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Electronic Theses, Treatises and Dissertations The Graduate School

2006

Measuring Thermal Conductivity of Powder

Insulation at Cryogenic Temperatures
Matthew Barrios

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 THE FLORIDA STATE UNIVERSITY

COLLEGE OF ENGINEERING

MEASURING THERMAL CONDUCTIVITY OF POWDER

INSULATION AT CRYOGENIC TEMPERATURES

By

MATTHEW BARRIOS

A Thesis submitted to the

Department of Mechanical Engineering
in partial fulfillment of the
requirements for the degree of
Master of Science

Degree Awarded:
Fall Semester, 2006
The members of the Committee approve the Thesis of Matthew Barrios defended
on August 9, 2006.

_______________________
Steven Van Sciver
Professor Directing Thesis

_______________________
Cesar Luongo
Committee Member

_______________________
Justin Schwartz
Committee Member

Approved:

_______________________________________________
Chiang Shih, Chair, Department of Mechanical Engineering

_______________________________________________
Ching-Jen Chen, Dean, FAMU-FSU College of Engineering

The Office of Graduate Studies has verified and approved the above named
committee members.

ii
To my Godsons, Austin and Dayton. This is why I haven’t been around quite as
much as I’d like to be.

iii
 ACKNOWLEDGEMENTS

First I would like to thank the members (and former members) of the
Cryogenics Group at the NHMFL for their assistance and contributions. Yeon
Suk Choi’s guidance has been instrumental in the development of this work.
Scott Maier’s technical advice and assistance have proven invaluable time after
time. Also, the completion of this work would not have been possible without the
direction of my advisor, Professor Steven Van Sciver.
Thanks to my committee, Professor Cesar Luongo and Professor Justin
Schwartz, for their advice and comments.
James Fesmire and the group from NASA Kennedy Space Center are responsible
for the funding of this project. Their suggestions and financial support have been
integral.
Thanks also to my fellow graduate students, who have provided friendship
and aid over the past two years.
A special debt of gratitude is owed to the doctors and nurses who have
treated me over my period of illness. Without Dr. Stephen Bardot, Dr. Jyotsna
Fuloria, Dr. Joseph Camps, and Dr. James Mabry, I may not be here today.
Lastly, I would like to express the most sincere thanks to my family and
closest friends. The support and encouragement I’ve received from my parents,
Andre and Wendy Barrios, and my siblings, Chris, Ryan, and Katy, have been
instrumental in the completion of this work.

iv
 TABLE OF CONTENTS

List of Tables ............................................................................................Page vi

List of Figures ............................................................................................Page vii
Abstract ..................................................................................................Page viii

1. Introduction ............................................................................................Page 1

Cryogenic Insulation Systems..................................................................Page 2

Overview of Insulation Testing Techniques .............................................Page 5
Scope of Thesis .......................................................................................Page 5

2. Basics of Thermal Insulation Measurement .................................................Page 7

Thermal Conductivity Measurement Methods..........................................Page 7

Theory of Measurement ...........................................................................Page 12
Thermal Conductivity of Powder Insulation.............................................Page 17

3. Experiment Design and Procedure ...............................................................Page 19

Experiment Design ..................................................................................Page 19

Hardware/Software..................................................................................Page 23
Experiment Procedure..............................................................................Page 27

4. Results and Conclusions ..............................................................................Page 32

Phase 1 Results........................................................................................Page 32
Phase 2 Results........................................................................................Page 34
Thermal Gradient Test .............................................................................Page 39
Conclusion ...........................................................................................Page 39
Suggested Future Work ..........................................................................Page 40

APPENDIX ............................................................................................Page 41

A Uncertainty Analysis..........................................................................Page 41

BIBLIOGRAPHY ............................................................................................Page 44

BIOGRAPHICAL SKETCH ...........................................................................Page 46

v
 LIST OF TABLES

Table 1.1: Powder Insulation Properties ...........................................................Page 4

Table 3.1: Temperature Sensors........................................................................Page 24

Table A.1: Uncertainty Values for Basic Measurements ...................................Page 42

Table A.2: Uncertainty Values for Phase 2 .......................................................Page 42

vi
 LIST OF FIGURES

Figure 1.1: Liquid Hydrogen Tank ...................................................................Page 1

Figure 1.2: Powder Insulation...........................................................................Page 4

Figure 2.1: Guarded Hot Plate Design ..............................................................Page 8

Figure 2.2: Concentric Sphere Apparatus..........................................................Page 10

Figure 2.3: Comparative Thermal Conductivity Measurement ..........................Page 11

Figure 2.4: Boundary Conditions for Lumped Capacitance Method ..................Page 14

Figure 2.5: Boundary Conditions for Steady State Calculations ........................Page 16

Figure 2.6: Thermal Conductivity of Powder Insulations ..................................Page 18

Figure 2.7: Aerogel Thermal Conductivity (Rettelbach) ...................................Page 18

Figure 3.1: Experiment Picture and Schematic..................................................Page 20

Figure 3.2: Schematic of Complete Experimental Apparatus ............................Page 22

Figure 3.3: Temperature Sensor Calibration Curve ...........................................Page 25

Figure 3.4: Heaters for Experiment...................................................................Page 28

Figure 4.1: Temperature History of the Hot Cylinder (Phase 1) ........................Page 33

Figure 4.2: Aerogel Thermal Conductivity (Phase 1) ........................................Page 33

Figure 4.3: Cooldown Time for Phase 2 ...........................................................Page 34

Figure 4.4: Production of Steady State Conditions ............................................Page 35

Figure 4.5: Steady State Temperatures..............................................................Page 36

Figure 4.6: Aerogel Thermal Conductivity (Phase 2) ........................................Page 37

Figure 4.7: Compilated Thermal Conductivity Data..........................................Page 38

vii
 ABSTRACT

A device to measure bulk effective thermal conductivity of powder insulation at

cryogenic temperatures has been designed and tested. The design consists of two
concentric cylinders which are suspended inside of a cryostat. The insulation being
tested is filled into the annular space between the cylinders. In the first test method the
insulation space is evacuated, and the cryostat is filled with LN2 until the outer cylinder is
completely submerged. The ensuing temperature drop of the inner cylinder over time is
recorded. The rate of temperature decrease is used to calculate the bulk effective thermal
conductivity of the insulation. For the second test method, a Gifford-McMahon single
stage cryocooler is used to cool the apparatus to a desired temperature range. The
insulation is evacuated, and a heater mounted on the inside cylinder creates a temperature
difference between the two cylinders. Fourier’s law of heat conduction is used to relate
that temperature difference to a bulk effective thermal conductivity of the powder
insulation.
The insulation specimen used for this experiment was aerogel bead insulation.
The first test method covered an average temperature range of 85-130 Kelvin. The
calculated bulk effective thermal conductivity from the first method for this range
increases from 0.333 to 0.714 mW/m*K. Six data points have been produced by the
second test method. The average temperature for the second method ranged from 30-80
Kelvin. Over this temperature range the thermal conductivity shows an increase from
0.142 to 0.377 mW/m*K.
Feasibility of use of the concentric cylinder thermal conductivity measurement
apparatus as a standard measurement technique is discussed. The implementation of a
cryocooler gives the ability to reach lower temperature ranges and create smaller
temperature differences than previous research has produced. However, a few difficulties
such as electrical problems and an unexpected temperature gradient through the outer
cylinder must be resolved prior to further implementation of the apparatus. Plans for
further research and development of the apparatus are presented.

