cool to low temperature, and
be stored safely at moderately high pressure (10 atm). This,
require a costly and inefficient transfer of 4 He. Conventional
along with the fact that the amount of 3He in the system is
3He cryostats share these shortcomings, but in addition re-
small, allows the room temperature storage volume to be
quire a complex and expensive gas-handling system to con-
quite small (~ 100 cc).
tain the precious 3He without loss. Further, the need for
This cryostat has been used for calibrating thermom-
large pumps and pumping lines makes vibration isolation a
eters, measuring solid-solid thermal boundary resistances, 5
necessary and difficult task. In a previous publication, I we
and measuring heat capacity. The measurement of samples
presented a 4He cryostat which could be inserted into a stor-
of small heat capacity has been a very sensitive test of the
age Dewar. That cryostat will be referred to in this paper as
cryostat's capabilities. In addition, with its rapid turnaround
the 4He dipper. Some advantages of that cryostat are its
time and simplicity of operation, this cryostat is ideal for
quick cooldown and fast turnaround times, low and recover-
quick testing of components and samples. Because orits sim-
able helium consumption, and its size and portability. In this
plicity, size, low operating costs, and low initial cost, this
publication, we present a 3He cryostat which has all the ad-
cryostat should make .1He temperatures accessible for the
vantages of the 4He dipper, and is almost as simple to use.
first time to many laboratories. Cryostats of this design can
This cryostat requires no external gas-handling system, no
be purchased from RMC, Inc. 6
large pumping lines, no transfer of helium, and it is equally
In Sec. I we will describe the principles of design and
small and portable.
operation of the cryostat. In Sees. II and HI, we will discuss
The use of activated charcoal to pump the 3He elimi-
the activated charcoal pump configuration, temperature
nates the problem of the complex pumping system 2 -4 em-
control of the cryostat, and the performance that can be ex-
ployed by conventional 3He cryostats. However, using a
pected. In Sec. IV, we will discuss some of the details of the
charcoal pump introduces the problem of how to desorb the
design of the cryostat. To demonstrate the performance of
.1He after it has been completely adsorbed by the charcoal.
the cryostat, we will briefly discuss thermal boundary resis-
The crux of the problem has been that keeping the tempera-
tances in Sec. V, present our techniques for performing ther-
ture of the charcoal as low as possible during adsorption
mal boundary resistance measurements, and show some rep-
requires a close thermal contact to the "He bath, but this
resentative data.
strong link makes it difficult to heat the charcoal hot enough
( ~ 25 K) for desorption without using several watts of heat.
I. PRINCIPLES OF DESIGN AND OPERATION
We have found it way not only to provide the necessary
strong thermal anchor of the charcoal to 4.2 K, but also to The basic principle of operation of a 3He cryostat is es-
heat the charcoal to desorption temperature with only about sentially the same as operating a 4He cryostat, in two stages.
0.1 W. Shown in Fig. 1 is a cutaway view of the cold end of the
Storing the 3He at room temperature (when a conven- cryostat. The first stage is a continuously fitled 4He pot
tional 3He cryostat is not in operation), even when a char- which cools to about 1,5 K. This stage is kept at 1.5 K con-
coal pumping scheme is employed, typically necessitates a tinuously while the cryostat is operating below 4 K. The
large storage container. Our charcoal pump occupies a very continuously filled 4He pot in the "He dipper is essentially
small volume, very close to the 3He pot, so that it will fit into identical in both geometry and operation to the continuously
a storage Dewar where there is limited space. We have also filled 4He pot which is the first stage of this 'He cryostat. A
eliminated much ofthe dead volume in the pumping system, smallliquid-nitrogen-trapped mechanical roughing pump is
so that a large fraction of the available 'He can be condensed sufficient for pumping on the 4He pot. (This trapping is

881 Rev. Sci. Instrum. 58 (5), May 1987 0034-6148/87/0508S1"()9$Ol.30 @ 1987 American institute of Physics 881

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224
.••• -•••.• ,. •••• ,.•".-.; •.••••••••••-.-.;.; •.•••, ••••• ,..'•. <.;.;.; •• ' •••••' •••••••••;•.•••,......... ,.•.•-.,.; •• ' ••••• ' •••••••••••. ' .... , •.•••.•-,-••.•• ' •••••••••.•;.; •.•,.•••• , ••••. ,:.:.;;>;•• '. On: Mon, 24 Nov 2014 21:12:02
 as those for the continuously filled 4He cryostat in the 4He
OUTER CHARCOAL dipper. After a sample is mounted in the cryostat, a radiation
VACUUM ----VOLUME shield and a vacuum can are installed. The vacuum can is
CANFOR~ evacuated and the cryostat is precooled in liquid nitrogen.
PUMP I ISOTHERMAL
POSTS Then the cryostat is gradually lowered into a storage Dewar
over a 20-min. period until the bottom of the vacuum can lies
PUMP
II PUMP
just above the bottom of the Dewar. For operation of the
SWITCH
HEATER I cryostat below 4.2 K, it is necessary for the helium level in
4.2 K I VACUUM CAN the Dewar to reach at least the top of the 4.2 K baffles (see
BAFFLES 1"'1'AND 4 He POT Fig. 1). The helium boil-off of the Dewar with the cryostat in
PUMP TUBES
WIRE place will not be significantly greater than the normal 2 1 per
FEED- day boil-off without the cryostat, except during operation of
THROUGHS TAPERED
-GREASE the cryostat above several tens of Kelvin. Therefore, the
THERMAL
SEAL cryostat can be operated below 4 K for over a week if a full
ANCHOR
60-1 storage Dewar is used. Then the experimentation above
POSTS FOR
WIRING 4 K can be done with the level below the top of the 4.2 K
3He
CONDENSING
baffles. Use of the cryostat inside the storage Dewar at a
4He POT
SURFACE
temperature as high as 150 K is routine, and by following the
WIRING
same procedure as for the 4He dipper, data can be taken with
FEEDTHROUGH the cryostat up to room temperature.
TUBES Shown in Fig. 2 is the top end of the cryostat. Note that
BRASS the mounting post for the 3He storage volume is for physical
THERMAL support only; it does not connect the two vacuum spaces. The
LINK 3He storage volume is connected directly via a lkin.-o.d. 304
stainless-steel tube to the 3He pump. The vacuum seals
SAMPLE
between the tubes and the aluminum manifold are made by
MOUNT
silver soldering the tubes into pipe fittings and screwing the
- 1 CM ------"" 1 INC H pipe fittings into the tapped aluminum with Stycast 1266
epoxy in the threads. This provides a strong and reliable
joint. The vacuum can and pumping tubes for the 4He pot are
FIG. 1. Cutaway view of the low-temperature section of the cryostat. The
vacuum can and radiation shield are not shown, but are identical to those of arranged coaxially so that a single quick-connect coupling
the "He dipper. All material is copper except the thin-walled tubing, and can be used to make a sliding seal between the tubes and the
where noted. The clearance between the charcoal can and the outer call for flange that mates to the top of the storage Dewar. (The
the pump is 0.015 mils (0.38 mm).
cryostat requires a 2-in.-diam neck-size Dewar.) The two
pumping tubes are split before they connect to the lower
portion of the cryostat.
The electrical feedthroughs and wiring procedures for
needed only to keep pump oil from condensing in the cryos- this cryostat are again the same as for the 4He dipper. We use
tat. We suspect a molecular sieve trap would also suffice, two 19 pin hermetically sealed feedthroughs 7 for most of our
although we have not checked this.) The second stage is a needs, and several vacuum feedthrough BNC connectors
3He pot which, in principle, operates in the same way as the can also easily be installed. The wires are fed through the
first stage, but is not continuously filled. The most important pumping tube for the vacuum can and are carefully thermal-
purpose of the 4He pot is to generate a temperature low ly anchored to 4.2 K using the thermal anchor posts for
enough for 3He to condense. The pumping tube for the 'He wiring shown in Fig. 1. The wires are thermally anchored to
pot is anchored to the 4He pot so that when 3He is introduced the 4He pot, and finally are anchored to the 3He pot and fed
into the pumping tube (at a pressure greater than the satu- through the wiring feedthrough tubes to the temperature-
rated vapor pressure of 1He at the temperature of the 4He control platform. Several inches of extra length of the wires
pot), the 3Re will condense on the walls of the pump tube should be left between the 4.2 K anchor posts and the 4He
and drip into the 3Re pot. In order to facilitate this, the 'He pot, and between the "He pot and the 3He pot. We use 40-
pumping tube inside the "He pot is made of copper and is gauge (75 fl diameter) Constantan wires (30 n per foot) as
tapped (i-28) to increase surface area. The effect of the con- much as possible, and 36- or 32-gauge ( 125 and 200 f-t diame-
densation and dripping is not only to provide liquid, but also ter, respectively) Constantan (~11 and ~ 3 n per foot, re-
to speed the cooling of the 'He pot to the temperature of the spectively) when higher currents may be necessary. If coax-
4He pot. This is analagous to the cooling mechanism for the ialleads are needed, we recommend that at least between the
4He pot in the 4He dipper resulting from 4He condensing on 4He pot and the 3He pot the coax be as fine and resistive as
the 4.2 K walls of the pumping tubes for the 4He pot and possible (i.e., fine, braided stainless-steel coax), and that
dripping into the 4He pot. very careful consideration to thermal anchoring be given.
The general layout of the cryostat and the general (The coaxial leads will need to be split open and both con-
mounting and cooldown procedures are essentially the same ductors separately thermally anchored.) In general, the per-