viii
 CHAPTER 1

INTRODUCTION

Since the liquefaction of helium in 1908 by Kamerlingh Onnes there has been an
increasing demand for high performance insulation systems. This demand has resulted in
the development of vacuum systems, multi-layered insulation (MLI), various powder
insulations, and low heat leak mechanical supports. Though MLI has proven to have a
lower effective thermal conductivity than any other insulation type, its need for a high
vacuum environment and lack of load bearing capacity has generated interest in powder
insulations, such as perlite, silica aerogels, and glass microspheres, particularly for
insulating liquid hydrogen and liquid oxygen vessels. Many powder insulations have the
advantages of moderate load bearing capacity as well as high performance in applications
with soft vacuums and higher pressures. Such advantages make powder insulation well
suited for use in many current engineering applications. An example of one of such
applications is the 850,000 gallon liquid hydrogen tank (Fig.1.1) located at NASA’s
Kennedy Space Center (NASA KSC). As a thermal barrier, the insulation space around

Figure 1.1 LH2 Tank at NASA KSC

(Photo: D. Wood)

1
the tank houses roughly the same volume of powder insulation (currently perlite). The
affordability and ease of installation of perlite make it an attractive option for an
insulating material. However, data from the literature suggests that synthetic powders
similar to perlite, such as aerogel and glass microspheres, possess better insulating
properties than perlite under similar conditions [1,2]. Unfortunately, there is a shortage
of reliable experimental data regarding the thermal conductivity of aerogel and glass
microspheres, particularly below liquid nitrogen temperature, T=77 K.
Furthermore, advances in insulation kindle a need for a movement towards a
standardized testing procedure at cryogenic temperatures. This would allow for more
accurate empirical results that can be compared between laboratories. The present
research is intended to obtain experimental data regarding the effective thermal
conductivity of aerogel beads, while taking steps toward providing a standard procedure
for making such measurements.

1.1 Cryogenic Insulation Systems

1.1.1 Multi-Layered Insulation

Currently, the most effective insulation used in cryogenic applications is multi-
layered insulation (MLI). MLI consists of multiple sheets of highly reflective material
alternating with poorly conducting fibrous materials. The space containing the MLI must
be evacuated to pressures below 0.001 Torr for maximum effectiveness [1]. The high
vacuum eliminates convection and makes gas conduction negligible. The reflective
material (usually a very thin aluminum or gold layer coating a mylar film) significantly
decreases the emissivity of each layer of MLI thereby approximating multiple reflective
radiation shields. The low density, low thermal conductivity fibrous materials act as a
physical separation between the reflective layers.
MLI is generally considered the most effective form of cryogenic insulation
available. However, MLI does have some disadvantages. The effective thermal
conductivity of MLI shows a significant increase with an increase of pressure in the
insulation space [3]. Reaching the high vacuum ranges required for optimum
performance of MLI is impractical in many situations. The load bearing characteristics

2
of MLI are also very poor. Thus, many vacuum spaces containing MLI require
mechanical supports, which can be main sources of heat leaks.
1.1.2 Perlite
Perlite is a naturally occurring silicate glass. When crushed, perlite can then be
expanded under intense heat to nearly 20 times its original volume. Perlite is one of the
earliest used forms of powder insulation and is still used in many applications because of
its affordability and wide range of uses. However, more advanced forms of powder
insulation, such as those listed in the following sections, are steadily replacing perlite due
to their superior insulating properties.
1.1.3 Aerogel Beads
Aerogel is a low density granular solid produced by a solution-and-gelatin (sol-
gel) process. In this process a silicon solution is hydrolyzed to form an SiO2 gelatin
structure. The gelatin is then dried to form a nano-porous solid with roughly the same
structure. A continuous spray process is employed to produce the aerogel beads.
The beads used in the present experiment are Nanogel® aerogel beads produced
by the Cabot Corporation. Various properties of the beads, along with some other
insulating powders, are shown in table 1.1. Some advantages to aerogel beads are
affordability, ease of installation, nonsettling, no preconditioning required, and a highly
porous structure. The nanopores tend to trap gas molecules, thereby significantly
reducing convection and gaseous conduction.
1.1.4 Glass Microspheres
Glass microspheres, or bubbles, are similar to aerogel beads in many respects.
The microspheres consist of borosilicate glass and amorphous silica. The production
process for microspheres is also fairly similar to that of the aerogel beads. However, as
the name suggests, microspheres are at least an order of magnitude smaller than aerogel
beads. Recent experimental data from Fesmire et al [2] has shown that under certain
conditions glass bubbles have a lower thermal conductivity than aerogel beads and thus
may be the most effective insulating powder available. However, thermal conductivity
data is needed for glass bubbles over a larger temperature range to confirm the powder’s
superior insulating properties.

3
 Table 1.1 Powder Insulation Properties

Name Diameter Density Main Component

Nanogel (R) Aerogel Beads 1-4 mm 1900-2200 kg/m^3 Silica Gel >97%

3M (TM) Glass Bubbles 10-120 microns 100-600 kg/m^3 Soda Lime Borosilicate Glass >97%

Ryolex (R) Perlite 50-1000 microns 2350 kg/m^3 Expanded Perlite 100%

Figure 1.2 Powder Insulation

4
 1.2 Overview of Insulation Testing Techniques

Attempts to measure the thermal conductivity of poorly conducting materials date

back to the mid 19th century when Péclet, a French physicist, determined the thermal
conductivity of various common solids [4]. Péclet used insulated rectangular plates
heated with steam on one side and exposed to ambient air on the other to perform his
measurements. Richard Poensgen of Germany developed the original version of the
guarded hot-plate insulation test method in 1912 [5]. This test method, which will be
discussed later, has undergone a number of improvements and modifications, but it
continues to be the most widely used thermal conductivity testing method to date.
Thermal conductivity measurement methods for vacuum insulation at cryogenic
temperatures began in the 1950’s when Fulk, Kropschot, and other researchers at the
National Bureau of Standards (NBS) tested multi-layer insulation and evacuated powders
[6,7,8]. Fulk et al. used radial flow boiloff calorimeters to obtain their measurements.
Most recently, J. E. Fesmire et al. have developed several measurement cryostats
consisting of LN2 boiloff calorimeters, which provide different insulation geometry and
measurement methods [9,10].

1.3 Scope of Thesis

The present work is describes the development of a thermal conductivity

measurement apparatus for testing of powder insulation. The apparatus is designed to
have the ability to cover a large range of cryogenic temperatures while maintaining a
relatively small difference between boundary temperatures. The apparatus also allows
for future measurements at various vacuum levels and using different interstitial gases.
Chapter 2 of this thesis sets the background for the development of the current
experiment. Other thermal conductivity measurement techniques and their main
application areas are discussed. The mathematics used to calculate thermal conductivity
are explained and conformed for use with the present measurements. Finally, data from
outside sources is presented to show what may be expected from the results obtained
from the current experiment.

5
 Chapter 3 of the thesis describes the details of the apparatus and the experimental
procedure. Design considerations and requirements needed for an apparatus to perform
at cryogenic temperatures are discussed. Software and hardware used in the experiment
are noted, as are the corresponding operating conditions and capabilities. Required
calibrations and mounting procedures are recounted. Two experimental procedures are
then discussed in detail from the assembly of the apparatus, through obtaining data
points, to warmup and disassembly.
Chapter 4 of the thesis begins with the presentation of results. Results from both
experimental techniques used are shown and compared with other data from the
literature. An unexpected apparent temperature gradient through the apparatus is also
discussed. Conclusions are then drawn about the performance of the apparatus and the
feasibility of its use in the standardization of cryogenic thermal conductivity
measurement. Finally, future work is discussed, along with suggestions for
improvements and further research.

6
 CHAPTER 2

BASICS OF THERMAL INSULATION MEASUREMENT

In general, there are three modes of heat transfer which can occur through a given
medium: conduction, convection, and radiation. All thermal insulation types attempt to
minimize these heat transfer methods. Effective thermal conductivity is a simplified
measure of insulation performance. It incorporates a material’s resistance to all modes of
heat transfer into a single coefficient. The present chapter gives an overview of several
methods to find the effective thermal conductivity of powder insulation. Next, the theory
behind the calculation of effective thermal conductivity is presented. Finally, thermal
conductivity data for various insulating materials from the literature is discussed.

2.1 Thermal Conductivity Measurement Methods

The purpose of the present experiment is to test various types of powder

insulation to find effective thermal conductivities. The testing apparatus was designed to
create, as best as possible, a controlled volume which utilizes various devices to produce
conditions suitable to measure thermal conductivity. Several past and current
experiments were taken into consideration before attempting to design a new apparatus
which would allow for a larger temperature range, a smaller temperature difference, and
more accurate measurements, if possible. Current thermal conductivity measurement
devices are discussed in this section.
2.1.1 Measurement Configurations
2.1.1.1 Guarded Hot Plate The guarded hot plate method of testing thermal
conductivity was the first to become a nationwide standard (ASTM C177) [8]. This
method employs an electrically heated plate sandwiched between a pair of specimens.
Each specimen is then enclosed by a cooling plate. The earliest guarded hot plate
mechanisms used water or ambient air as a heat sink for the cooling plate. A schematic
of a guarded hot plate apparatus is shown in figure 2.1.

7
 Figure 2.1 Schematic of basic guarded hot plate design

The guarded hot plate method is an excellent method of testing the effective
thermal conductivity of solids under certain conditions. The method attempts to create
unidirectional heat transfer through the insulation specimens. The thickness and surface
areas of the specimens can be measured precisely. Then, by adding a known heat flux to
the hot plate while providing a heat sink at the cold plate a temperature gradient within
the insulation specimen is formed. The subsequent temperatures at each side of the
specimens are measured when the system reaches steady state. Using the heat flux,
sample thickness and surface areas, and temperature measurements, Fourier’s
unidirectional heat conduction equation can then be applied to easily calculate an
effective thermal conductivity for the samples.
The guarded hot plate method, although very effective for many practical
insulation tests, is difficult to apply to powder insulation. Containing the powder within
the apparatus is much more difficult than installing a solid specimen. Any mechanical
supports used would create a heat leak and make material thermal conductivity much
harder to calculate. Therefore, other configurations which may be more conducive to
powder insulation should be examined.

8
 2.1.1.2 Concentric Cylinders Steady state thermal conductivity measurement
methods involve the production of a temperature difference between the sides of an
insulation specimen. The configuration of the specimen and apparatus varies for
different methods. Two configurations which have proven to be suitable for powder
insulation measurement are the concentric cylinder and concentric sphere.
The concentric cylinder method has been used since as early as 1926 by Aberdeen
and Laby [11]. In most cases the apparatus consists of a liquid cooled outer cylinder and
an electrically heated inner cylinder. Between the cylinders powder can be filled and
evacuated to the desired pressure. Ideally, the concentric cylinder apparatus should
create a uniform heat flux in the radial direction. However, mechanical supports are
required at the top and bottom of the inner cylinder. The supports act as heat leaks and
create a temperature gradient in the inner cylinder. Therefore, the cylinder is designed to
be very long with respect to its radius. This allows for a fairly uniform temperature along
a sufficient length of the cylinder. However, axial heat leakage can still be problematic
when using the concentric cylinder method.
2.1.1.2 Concentric Spheres The concentric sphere method used by Nayak and
Tien [12] is designed to eliminate end effects and guard plates associated with the
concentric cylinder and guarded hot plate methods, respectively. A schematic of their
concentric sphere apparatus is shown in Fig. 2.2. Thin nylon supports and electrical
collections minimize the heat leak between cylinders, making it negligible. Small holes
in the outer cylinder covered with filters allow for the insulation space to be evacuated.
The temperature of the outer sphere is maintained by adjusting the cryogen level on the
copper stem and the heating power of the stem heaters. The insulation space is
evacuated, and the heater on the inner sphere is powered to create a temperature
difference between the spheres. By this method any temperature range between the
temperature of the cryogen and ambient temperature can be reached. A filler spout is
placed atop the outer sphere to replace any powder lost from settling. The concentric
sphere method is a novel approach to measuring effective thermal conductivity of
powder. However, spheres are expensive to manufacture and difficult to work with.
Therefore, other configurations would be more suitable for the standardization of a
powder insulation thermal conductivity testing method.

9
 Figure 2.2 Schematic of concentric sphere apparatus

2.1.2 Heat Flux Measurement

The determination of thermal conductivity under steady state conditions requires
the precise measurement of boundary temperatures and heat flux. Temperature
measurement can be achieved with any number of sensor types or with the use of a
cryogen at its boiling point. However, more elaborate methods have been developed to
accurately measure the heat flux through the insulating material. Measuring the power
supplied to a heater is the simplest method of measuring heat flux. However, direct

10
measurement of heating power is insufficient when large heat leaks may be present. The
following sections discuss a few techniques which have been developed to negate the
effects of heat leaks on heat flux measurement.
2.1.2.1 Comparative Thermal Conductivity Comparative thermal conductivity
measurements use a material with a well known thermal conductivity in series with the
insulation specimen. A precisely measured thickness of the known material is placed on
either side of the insulation specimen (Fig. 2.3). By monitoring the temperatures on each
side of the known materials, the heat flux through the materials can be calculated fairly
accurately (depending on the accuracy of the “known” thermal conductivity). In this
manner the heat flux through the specimen between the materials can be obtained.

Figure 2.3 Schematic of comparative thermal conductivity measurement configuration

2.1.2.2 Boiloff Calorimetry Boiloff calorimeters house a cold mass which

contains a liquid. The cold mass is separated from a heat source by the insulating
material being tested. The heat source increases the temperature of the hot side of the
apparatus to above the boiling point of the liquid. The liquid then maintains a constant

11
boundary temperature for the cold side (the boiling point of the liquid) and provides a
means to measure the heat flux through the insulation specimen. As the liquid boils the
flow rate of the escaping vapor is monitored. The heat flux entering the cold mass can be
calculated by measuring the flow rate of the escaping vapor.
Fesmire et al [9] have recently developed three cryostats which utilize boiloff
calorimeters at cryogenic temperatures. The cryostats vary in configuration (guarded hot
plate and concentric cylinder), and two of the three provide comparative thermal
conductivity measurements as well. In this manner, the heat flux can be measured
separately directly from the heat source, through the known materials, and into the cold
mass.
Boiloff calorimeters, although they can be implemented in many configurations,
are limited in their potential uses. The use of a cryogen to produce low temperatures
automatically sets a boundary point which cannot be changed without substituting the
cryogen for another. This causes either a very large ∆T and/or a very limited average
temperature range. Also, heat leaks to the cold mass through vents and supports may
affect the boiloff rate of the liquid. Lastly, measurements at liquid hydrogen and liquid
helium temperatures may be impractical using boiloff calorimetry due to economic and
safety factors.