882 Rev. Sci. Instrum., Vol. 56, No.5, May 1987 Cryostats 882

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02

-1INCK
-1CM
FlG. 2. Cutaway view of the upper section of cryostat. Please note that the
tube between the -'He storage volume and the pumping tube for the vacuum
can is for support only. and does not connect the two volumes. The manifold
block (lightly stippled region) is aluminum, the 'He storage volume and
tubes (heavy lines and darkly stippled regions) are stainless steel. and all
the fittings (cross hatched) arc brass. Stainless to stainless joints are weld-
ed, brass to brass and brass to stainle,s joints are silver soldered, and brass to
alurninumjoints are threaded and epoxied. The electrical feedthrough con-
nector is soft soldered to a flange which is sealed with an G-ring to the mani-
fold block. and the sliding seal between the :J-in.-diam tube and the storage
Dewar uses a Viton G-ring in a quickconnect (Nupro Ultratorr or equiva-
lent). The pump port tlanges are brass KF-16 Klein flanges, which directly
connect to many A-in. vacuum valveso The second tube in the top of the 'He
storage volume is for the initial pump-out and filling, and a third tubc can be
added if a pressure sensor is desired.
formance of the cryostat is very strongly affected by the type
of wire used and the care taken to thermally anchor them.
II. CHARCOAL SORPTION PUMP
Cooling of the~He pot to 0.35 K is achieved by pumping
the 3He back into the activated charcoal pump. The configu-
ration of the pumping system is the most critical part of the
cryostat. The pumping capacity and pressure versus tem-
perature characteristics of activated charcoal, as well as oth-
er relevant information including another "'He cryostat de-
sign, have been published by Channin and Torre. 3
Adsorption curves have been measured by Hoffman, Edes-
kuty, and Hamme!.); The operation of the pump is most easi-
ly understood by following through a cycle of adsorption
and desorption. To desorb 3He from the charcoal, about 100
m Ware applied to the pump heater (a 400-H Allen-Bradley
883 Rev. Sci.rnstrum., Vol. 58, No.5, May 1987
This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
resistor,9 which also serves to monitor the temperature of the
pump). Since the pump is surrounded by an evacuated can
(labeled outer vacuum can for pump in Fig. 1), this small
power is enough to rapidly raise the temperature to over 25
K. The 3He leaves the pump through the thin wall stainless
pumping tube to the 4.2 K baffles, where its temperature
drops to about 4.2 K. The 3He continues through another
thin wall stainless pumping tube to the 3He condensing sur-
face in the middle of the 4He pot, where it condenses (if the
pressure. is greater than the saturated vapor pressure of 3He
at the temperature of the 4He pot). The condensed 3He drips
into the -'He pot, first causing the 3He pot to cool and then
filling the 3He pot. Once the JHe stops condensing, which
will take about 20 minutes, the heat on the pump is removed
and the pump will cool and start pumping.
At this point, helium exchange gas is added to the ex-
change gas space between the pump and the outer vacuum
can for the pump to cool the pump faster. This is accom-
plished by heating the pump switch assembly, which is itself
a small charcoal sorption pump. (During desorption, the
switch assembly is kept cold, and thus it docs maintain the
needed vacuum for desorption, as assumed above.) With
about 5 m W of heat, the pump switch is designed to desorb
on the order of a Torr of 4He gas (the exchange gas space is
initially fined to 100 Torr at room temperature). The gap
between the wall of the charcoal container and the wall ofthe
outer vacuum can for the pump is designed to be as small as
possible, about 15 mils (0.38 mm), so that the exchange gas
will be as efficient as possible. With this setup, the pump
cools very quickly and starts to adsorb 3He gas within about
a minute. Within about 5 min, the temperature of 3He pot in
our cryostat cools to about 0.301 K. One way to gauge the
performance of the charcoal pump in our cryostat is to note
that 0.301 K corresponds to a pressure over the 3He of about
2 X 10. 03 Torr.
The temperature of the charcoal near the walls of the
container is close to the temperature of the walls, but since
charcoal is a poor thermal conductor, when the pressure of
the 3He in the charcoal container is low, the heat of adsorp-
tion of the 3He will cause large temperature gradients in the
charcoal. This effect is minimized by putting isothermal
posts inside the charcoal container to reduce the mean dis-
tance between any point in the container and a cold surface.
Note that if the pump switch were not heated, the pump
would cool more slowly, and would remain at a somewhat
higher temperature. This would cause the pumping speed of
the pump to be reduced, and thus the temperature of the 3He
pot would not be as low as it would be if the pump switch
were heated. We will discuss this further and show how con-
trolling the temperature of the pump and of the pump switch
can be used to coarsely control the temperature of the 3He
pot.
III. TEMPERATURE CONTROL
A. Below 1.5 K
Once the 4He pot is stable at about 1.5 K and the 3He is
condensed in the 3He pot, the 3He pot is ready to operate. We
find it convenient when taking data over a broad range of
temperature to stabilize at successive temperatures as the
Cryostats 883
 cryostat cools. This procedure uses the 3He most efficiently. the power heating the pump, one can adjust the amount of
Three heaters are used for temperature control: the heater on power that the temperature controller supplies. Ideally, the
the pump (the pump heater), the heater on the heat switch pump heater should be adjusted until the temperature con-