2.2 Theory of Measurement

The purpose of the present experiment is to measure the bulk effective thermal
conductivity of powder insulation. “Bulk” means that the measurement volume is much
larger than that of an individual particle. Effective thermal conductivity ( keff ) differs

from true thermal conductivity ( k ) in that keff incorporates all forms of heat transfer,

whereas k is concerned solely with conduction. Effective thermal conductivity is

especially useful when working with solids which are not homogeneous or uniform (i.e.
powder, MLI, porous media). In these cases, the material thermal conductivity is
difficult to measure and may be difficult to apply. The disadvantage of using keff is that,

unlike k , keff is dependent on interstitial gas type and pressure. Therefore, when using

12
keff , as opposed to k , more independent variables are introduced, but insulation

performance can be estimated much more easily.

The present experiment, which will be explained in detail in the next chapter,
employs a closed concentric cylinder apparatus to measure effective thermal
conductivity. The equations required to calculate effective thermal conductivity from the
closed concentric cylinder configuration can be derived as follows.
Phase 1 of the experiment consisted of a cooldown from ambient temperature to
about 85 K. The lumped capacitance method was used to model the cooldown
mathematically. The lumped capacitance method is normally based on convection heat
loss causing a decrease in the internal energy of a body. In mathematical form,
∂T
q = hA(T − T∞ ) = − mc(T ) (2.1)
∂τ
where h , A , and c(T ) represent the convection heat transfer coefficient, the heat
transfer area of the body, and the specific heat of the body, respectively. The requirement
for the lumped capacitance method to yield estimates within 5% is the following
h(V A)
< 0.1 (2.2)
kCu

where kCu and V are the thermal conductivity and volume of the body (a copper cylinder
in the present experiment), respectively. However, the present experiment involves heat
transfer through insulation, which is modeled as conduction, in lieu of convection.
Therefore, the following substitution must be made for h
kins
h= (2.3)
z
where kins and z represent the effective thermal conductivity and thickness of the
insulation, respectively. The condition in equation 2.2 then becomes
kinsV
< 0.1 (2.4)
kCu A ⋅ z
kinsV
Calculations using experimental data show that < 10−5 in this experiment.
kCu A ⋅ z
Applying the lumped capacitance method, the solution to equation 2.1 is

13
  kins ( T )⋅ A 
T − T∞ − τ
= e  z ⋅ m ⋅ c (T )  (2.5)
To − T∞
where T∞ represents the temperature of the outer cylinder. To and T represent the initial
temperature and temperature after time τ of the inner cylinder, as seen in Figure 2.4.

Figure 2.4 Boundary conditions for lumped capacitance method

Solving for kins yields the following

− z ⋅ m ⋅ c (T )  T − T∞ 
kins (T ) = ln   (2.6)
A ⋅τ  To − T∞ 

14
Here it must be noted that the above solution assumes that the specific heat of the copper
and thermal conductivity of the insulation are independent of temperature. This does not
hold true over large temperature ranges. Therefore temperature increments of 10 K or
less were sampled, and the resulting calculations used an average heat capacity for each
temperature range. In turn, the thermal conductivity data obtained were also the average
thermal conductivities for each range. To ensure that the 10 K data range produced
negligible error due to the change in heat capacity, final calculations were performed
which included a temperature dependent function for heat capacity in the solution of
equation 2.1.
Phase 2 of the present experiment involved data collection under steady-state
conditions. Fourier’s law of heat conduction, equation 2.7, is used to calculate the
thermal conductivity for phase 2.
dT
q = − k (T ) A (2.7)
dx
Equation 2.7 applies to one dimensional heat conduction. In this experiment, however,
the heat flux will be in the radial and axial directions. Therefore, the data calculated in
this experiment must be considered approximate. The solution of equation 2.7 is

q = −k (T ) A
(Ti − To ) (2.8)
z
Solving for thermal conductivity leaves
zq
k (T ) = − (2.9)
A ( Ti − To )

Equation 2.9 was used to calculate the effective thermal conductivity data for phase 2 of
the experiment.
The experiment can be more accurately modeled in cylindrical coordinates. In
this case the heat transfer rate in the radial direction becomes
∂T
qr = −2π rlk (2.10)
∂r
where l and r represent the length and radius of the cylinder, respectively. After
applying the boundary conditions
T = Ti at r = ri

15
 T = To at r = ro
where i and o denote inner and outer surfaces, respectively, the solution of equation
2.10 becomes
(Ti − To )
qr = −2π lk (2.11)
ln(ro ri )
From equation 2.8, the heat transfer rate through the top and bottom of the cylinder is
∂T
qz = −2π r 2 k (2.12)
∂z
The solution of equation 2.12 is simply
(Ti − To )
qz = −2π r 2 k (2.13)
z
where z is the insulation thickness. Due to symmetry and the cylindrical boundary of

Figure 2.5 Boundary conditions for steady state conduction calculations

16
the material region it can be assumed that there is negligible heat transfer in the angular
( θ ) direction. Therefore the total heat transfer rate through the cylinder is
(Ti − To ) (T − T )
qtot = −2π lk − 2π r 2 k i o (2.14)
ln(ro ri ) z
However, calculations were performed which show that equation 2.14 can be replaced
with equation 2.8, where A represents the inner cylinder heat transfer area (including the
top and bottom surfaces). The simplification made by using equation 2.8 results in a
difference of less than 5%. A more accurate method for calculating the thermal
conductivity will be used in future works. Equation 2.8 was used for the present
experiment because the measurement apparatus and experimental procedures must be
tested before more accurate (and thereby tedious) calculations are required.

2.3 Thermal Conductivity of Powder Insulations

Previous research has provided an excellent starting point for the current
experiment. Many thermal conductivity measurements have been recorded for powder
insulation; however, the majority of these measurements are taken between LN2 and
room temperature. Several measured thermal conductivity values of different types of
insulation are shown in Figure 2.6. This plot of thermal conductivities simply gives an
idea of the range of values that can be expected from the experiment. A more direct
comparison of our data can be made with the data from Rettelbach et al [1]. Rettelbach et
al employed a liquid helium cooled guarded hot plate apparatus to obtain thermal
conductivities for evacuated aerogel (and opacified aerogel) powder from 10 K to 275 K.
Figure 2.7 is a graph taken from [1] which shows thermal conductivity data for various
aerogel samples.

17
Figure 2.6 Recorded thermal conductivities of various types of powder insulation

Figure 2.7 Aerogel and opacified powder thermal conductivity [Rettelbach 1]

18
 CHAPTER 3

EXPERIMENT DESIGN AND PROCEDURE

The current chapter recounts the design parameters, experimental setup, and
operating procedures of our specialized apparatus to measure the thermal conductivity of
powder insulation at cryogenic temperatures. Difficulties in construction and
implementation of the apparatus are also discussed. So as not to be credited for the work
of others, at this point the author would like to note that Yeon Suk Choi, PhD., and
Steven Van Sciver, PhD., are responsible for the vast majority of the design and original
assembly of the apparatus. Dr. Y. S. Choi also carried out phase 1 of the project,
consisting of measuring the effective thermal conductivity of aerogel to LN2 temperature.
The results of this work can be found in [11].