pump (the switch heater), and the heater on the experiment trol heater uses less than 0.05 m W to control the tempera-
stage (the temperature control heater). We assume that the ture. After the data are taken at 1.25 K, set the temperature
temperature control heater is controlled by a three-term controller to the next lower temperature. Then decrease the
(proportional, integral, and differential (PIO) I tempera- power in the pump heater to allow the pump to cool and to
ture controller. The pump heater and switch heater are 400- increase its pumping speed. This will cause the cryostat to
n Allen-Bradley carbon resistors, and the temperature con- cool, and the above temperature control process is repeated.
trol heater is a wire-wound 400-.0 heater. Just at the Below about 0.8 K, heating the switch heater becomes
completion of the condensation ofthe 3He in the 3He pot, the necessary in order to cool the pump more quickly and thus
states of the heaters are as follows: the pump heater is on at increase the pumping speed. To control the temperature at
maximum power ( 100mW), the switch heater is off, and the 0.8 K, about 0.25 m W should be applied to the switch heater.
temperature control heater is off. Table I is a collection of With this power, a small fraction of the available exchange
representative values of heater powers that are recommend- gas will be emitted into the exchange gas volume. The ex-
ed as a guide for temperature control. They will, of course, change gas will transfer heat between the pump and the wall
vary from cryostat to cryostat depending on the design and of the vacuum can for the pump, cooling it enough that
wiring of the cryostats, and the heat load from the experi- about 8 mW must be applied to the pump heater to keep the
ment. pump at the temperature needed to allow temperature con-
To control the temperature at 1.25 K, set the tempera- trol of the lHe pot at 0.8 K. The power applied to the switch
ture controller at 1.25 K. (The temperature controller will is not criticaL The switch heater power should be high
not apply any heat until the cryostat temperature drops be- enough so that the pump will cool sufficiently, but not so
low 1.25 K.) Then reduce the heat in the pump heater to high that several tens of m Ware needed on the pump heater
about 10 mW, and the pump will start cooling very slowly. to control the pumping speed. This procedure works for all
The temperature of the 3He pot should then start to fall. temperatures below 0.8 K.
When it drops below 1.25 K, the temperature controller will To cool to the lowest temperature possible, about 0.30
start to apply heat, and the temperature will quickly stabi- K, the procedure is to heat the switch only; about 1 m W is
lize. Set the temperature controller so that its maximum cur- sufficient. The temperature will drift, though, unless the
rent is no more that 2 mA, so that it cannot accidentally boil temperature controller is used and the temperature is con-
away the liquid too quickly. If the temperature does not drop trolled at least a few mK above the lowest temperature. The
to 1.25 K, reduce the heat in the pump heater so the pump magnitude of the temperature fluctuations of the uncon-
will cool and pump more quickly. If the temperature con- trolled, unloaded cryostat at the lowest temperature is about
troller uses nearly the maximum output to maintain 1.25 K, 0.1 mK with a characteristic time scale of a minute. In addi-
or if the maximum power from the temperature controller is tion to these short-term fluctuations is a very slow long-term
insufficient, increase the power in the pump heater so that warming trend of about 5 mK per 10 h presumably due to the
the pumping speed is reduced. Thus by manually controlling charcoal changing its pumping properties as it fins.
Although there are three heaters used to control the
temperature, and what seems initially to be a complicated
TABLE 1. Temperature control parameters. These values are meant only as a control algorithm, the above procedure can be mastered in
guide, as they can vary from cryostat to cryostat and even from application
one afternoon. There are faster algorithms for changing tem-
to application in the same cryostat.
peratures and stabilizing at the new temperature. These in-
Temperature Controller Pump heater Switch heater 4Hepot volve overcooling the pump to initiate a fastcr 3He pot cool-
of 3 Hepot power (mW) power (mW) power (mW) temperature down and then warming the pump back to the proper
temperature as the lIfe pot approaches its desired tempera-
cooldown off off off cooling
regeneration off 100 0 min (-1.5) ture. (This is analagous to critical damping in second order
1.25 <0.1 10.0 0 min control theory. to) Because the thermal time constants of the
1.12 <0.1 8.0 0 min pump and switch are several seconds, some anticipation is
1.00 <G.! 5.0 0 min needed in this case. With some practice, we have been able to
0.90 <G.OS 3.0 () min
0.80 <0.05 8.0 0.25 min change temperature and stabilize at a new temperature in
0.70 <0.05 5.0 0.25 min less than a minute.
0.60 <0.01 3.0 0.25 min With a properly designed PID temperature controller,
0.50 <0.01 3.0 0.50 min
temperature stability to a few,uK can be achieved. Our tem-
0.40 <0.01 1.0 0.50 min
min (-0.30) <0.005 0 1.0 min perature control scheme uses carbon resistors as thermom-
1.50 <0.2 50 0 1.48 eters, a three-lead bridge and lock-in amplifier to read the
1.75 <0.2 50 0 1.73 thermometer and produce an error signal, and a homemade
2.00 <0.2 50 0 1.98
analog PIO controller (the Piddiddler, originally designed
2.25-\0 As needed 0 1.0 min
1(}-lOO As needed 0 1.0 Floating by David McQueeney at Cornell]! ), to convert the error
Alt: 8-60 As needed 5.0 0 4.2 signal into the appropriate heater level.
Manual control of the pump and switch heater is not