3.1 Experiment Design

In the interest of uniformity and ease of installation, the present experiment has
been designed as two closed, concentric copper cylinders, as seen in Figure 3.1. The
inner cylinder is the hot cylinder (HC), and the outer cylinder is the cold cylinder (CC).
The CC is suspended from the top plate by four 6.35 mm diameter GFRP rods. The HC
is suspended from the CC by three 1.6 mm diameter GFRP rods. An electric heater is
mounted between a copper plate and the bottom of the HC. This mounting configuration
is to ensure good thermal contact with the HC. Temperature sensors are mounted on the
side and top of the HC. Temperature sensors are also mounted on the side and top of the
CC. Placement of temperature sensors is shown in Figure 3.1.
The main goal of the present experiment is to measure the effective thermal
conductivity of powder insulations over a large cryogenic temperature range. However,
to compare with previous work, the first phase of the experiment was performed simply
by immersing the CC in LN2 and recording the temperature of the HC over time. This
technique, however, was very time consuming and only provided thermal conductivity
measurements down to roughly 80 K. A method which covers a lower temperature

19
range, preferably down to 20 K or below, was needed. The use of another cryogen, such
as liquid hydrogen or helium, was an option. However, cryogens such as these must be
refilled frequently and, especially in the case of hydrogen, can pose a serious safety
hazard. Therefore, the best available option was the use of a single stage Gifford-

Figure 3.1 Left: Photograph of experimental apparatus

Right: Schematic of experiment cross section

20
McMahon cryocooler capable of reaching ~20 K. The cryocooler used in this experiment
was a Cryomech AL63-2106300. Specifications of the cryocooler are listed in section
3.2.4.
The cryocooler coldhead must have good thermal contact with the CC of the
measuring apparatus for the experiment to perform effectively. As seen in Figure 3.1,
flexible, tinned copper braids form a thermal link between the cryocooler coldhead and
the CC while allowing for thermal contraction/expansion. Copper plates bolted together
connect the coldhead to the copper braids, and the braids to the CC. Each plate surface is
coated with Cryo-Con thermally conductive grease to ensure proper thermal contact.
In order to allow the experiment to reach its minimum temperature, the cryocooler
and the measurement apparatus must be well insulated from any outside heat sources.
Insulation of the apparatus from its surroundings is provided by several means. Two
radiation shields are installed between the measurement apparatus and the top plate.
Also, MLI is applied to the CC and one of the radiation shields for the steady state phase
of the experiment. The entire apparatus is then placed inside of a vacuum insulated
cryostat, which employs a liquid nitrogen (LN2) thermal shield. The inner space of the
cryostat contains the apparatus and is continuously pumped with a high vacuum system
which maximizes thermal insulation of the experiment. Figure 3.2 is a schematic of the
experimental assembly while in the cryostat.
The experiment uses pressurized gaseous helium in the HC to ensure a uniform
temperature. The pressure in the annular space (insulation space) and outside the CC
may vary. Therefore each cylinder must be vacuum sealed so as to prevent gaseous
conduction or convection between the cylinders. Also, ports must be provided to all
spaces to allow for pressurizing and/or vacuum pumping. All ports and wiring feeds
directly connected to the apparatus are connected by solder, welded, or stycast and are
tested individually to assure that they are leak tight. To ensure that the vacuum pump
connected to the insulation space is not contaminated with insulation powder, a fine
screen is placed where the vacuum port meets the top of the CC.
Because the cylinders must be opened and closed relatively frequently, less
permanent measures to prevent gas leaks must be taken. To this end, prior to closing,

21
Figure 3.2 Schematic of complete experimental assembly

22
indium O-rings are fit into grooves set into the top and bottom of each cylinder. As the
caps are bolted to the cylinders the indium O-ring is compressed to form a leak tight seal.
Several measures must be taken to ensure the accurate measurement of heat
transfer and temperature. The present experiment is thus designed to minimize heat
leaks, especially heat leaks to the HC. Heat leaks to the CC affect the performance of the
cryocooler but, unless the heat leaks are very large, should not affect the temperature
difference between the cylinders. As mentioned above, GFRP rods are used as supports
for the cylinders. GFRP is used for its high strength to thermal conductivity ratio. The
supports for the HC have small diameters (1.6 mm), and they also extend well above and
below the top plate of the CC and the top plate of the HC, respectively. The added length
and small cross-sectional area decrease heat transfer through the rods in accordance with
Fourier’s one-dimensional heat conduction equation (Eq. 2.7). Wires connecting the
temperature sensors in the HC are run through a vacuum sealed stainless steel tube and
are composed of fine manganin. Heater wires follow the same path but are made of fine
copper.
Installation of insulation is another design issue. As has been noted, an advantage
of powder insulation is that most powders used are free flowing. An installation port at
the top of the CC allows for insulation to be filled manually following a procedure
outlined in section 3.3.1. Because settling of powders can occur during the experiment
due to vibration, applied load, or particle breakage, a stainless steel canister sits atop the
installation port to hold excess powder. If some settling occurs, powder from the canister
falls into the annular space, ensuring insulation uniformity.

3.2 Hardware/Software

The present section lists the specific types of sensing equipment, heaters, coolers,
software, etc., utilized in this experiment. Also noted are the capabilities and/or ranges of
operation for the equipment.
3.2.1 Temperature Sensing Equipment
As has been noted previously, several temperature sensors are required to ensure
accurate temperature measurement over the range from ambient to liquid hydrogen’s

23
boiling point (20 K). Two basic types of Lakeshore® temperature sensors were chosen
for the present experiment configuration. Platinum sensors are applied for their accuracy
from room temperature to below LN2 temperature. Cernox™ sensors are used mainly for
their excellent accuracy over the lower cryogenic range of temperatures, from LN2
temperature to below 20 K. Sensor types and placements are shown in Table 3.1.

Table 3.1 Temperature sensors

Sensor Placement Serial # Type

Cryocooler Head P11792 Platinum
Cold Cylinder Top X04275 Cernox
Cold Cylinder Side P10281 Platinum
Hot Cylinder Top X37462 Cernox
Hot Cylinder Side P10280 Platinum

During the experiment the voltages produced by the platinum sensors were
converted to temperatures using a standard curve from the Lakeshore® catalog. Further
analysis of the data proved that the standard curves have insufficient accuracy for this
experiment. Therefore, a temperature sensor calibration was performed after the
experiment was complete. To perform the calibration, all of the sensors were mounted to
a specialized calibration rig and placed in a thermally insulating cryostat. The calibration
rig consists of a short copper cylinder designed to produce a uniform temperature
throughout. A recently calibrated Cernox™ sensor is also mounted to the rig. The rig is
then immersed in liquid helium and allowed to slowly warm up to room temperature.
The raw voltages from the sensors were recorded throughout the warm up process. The
voltages were plotted in an Excel graph versus the temperature readings from the
calibrated sensor. An example of one such voltage vs. temperature plot is shown in
Figure 3.3. The Excel trendline feature is used to create an approximate curve and

24
corresponding equation to fit the data plot. In general, it was necessary to generate two
or more curves to fit each plot accurately over the entire temperature range (see Figure
3.3). Here it should be noted that when liquid helium was placed in the cryostat, the
calibrated sensor read nearly 0.6-0.8 K less than the expected 4.2 K. Also, in a separate
LN2 test, the calibrated sensor showed voltages which corresponded to a temperature
nearly 1 K below the expected 77.36 K. The resulting offset may have slightly affected
the average temperature at each data point. However, thermal conductivity values should
have been unaffected because a temperature difference was used to calculate thermal
conductivity (as opposed to an absolute temperature). All temperature sensors were
mounted to the

Figure 3.3 Example of a calibration curve for a Cernox sensor. Equations

shown correspond to the nearest section of the curve.