884 Rev. Sci.lnstrum., Vol. 58, No.5, May 1987 Cryostats 884

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
 much of a burden, but for those with less patience, it could be
easily computer controlled. In Fig. 3 is the schematic for
both simple heater circuits, including the option of control-
ling the output with a O-lO-V signal (this provides a simple
method for computer control). I would suggest an algorithm
be designed so that the computer can conservatively use the
above shortcut to maximize effective running time.
B. Between 1.5 and 2 K
For temperatures above 1.5 K, it is no longer necessary
to pump 011 the .lHe pot, On the other hand, with no 'He in
the 3He pot and in its pumping tube, the temperature of the
3He pot can drift significantly above the temperature of the
4He pot since the thermal link between the two pots is very
weak-a thin-walled stainless-steel tube. Therefore, tem-
perature control at temperatures between 1.5 and 2.0 K can
be tricky. We have found that the best way to achieve a stable
temperature is to desorb all the 3He gas from the pump and
keep the pump hot enough so that it does not start pumping
(30 mW should suffice). The 3He pot will then be full and
locked to the temperature of the 4He pot. The temperature of
the 4He pot is controlled by varying the speed at which it is
pumped. Then the temperature of the temperature control
stage is controlled at about 20 mK higher than the tempera-
ture of the 3He pot. This is made possible by the use of the
brass thermal link between the 3He pot and the temperature
control stage. If a much larger temperature difference
between the temperature control stage and the lHe pot is
imposed, the 3He pot temperature will also rise significantly
and temperature instabilities will result. This is caused by
discrete drops of 3 He at the temperature of the 4He pot drip-
ping into the 3He pot.
There is a vast parameter space that we have not yet
explored that may allow even better temperature control
between 1.5 and 2.0 K than we have been able to achieve.
Co Above:2 K
Above 2 K, temperature control with our 3He cryostat
design is very simple. Between 2 and 10 K, the .tHe pot and
the pump are kept as cold as possible; all of the 3He is in the
pump. Then the temperature controller is used to raise the
temperature of the 3He pot to the appropriate temperature_
The relevant thermal iink in this regime is the thin wall stain-
less-steel tube between the 3He pot and the 4He pot, and since
this is a weak link, only very little power is needed to control
the temperature. We recommend that the 4He pot be kept at
1.5 K for temperature control below 10 K, as this seems to
work best, although in principle the 4He pot need not be
pumped when controlling above 6 K. Above 10K, pumping
the 4He pot is no longer necessary. Other than that, tempera-
ture control is as below 10 K. (Also, above 10 K, tempera-
ture control is achieved in the same way as in the 4He dip-
per). With this procedure, temperatures as high as lOOK are
easily reached. Temperatures up to 300 K can also be
reached using the procedures outlined for the 4He dipper.
Note that because the stainless-steel tube between the
-'He pot and the 4He pot is a weak thermal link, temperature
control is easy above 2 K, but the maximum allowed heat
load is small. Above 8 K, there is a trick which can be used to
increase the available cooling power. To use this, do not

05J
it--.
: ~
R1
,__t ___ ~

FIG. 3. Electrical schematic for the current sources driving the -'He pump heater and the switch pump heater. Due to the temperature dependence of the
resistance of the heater resistors RL, ( 400-H Allen-Bradley resistors) , a current source is superior to a voltage source. (The temperature dependence of the
resistance provides some negative feedback if the resistors are driven with constant current and positivefeedback if they lIre driven with a constant voltllgC.)
The transistor is a 2N3905. For the mekr selection switch, the top position reads the voltage across the heater, the lower positioll rcads the voltage across the
series resistor to deduce accurately the current, and the center position is off, the suggested idle state of the switch. The switch on the left selects between
manual operation (upper position) or computer controlled with a 0--10- Y digital-to-analog converter. For computer-controlled operation, the helipoi R2
should be at maximum resistance. Fa> the 'He pump heater, the values of the resistors are Rl = 40 kn, and R2 = 0-5 kn helipot, R3 ~c 100 n. For the
switch heater, the values oftne resistors are Rl = 30 kO, and R2 =, 0-20 k!1 helipot, R3 ~" 1000 n. The two current sources can be mounted in the same box
with a common power supply.