25
experiment using VGE-7031 varnish. Where possible, sensors were imbedded inside
holes drilled specifically for sensor mounting. In these cases, Cryo-Con® thermal
conductive grease was applied to ensure good thermal contact with the cylinder.
Otherwise, sensors were weighted down or held tightly against the cylinder as the varnish
cured. Varnish was also used to adhere several inches of the lead wires of each of the
sensors to the surrounding surface. The adhesion acts as a heat sink, preventing heat
generation and conduction from outside sources from affecting the sensor’s temperature
reading. The bare chip Cernox™ sensors also require electric insulation so that the leads
don’t short circuit to the cylinder or to each other. Electric insulation was provided by a
segment of cigarette paper adhered to the cylindered with varnish. The sensor and its
leads were then mounted atop the paper. This method is recommended in the
Lakeshore® catalog as a way to ensure good thermal contact while providing electrical
insulation.
Power was supplied to each sensor by one of two Lakeshore® 120 current
sources. The platinum sensors require a constant current of 1 mA, whereas the
recommended excitation for the Cernox™ sensors is 10 mV. The power supplies have
been found to supply a current within 0.06% of the desired current setting.
3.2.2 Pressure Sensors
Two pressure sensors were used to monitor pressures inside the apparatus. A
Varian® Type 0531 vacuum gauge was used to measure the approximate vacuum level
inside the insulation space. An analog output device for the Varian gauge gives a
pressure reading between 1 atm and 1 mTorr. An MKS Baratron™ vacuum gauge
provides a pressure reading within the HC. This gauge was used to maintain the helium
pressure inside the HC so that it could be maintained at an appropriate level. The
Baratron™ has a 1000 Torr pressure range and was monitored with an LCD display.
3.2.3 Data Acquisition
When performing an experiment which utilizes several sensors, it is important to
have a reliable data acquisition system. Phase 1 of the experiment employed several
Keithley® multimeters to read the voltage output of each sensor separately. Readings
from the multimeters were sent to a PC where a Labview program converted the raw

26
voltages to temperature readings. These temperatures were constantly monitored and
recorded within the program.
Data acquisition for Phase 2 of the experiment was simplified with the use of only
one Keithley® Integra Series™ 2700 multimeter. The multimeter simultaneously
received the voltage output of all sensors, and reported the information to the PC. The
Excelinx software, provided with the multimeter, was used to record all voltages into a
Microsoft Excel file. Calibration equations were nested in the file to instantly calculate
and plot temperatures.
3.2.4 Cooling/Heating
The Gifford-McMahon cryocooler used in the present experiment is a
Cryomech® model AL63-2106300. The cryocooler was operated by the Cryomech®
CP435 compressor. The cooling capacity for the cryocooler is listed as roughly 40 W at
50 K and 5 W at 20 K. Cryocooler installation has been outlined previously.
Three Minco® heaters were used in the present experiment. All three are Kapton
Thermofoil™ heaters (Fig. 3.4). A Minco® model D/C0518 was used to provide heating
power to the HC. This heater was placed in a circular cavity in the bottom plate of the
HC. A layer of Cryo-Con® thermal conductive grease was applied to ensure good
thermal contact with the cylinder. A small copper plate, whose diameter is slightly less
than that of the cavity, was then placed on top of the heater and soldered in place. This
method of mounting the heater ensures that all heating power from the heater is
transferred to the HC. This is important because the heating power to the HC is used in
thermal conductivity calculations. It is less important to know the exact heating power
from the heaters on the CC and cryocooler head, therefore they were simply mounted
using a high strength epoxy. Power was supplied to the heaters by a Tenma® model 72-
7245 dual DC power supply.

3.3 Experiment Procedure

The present section describes the process by which insulation is installed and
thermal conductivity is measured. Assembly of the apparatus has been sufficiently
described previously.

27
.
Figure 3.4 Kapton Thermofoil™ heaters used in the experiment

3.3.1 Installation
Installation of the powder begins with a volumetric measurement. A large
amount of powder is placed in a glass beaker, and the volume is recorded. Any
remaining volume of powder after installation can be subtracted to find an estimated
volume of powder inside the annular space. Powder is poured through the installation
port until the level reaches near the top of the reserve powder canister. The canister and
CC can be lightly tapped to cause the powder to settle. It has been found, however, that
the most effective way to clear the installation port and ensure a proper fill is by closing
the installation port and connecting a roughing pump to the vacuum port. When the
roughing pump is used the powder moves from the installation port and allows for
additional powder to be filled. The filling/pumping process is repeated until the powder
level inside the canister is not noticeably changed when pumped on for a minute or more.

28
The canister is then sealed with an EVAC chain clamp and aluminum seal produced by
Nor-Cal Products, Inc.
The apparatus is then leak checked, and the electronics are tested. The apparatus
is then placed inside of the cryostat and the top flange is bolted in place. From this point
there are separate courses of action depending on the kind of experiment to be performed.
3.3.2 Phase 1 (Transient Cooldown Measurements)
The temperature data software is initiated and begins taking data points with both
cylinders at room temperature. The insulation space is then evacuated to the desired
pressure, and helium gas is filled inside the HC to slightly above atmospheric pressure.
LN2 is then filled into the cryostat until the liquid level is above the top of the CC. The
temperature of the CC rapidly reaches equilibrium with that of the LN2 (T= 77 K). The
liquid level is maintained with a large external dewar of LN2. A solenoid valve, operated
by a LN2 level indicator inside the cryostat, controls the LN2 flow from the supply dewar.
Temperatures are recorded as the HC slowly cools down. When the experiment
contains cryogenic insulation in vacuum, such as aerogel, the cooldown is a very time
consuming process. In the case of aerogel, it required nearly a month for the temperature
difference between the CC and HC to reach 10 K. At this point the LN2 is no longer
refilled and is allowed to boil off. Helium gas can be added to the insulation to increase
heat transfer between the cylinders and expedite the warm-up process. Once the
apparatus has reached ambient temperature it can be removed from the cryostat and be
modified as desired (i.e., changing insulation, changing temperature sensors, etc.).
3.3.3 Phase 2 (Steady State Measurements)
In phase 2, steady state measurements are made utilizing a cryocooler to cool the
CC. Therefore different measures must be taken to insulate the apparatus from its
surroundings. Once the apparatus is inside the cryostat, the cryostat must be checked for
leaks and subsequently pumped down to a suitable vacuum level. Temperature
measurement may then begin in the interest of monitoring the cooldown process. It is
preferable at this point to pressurize both the insulation space and the HC with helium
gas. Helium gas inside the insulation space greatly decreases the time required for the
HC to reach the desired temperature. The cryocooler is then turned on and allowed to
reach its minimum temperature or a desired point. As the temperature of the CC nears a