885 Rev. Sci.lnstrum., Vol. 58, No.5, May 1981 Cryostats 885

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
 pump on the ~He pot, and heat the charcoal pump just
enough (~5 mW) to introduce a few Torr of iHe gas into
the pumping tube for the 'He pot. Since no temperature seen
by the 3He is below its vaporization point, it cannot drip and
cause temperature instabilities. The only effect of a few Torr
of :'He exchange gas is to increase the thermal link between
the 'He pot and the 4He pot, thus significantly increasing the
cooling power. With this trick, the temperature can be con-
trolled easily to 60 K with increased cooling power.
Another trick which we do not suggest for routine use,
and which would be acceptable only for some types of ex-
periments, is to introduce 4He exchange gas into the vacuum
can. This obviously increases the thermal contact to the 4.2
K 4He bath. By pumping the gas out in a controlled manner,
the amount of thermal conduction by the exchange gas can
be controlled over a wide range. \Ve have used this technique
when measuring thermal boundary resistance, and have
been able to temperature control at 10 K with as much as a
25-m W heat load, and at 40 K with a heat load up to 100
mW. The problems with this approach arc that removing all
of the exchange gas is difficult without heating the entire
cryostat to room temperature, and that the thermal conduc-
tion due to the gas may also directly a1Iect some experi-
ments.
D. Hold times and cooling capacity
The cryostat contains a charge of about 1.1 STP liters, a
little over 1.5 cm 3 ofliquid. That is enough to absorb ahout 1
J of heat before regeneration is needed. Several parameters
affect the amount of time the cryostat will remain cold, in-
duding residual heat leak to the 'He pot, temperature con-
trol power, power input to the experiment, and to a smaller
extent, the temperature of the 'He pot. The residual heat
leak to our cryostat is dominated by the pump tube, and is
just under 10 Jl W. The most common sources of unnecessary
heat leaks are electrical ground loops and improperly ther-
mally grounded electrical leads.
When left unloaded and uncontrolled, our cryostat has
remained cold (below 0.31 K) for over 24 h. With a constant
load of 100ft W, the "He charge lasted about 21 h. Assuming
an additional residual heat leak of 10 ,U W, this corresponds
to a usable energy absorption of about 0.8 J, indicating that
almost an of the 3He has been condensed.
The temperature versus heat load characteristics ofthe
cryostat are adjustable. We need only very little cooling for
our experiments, so to facilitate temperature control, we
have arranged for the temperature control stage to be weakly
linked to the 3He pot. The weak link, as mentioned before is
the brass post between the stage and the pot. At 0.3 K the
thermal resistance of the brass is about 5 mK per pW, and
that is what dominates the load characteristics of the cryos-
tat. At higher loads, 100 f-t Won the stage raises the tempera-
ture of the stage to about 0.63 K. Again, almost all of that
temperature rise is due to the temperature gradient in the
brass.
If a larger heat dissipation capacity is required, either
the brass link can be replaced with a copper link, or copper
braids can be used to reduce the thermal resistance between
the stage and the pot. The latter procedure allows a tuning of
886 Rev. SCi.lnstrum., Vol. 58, No.5, May 1987
This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
the cooling power, which allows for the most efficient and
convenient temperature control. With the solid copper link,
at 0.3 K the stage temperature will rise about 0.3 mK per
pW; this is the same as the temperature rise of thelHe pot
itself, independent of the thermal link between the pot and
the stage.
With the present design, if the brass thermal link were
replaced by solid copper, the Kapitza resistance would be
the dominant factor in determining the temperature of the
stage for a given power input. The area inside the 'He pot
available for thermal transport between the liquid and the
copper is about 30 cm? A Kapitza resistance of 160 T- l
K 4 /(W /cm 2 ) at 0.3 K would cause about 0.2 mK tempera-
ture rise per ft W of power input, within the usual factor of 2
or 3 variation in the Kapitza resistance. We do not know
how much better one could do by increasing the area inside
the 3He pot because we do not know precisely the character-
istics of the charcoal pump. Its pumping speed is a function
of the temperature of the charcoal, which is a complicated
function of geometry, heat load due to adsorption, and pres-
sure. The impedance of the pumping tubes would eventually
become the dominant factor in determining the temperature
versus load characteristics of the cryostat if some sinter were
added to the 3He pot, and if the pump were laced with iso-
thermal surfaces, or if the bath temperature were lowered.
Such optimization would have limited usefulness in a cryos-
tat with such a small 3He charge, and we have not pursued it,
IV. DESIGN DETAILS
In this section, we will try to explain some of the less
obvious design details. We strongly recommend following
the general guidelines discussed for the 'iHe dipper that per-
tain to using silver solder joints whenever possible, and using
soft solder joints to promote modularity between subsections
of the cryostat. We use soft solder joints to connect the
pumping tubes at the points marked in Fig. 4, to connect the
iHe pot to the -1He pot, and to connect the 4He pot to the top
of the vacuum can. Soft solder is used to connect the vacuum
taper seals to the vacuum can and vacuum can top. This is
done hecause these seals can be damaged by an impact to the
vacuum can, and then it would be convenient to be able to
replace them without major disassembly. Some soft solder
joints are needed to finish the charcoal pump assemblies be-
cause thc heat required by the silver solder would damage
the wiring of the pump and switch heaters. All other joints
are either welded or silver soldered.
Figure 4 is a drawing of the pumping tubes connecting
the top to the bottom of the cryostat. We have tried many
geometries for the pumping tubes, and have found the geom-
etry in Fig. 4 to be the best. Some of the considerations in-
volved in the design are the following:
( 1) Making a reliable sliding vacuum seal to one tube is
easier than to two. PreviouslHe cryostat designs utilized
two parallel tubes for the ~He pot pump tube and the vacuum
can pump tube. By making these tubes coaxial, only one seal
to the storage Dewar is necessary.
(2) The pumping tube for the 4He pot must directly
contact the 4He bath in the storage Dewar. Therefore, the
above coaxial tubes must be separated above the vacuum
Cryostats 886
 can. (If the pumping tube for the "He pot is pressurized, 4He 1/2
will condense on the walls of the tube and drip into the "He
pot, but only if the tube is in direct contact with the bath.)
(3) Enough room must be available to easily feed the
cryostat wiring through the pumping tube for the vacuum
can.
The layout of the tubes in Fig. 4 is quite complex, and
merits a careful explanation. The left view has the same ori-
entation as Fig. 1, and shows the general layout. This view
cannot show all the tubes because many are hidden; the two
side views are included to show the details of the large and .- - 1
~
small tubes. The small tubes are shown as solid heavy lines,
I
'
. B'
except where they are inside the pump assembly: in this case ., '(COPPER)
they are outlined. Tube A is the 'He fill tube. Tube A' con-

'
A'
nects to tube A and together they connect the IRe storage
volume (in Fig. 2) to the 4.2 K baffles in the ~He system.
Thus, the tubes A and A' are used to supply the IHe and to ,,

I
initially evacuate the -'He system. Tube B connects to the ,,
vacuum space between the charcoa1 pump and the outer .,

~:
vacuum can for the pump (the exchange gas volume), and is
used to evacuate the exchange gas volume and 10 supply the
I
I~:
jr:.itial charge of exchange gas. Once this is done, tube B is

"II
permanently scaled at the location marked S. To do this, ,
,,
tube B is connected to a copper tube, marked B', and B' is L __

sealed by crimping and then soft soldering over the crimp for , -~ --It:
mcchanil.:al support. Tube C is a brass feedthrough tube for I~
the continuous fill impedance capillary. (This is described in / 1\ - c
Ref. 1.) Brass is used so that reliable and easily replaceable I ( 1/15

joints to the fill impedance capillary can be made. As with

the 'He dipper, there are two options for continuous filling.
U .016
BRASS
(C)
Either the fill impedance is terminated just above the vacu- J - - - --; ~K-----I

um can, in which case the 4He is drawn from the storage
Dewar; or the tuhe C is connected to the tube C', which
extends outside the top oftlle cryostat and can connect to an
external supply of pure helium. When thelHc is drawn from
the Dewar, tube C' is carped as in Fig. 4. In the side vicw of
the larger tubes, the tube on the left is the pumping tube for
the .jHe pot and the lube on the right is the pumping tube for
vacuum can. This is the tube which must contain all the
wiring.
The ability to measure the pressure in the 3He system is
not absolutely necessary, but it is convenient when looking
for problems or establishing algorithms for temperature con-
trol and regeneration. Measuring the pressure at tht;'He pot
directly is not necessary, therefore, the pressure sensor can
be mounted wherever is most convenient 'we suggest that a
third capillary can be put in the top of the1He storage vol-
ume in Fig. 2, and a capacitive pressure sensor be connected
to this capillary. The use of a capacitive pressure sensor is
superior to a Bourdon gauge because a single capacitive sen-
sor can be made to read accurately over a broad range of
pressures, from fractions of a Torr to tens of atmospheres.
These sensors are also small, light, and reliable. A discussion
of capacitive pressure sensors call be found in Cornell's low-
tcmpemture techniques book. 12
V. THERMAL BOUNDARY RESISTANCE
MEASUREMENTS
In order to test the cryostat and provc performance,
thermal boundary resistance measurements were performed
1 in. ~ em.
FIG. 4. Tuhing details, ~howing tubing sizes and connections. The front
view (on the kit) ,hows the gt,nemllayout, while the side views' (center and
right) show the larger and smaller tuhes, respectively. The pump assembly
is outlined with dashed lines for reference. In the labels, upper dimensions
represent outer diamcteno, and lower dimensions represent w~t!l thicknesses
of the tube, in inches. Except where noted, all joints are soft soldered and all
tubes are 304 stainless steel. The lwo short I~-in.-diam tubes (between the
pump assembly and the bottom of the ::-in.-diam tube) are for mechanical
support only. The cryostat can be separated by disconnecting the soft solder
joints. between tubes shown in this figure. The lower l\,-in.-diam brass tube is
a fcedthrough for the continuous fill impedance, as with the 'Ht' dipper. For
ddails, see the text.
in the cryostat. A thermal boundary resistance is the resis-
tance to heat flow caused by the presence of an interface
between two materials. The classic example of a thermal
boundary resistance is the Kapitza Resistance (the thermal
boundary resistance between helium and a solid) first ob-
served by Kapitza,13 and 111'st explained by Khalatnikov. 1,1
Thermal boundary resistances typically have been measured
only below a few Kelvin, because they decrease roughly as
T- 3 with increasing temperature, thus becoming very small
above a few K relative to the thermal resistance in the bulk
materials on dther side of the interface.
Conventionally, measurement of the thermal boundary
resistance betvveen two solids has been done using an experi-

887 Rev. ScI. Im,trum., Vol. 51.!, No.5, May 1987 Cryostats S81

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
 mental geometry similar to the geometry used for measuring
r-~- --~-~~ em --~- - -,
thermal conductivity, as shown in the upper corner of Fig. 5.
The temperatures on the two sides of the interface are ex-
trapolated to the interface, and the boundary resistance is
defined as
Rbd = f1T I(Q IA),
where Q /.1 is the power per unit area flowing through the
interface, and 111' is the temperature drop at the interface.
Because of the large area of the interface in the conventional
geometry, a large heat flux is required to produce a measura-
ble temperature discontinuity; for example, at 100 K well
over a kilowatt is typically required to produce a 1 K tem-
perature discontinuity across a l-cm 2 interface. Thus, in or-
der to measure the boundary resistance at such a high tem-
perature, much smaller interfacial areas are required. The
conventional geometry also suffers from the problem oftem-
perature gradients in the bulk leading to uncertainties in the
temperature drop at the interface. The solution is to put the
thermometers as close to the interface as possible.
Our geometry is schematically shown in Fig. 5. The
FIG. 5. Geometries for measuring the thermal boundary resistance. In the thermometers are photolithographicaUy produced narrow
upper left-hand corner is the conventional geometry. In the upper right- lines of vapor-deposited thin metal films. The relevant inter-
hand view, the two thermometer lines are shown separated for clarity; on face is that between one of the thermometers and the sub-
this scale, the two lines would not be resolvable. Note the difference in the
characteristic dimensions, between the conventional geometry and our ge- strate (sapphire). The experiment is equivalent to measur-
ometry. ing the self-heating of that thermometer, using the second
thermometer to measure the temperature of the substrate.
Because the areas ofthe thermometers are typically less than
10- ~ em" and the separation of the thermometers is only a
few microns, the temperature drop at the interface is large
compared to the temperature drop in the bulk even near
room temperature. At temperatures below about 70 K, the
bulk temperature drop is negligible relative to the tempera-
ture drop at the interface, and below 170 K, the bulk tem-
perature drop can be easily subtracted without introducing
!J U 0 Pin Holder error. For more details, see Ref. 5, and future publications. 15
--
--~-~"~

Copper Our actual experimental geometry is shown in Fig. 6.