29
desired point the helium gas from insulation space is evacuated. At this point the
temperature of the HC can be manipulated, in effect, separately from that of the CC.
The first step to the stabilization of the CC temperature is to supply power to the
electric heater mounted on the CC or cryocooler coldhead. These heaters are used to
supply enough heat to balance the heat being removed by the cryocooler and stabilize the
temperature. The temperature profiles of the cryocooler head and CC must be monitored,
and the power supplied to the heater must be adjusted accordingly in an attempt to
stabilize the temperatures at the desired level. For the cryocooler to reach its minimum
temperature, of course, the outside heaters are not required. Power can be supplied to the
heater in the HC during or after the stabilization of the CC depending on the preferred
temperature difference (5-10 K for the present experiment). Power is added to the heater
in the HC until there is very little change in HC temperature, assuming that it is within
the temperature range of interest. The power supply to the HC needed to maintain a
suitable temperature difference between the cylinders can be estimated if previous
thermal conductivity data exists for the insulation being tested. This helps to hasten the
stability process. Stability for the cylinder temperatures is defined as a temperature
change, or preferably a temperature oscillation, of no more than +/-0.5 K/day over a
minimum 12-24 hour period.
Once the stability conditions stated above have been reached and the first point
has been collected, another data point can be obtained. First, the insulation space is again
pressurized with helium. Then the heating power to the CC is increased or decreased as
stated above until the temperatures reach the intended temperature range. The helium in
the insulation space is once again evacuated, and the heaters are manipulated to reach
stability as previously noted. This process can be repeated as many times as necessary to
produce the appropriate number of data points.
When the final data point is found, the warm up procedure ensues. Again, the
insulation space is pressurized with helium. The cryocooler is shut down, and power may
be supplied to the heaters in order to accelerate the warm up process. When the
temperatures reach near room temperature all electronics are turned off, and the apparatus
may be removed for maintenance.

30
3.3.4 Removal/Disassembly
After warming up, the assembly is removed from the cryostat. If maintenance
must be performed or a new insulation is to be tested, the MLI is removed from the
apparatus. The bottom of the CC can then be removed, and care is taken to collect the
insulation which pours out of the annular space. The CC is then removed from the
apparatus, and any powder remaining on top of the HC is collected. If maintenance to the
HC is not required, the CC can be reattached after replacing the indium rings. If access
to the inside of the HC is required, the bottom plate of the HC is then detached, along
with the electrical connections to the bottom plate. Finally, the HC is removed, and
maintenance is performed.

31
 CHAPTER 4

RESULTS AND CONCLUSIONS

The current chapter presents the data obtained in phases 1 and 2 of the
experiment. The results are then compared with outside sources. Finally, future research
efforts and suggestions are discussed.

4.1 Phase 1 Results (Lumped Capacitance Method)

As has been detailed previously, phase 1 consisted of a transient cooldown from

ambient temperature to near LN2 temperature. However, a fault in the existing cryostat
caused the HC to be pressurized with pre-chilled helium gas. The helium proceeded to
cool the HC to a temperature of nearly 190 K. Therefore, results from phase 1 consist of
a HC cooldown from about 190 K to 90 K. The CC was constantly maintained at LN2
temperature by thermal contact with the bath.
The plot of the temperature history of the HC is shown in Figure 4.1. It must be
noted that the cooldown time for phase 1 was nearly one month. Figure 4.1 also shows
cooldown times calculated using the lumped capacitance method and constant effective
thermal conductivities. It can be seen that below 160 K the slope of the HC data
increases with a decrease in temperature compared to the slopes of the constant keff

curves. This shows that the effective thermal conductivity of the aerogel beads is also
decreasing with temperature.
Figure 4.2 is a graph of the effective thermal conductivity found in phase 1
(lumped capacitance method). It is clearly seen here that the effective thermal
conductivity of the aerogel beads shows a decrease with temperature. However, the slope
of keff versus T appears to decrease, suggesting a tendency for the thermal conductivity

to become constant at low temperatures (T<80 K).

32
Figure 4.1 Temperature history of the HC compared to with the lumped capacitance analysis

Figure 4.2 Thermal conductivity results from phase 1

33
 4.2 Phase 2 Results (Steady State)

Phase 2 of the experiment involved the use of a cryocooler and a steady state
temperature difference between the cylinders. Unfortunately, the original cryostat used
in phase 1 was found to have an abnormally large heat leak, which limited the minimum
temperature to 50 K. The original cryostat was replaced with a better insulated cryostat.
The cryocooler was then able to drop the temperature of the CC from room temperature
to approximately 20 K in less than 3 days. A cooldown process using the improved
cryostat is shown in Figure 4.3.

Figure 4.3 Cooldown time for phase 2

34
 Once the apparatus reached its minimum temperature a steady state temperature
difference was created. First, the inside of the HC was pressurized with helium gas to
help maintain a uniform temperature throughout. This caused a rise in the temperature of
both cylinders. The insulation space was then evacuated, and a temperature difference
was created between the cylinders by supplying power to the heater in the HC. The
temperature of the HC increased until the desired temperature difference was reached.
An example of the production of a steady state temperature difference is shown in figure
4.4.

Figure 4.4 Producing a steady state temperature difference.

35
 From this point, the HC temperature would either oscillate about a fixed
temperature or continue to rise slowly toward some maximum value. In this case, a
second order polynomial curve was fitted to a plot of the temperature increase, and the
maximum temperature was extrapolated from the curve.

Figure 4.5 Steady state data. Average temperature of 81.5 K

Figure 4.5 is a plot of the cylinders’ temperatures recorded by several temperature

sensors during one of the steady state periods. Here it can be seen that the temperature
sensors mounted on different surfaces of the cold cylinder show about a 0.5 K difference
between them. This apparent temperature difference suggests that there may be a

36
variation of temperatures on the surface of the CC. Tests to confirm the existence of a
temperature variation on the CC surface and attempts to eliminate it are discussed in the
following section. In any case, calculations were performed using sensors on the side of
both the CC and HC when available. The remaining calculations implemented the sensor
on the side of the HC and the sensor on the top of the CC. For these last calculations the
CC side sensor is believed to have been accidentally grounded, and therefore reported an
erroneous temperature value.
Six data points were produced from phase 2 of the experiment. An average
temperature of approximately 80 K was chosen for the first three data points collected.
These points were chosen in order to examine the agreement between the methods of
phases 1 and 2 near LN2. Two data points were collected near 50 K, and the remaining
data point was collected at an average temperature of about 30 K. The results are shown
in figure 4.6. As the figure shows, the effective thermal conductivity of the aerogel beads
tends to decrease with temperature. However, at 50 K and below, the thermal
conductivity begins to level off to a value near 0.14 mW/m*K.

Figure 4.6 Thermal conductivity results from phase 2

37
 Figure 4.7 Effective thermal conductivity of aerogel. Aerogel powder data from Rettelbach et al [1]
using steady state guarded hot plate apparatus. Aerogel beads’ data from current experiment.