The sample holder is designed to mount to either the 3He

. ~ 5);. :::~:i~e
~~ Substrate
cryostat or the "He dipper. Three pairs of thermometers (or
two sets of three thermometers), are patterned onto each
substrate. (The third line would be to determine the tem-
perature gradients in the substrate to verify the calcula-
Sapphire
Table
tions.) The substrate fits into the sample holder; the 24 elec-

Location
Posts
FIG. 7. Thermal boundary re-
sistance between Rh:Fe and
sapphire plotted on a log-log
scale from 0.4 to i 70 K. The
Rh:Fe is an alloy of 99.5
at. r:!,) Rh and 0.5 at. % Fe,
used becallse of its favorable
temperature-sensitive electri-
1-------1 ~--1
1 in. 1 em cal resistivity over the entire
temperature range. The solid
FIG. 6. Sample holder and sample used for the thermal boundary resistance curve is the prediction of the
measurements. At this scale, the thermometers on the sapphire substrate acoustic mismatch model,
arc not visible; the only visible features on the sample are the current and and the dashed curve is the
voltage pads to which the pins make electrical contact. The pins arc epoxied prediction of the diffuse mis-
into holes ultrasonically drilled into the sapphire pin holder. A piazon N- _ ~, _ _ _ _ 1.- _____ _
match model, as discllssed in
grease holds the sapphire substrate to the sapphire table and the sapphire ,OJ 10 1 I Ref. 5.
table to the copper basco lemp810ture in K

888 Rev. ScLlnstrum., Vol. 58, No.5, May 1987 Cryostats 888

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
 trica} contacts are made using spring loaded point
contacts. 16 In this way the samples can be quickly ex-
changed. Figure 7 shows the data for a Rh:Fe/sapphirc in-
terface from 0.4 to 170 K, plotted on a log-log scale, Note
the thermal boundary resistance spans over 6 orders of mag-
nitude, and has a T- 3 temperature dependence over almost
the whole temperature range. For a discussion of these data,
see Ref. 5.
ACKNOWLEDGMENTS
This work was supported by the Semiconductor Re-
search Corporation, Contract 82-11001. The author was
supported through a fellowship from the Fannie and John
Hertz Foundation. Photolithographic preparation of the
samples was performed at the National Research and Re-
source Facility for Submicron Structures.
4c. F. Mate, R. Harris-Lowe. W. L Davis, and I. G. Daunt, Rev. Sci. In-
strum. 36, 369 (1965).
'E. T. Swartz and R. O. Pohl, Proceedings of the 5th Conference 01/ Phonon
Scatterillg ill Condensed Matwr. edited by J. P. Wolfe and A. C. Anderson
(Springer. Berlin, 1(86).
"RMC, Inc .• 1802 W, Grant Rd, Suite 122, Tucson, AZ 85745.
'Detoronics, Inc .. Detroit, MI.
'c. J. Hoffman, F. J. Edeskuty, and E. F. Hammel, J. Chern. Phys. 24,124
( 1956).
"For Iypical calibration curves, see G. K. White, l!.xperimental Techniques
in Low Temperature Physics (Clarendon, Oxf()fd, 1979). At 4.2 K the
resistance is about 20 kH, and at 25 K the resistance is about 1 kB.
"JR. J. Mayhan. Al1a~l'.\'is o/Discrele Tim" and Continuous-Time Linear .sys-
tems (Ohio State University, Columbus. 1981).
l i n . F. McQlleeney (private communi.'atlon).
[-'l.ow Temperalurc Techniques ill Condensed IHatta Physics, in the Fron-
liers of Physics series, edited by R. C. Richardson and E.:><. Smith (Benja-
min, New York) (te be published).
"P. L. Kapitza, J. Phys. (USSR) 4, 181 (1941); also in Collected Papers 0/
P. L. Kapilza, Vol. 2, edited by D. ter Haar(Pergamon, Oxford, 19(5). p.
SR 1.
141. M, Khalatnikov. J. Exp. Theor.l'hys. (USSR) 22, 687 ( 1(52); also in L

M. Kapitza, All Introduction to the Theory ofSuperconductiuity (Benja-

[E. T. Swartz. Rev. Sci. lnstrum. 57, 2848 (1986).
'D. Walton, T. Timusk, and A. 1. Sievers, Rev. Sci. Instrum. 42, 1265
(1963 ).
3J. P. Torre and G. Channin, Rev. Sci. Inslrum. 56, 318 (1985).
min. New York, 1(65), p. 138.
"E. T. Swartz and R. O. Pohl, Solid-Solid Thermal Boundary Resistallces
(in preparation). See also E. T Swartz, Ph.D. thesis, Cornell University,
(ill preparation).
160stby and Barton, 480 Jefferson Blvd., Warwick, RI 02886,

839 Rev. SCi.lnstrum., Vol. 58, No.5, May 1987 Cryostats 889

This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitationnew.aip.org/termsconditions. Downloaded to IP:
.-•.• ;.:.;.;.;o••••••••••••••••••• •••••••:.-.:•••
~ :.:;:.:-:.:.:.:.:.~.;.:.:.~.:.:.;.:.; > •••••' •••••••••••: •••: ••••••••••........
129.97.125.224 On: Mon, 24 Nov 2014 21:12:02
•••••;••••••••••••••••••·s·.·;>.·.;.-.·.:.:.:.:.:.:.:.:-.:.:.;.:·:·:·:o;·;·;·;.;·:·.·.......................