Figure 4.7 shows a plot of the current data versus the data from Rettelbach et al
[1]. Because there have been very few attempts to measure the thermal conductivity of
aerogel beads in this temperature range, it is difficult to determine how well the current
results agree with previous data. It must be noted that the data from Rettelbach shown in
figure 4.7 are based on aerogel powder. Aerogel powder is simply the crushed form of
aerogel beads. Therefore, a direct comparison between the two may be misleading. The
aerogel powder data is included to show that the current results fall in what would appear
to be the appropriate thermal conductivity range and follow a similar trend with
temperature.

4.3 Thermal Gradient Test

Several design parameters, such as the use of copper cylinders and pressurized
helium gas, are meant specifically to produce uniform temperatures throughout the

38
cylinder. However, as has been mentioned above, as the experiment reaches steady state
unexpected temperature gradients seem to develop throughout the cylinders. The
gradient suggests that the temperature of the CC near the thermal link to the cryocooler is
0.5-2 K higher than the temperature at the side of the CC. Several steps were taken in an
attempt to alleviate this problem. First, the location of the heater controlling the
temperature of the CC was changed from the side of the CC to the cryocooler head. This
measure should eliminate any temperature gradient due to heating effects along the
cylinder. The next step was to recalibrate the temperature sensors to ensure that the
proper readings were being collected. Finally, after completing phase 2 of the
experiment, the insulation was removed, and a dry run (no insulation material) was
performed. Roughly the same gradient persisted through all the attempts to eliminate it.
A concerted effort to understand and eliminate the temperature gradient is to be made
prior to obtaining future data.

4.4 Conclusion

A new apparatus for measuring thermal conductivities of powder insulation has

been designed and tested. As expected, the use of a cryocooler has allowed for thermal
conductivity measurements over a wide range of temperatures without the use of a
cryogen to cool the apparatus. Results obtained from the current experiment fit well
within the expected range of thermal conductivities that previous research suggests.
However, more data must be collected to ensure the validity of the current results. The
apparatus seems to have successfully provided experimental data that has not previously
been recorded for aerogel beads. Several difficulties must be overcome, though, before
the apparatus can be recommended as a standard thermal conductivity measurement
instrument. The problem involving the temperature gradient throughout the cylinders
must be evaluated. Also, modifications must be made to more accurately measure gas
pressure within the insulation space. Nevertheless, the cryocooler-refrigerated, closed
concentric cylinder system shows promise as a cryogenic thermal conductivity
measurement device in the future.

39
 4.5 Suggested Future Work

The author plans to continue development of the current apparatus. Further

attempts to investigate and eliminate the temperature gradient will be taken in the near
future. A numerical model may be generated to examine temperature profiles and heat
flow through the experiment as well. Furthermore, data is to be taken using glass bubbles
and expanded perlite at temperatures from 30-100 K. Pressure variations in the
interstitial space and various interstitial gases are also to be examined.
Outside research involving the thermal conductivity of powder insulations at
cryogenic temperatures is needed to confirm the validity of the present experiment and
add to present knowledge. As mentioned above, experimental data involving pressure
and interstitial gas variation would also be very interesting. Other variants which could
be examined could include opacifiers, applied loads, or mixed insulation (i.e. MLI and
powder insulation).

40
 APPENDIX A

THEORETICAL UNCERTAINTY ANALYSIS

As a preliminary examination of the validity of the results obtained from the

current experiment, a propagation of uncertainty analysis has been performed for the
phase 2 data. The uncertainty analysis takes into account the possible error associated
with temperature sensor, heater, and distance measurements. In other words, the
uncertainty analysis encompasses solely measurement precision. Other factors, such as
cylinder alignment and temperature measurement difficulties, which are difficult to
quantify, may result in a much larger error than the present analysis suggests. More data
must be taken before a standard error analysis can be performed. A standard error
analysis would give a much better idea of the repeatability of our measurements.
The uncertainty analysis procedure was taken from [14]. The result ( r ) is
calculated using J basic measurements (X).
r = r ( X 1 , X 2,K, X J ) (A.1)

In our case, the final result is thermal conductivity (Eq. 2.9). However, several
intermediate results must be obtained (heating power, area, insulation thickness) prior to
calculating the final result. The equation used to calculate the uncertainty in any result
due to basic measurements is
1
  ∂r 2
  ∂r 
2
 ∂r  2
2

U r =  U X1  +  U X2  +L +  U XJ   (A.2)
 ∂X1   2 ∂X  ∂
 JX  

where U denotes uncertainty. Equation A.2 is used to find the uncertainty of each
intermediate result before finding the uncertainty in the thermal conductivity data.
Table A.1 shows the type of basic measurements performed, typical measurement
values, and uncertainties associated with the measurement instrument. Uncertainty due
to length measurement was obtained by taking several measurements with a micrometer.
The maximum deviation between length measurements was more than two orders of
magnitude greater than the precision of the micrometer. Therefore, the uncertainty of the

41
length measurements was given the value of the maximum deviation. Uncertainty
associated with the heating power was taken from the factory specifications of the
multimeter used to measure voltage and resistance. Uncertainty of the temperature
sensors was taken from the Lakeshore® product catalog.

Table A.1 Uncertainty values for basic measurements

Instrument Measurement Typical Value Uncertainty

Micrometer Cylinder Length 583.6 mm 0.41 mm
Micrometer Cylinder Diameter 167.3 mm 0.05 mm
Multimeter Heater Resistance 513 Ω 2Ω
Multimeter Heater Voltage 5.50 V 0.01 V
Cernox Temp Sensor Cylinder Temperature 55 K 50 mK
Platinum Temp Sensor Cylinder Temperature 55 K 30 mK

Table A.2 shows the results of the uncertainty analysis at all six steady state data
points. It is necessary to perform the analysis for each point because instrumentation
precision may fluctuate under different conditions. However, it can be seen in the table
that the uncertainty for all data remains around 1%.

Table A.2 Uncertainty values for all data points in phase 2

T avg k (mW/m*K) Uncertainty (mW/m*K) % Uncertainty

31 0.150 0.002 1.11
52.55 0.176 0.002 1.00
56.95 0.206 0.002 0.90
80.8 0.393 0.006 1.43
81.5 0.366 0.005 1.35
81.65 0.400 0.006 1.46

42
 Errors associated with other factors are dealt with separately. An adjustment was
made to account for heat leak from the HC to the CC through supports and electronics.
The correction alters the heating power to the HC and is included in the results. Several
of the current sources used in the experiment and temperature calibration were found to
have slight deviations from their intended settings. The current offsets were measured
using a high precision multimeter and taken into account in the temperature calculations.

43
 BIBLIOGRAPHY

1 T. Rettelbach, J. Säuberlich, S. Korder, J. Fricke, “Thermal conductivity of silica

aerogel powders at temperatures from 10 to 275 K”, Journal of Non-Crystalline Solids
186, pp. 278-284, 1995

2 J.E. Fesmire, S.D. Augustynowicz, “Thermal Performance Testing of Glass

Microspheres Under Cryogenic Vacuum Conditions”, Advances in Cryogenic
Engineering, Vol. 710, Issue 1, June 2004

3 S.W. Van Sciver, Helium Cryogenics, Plenum Press, New York, 1986

4 E. Péclet, Traité de la chaleur Fourth Edition, Paris, 1878.

5 R. Poensgen, “Ein technisches verfahren sur ermittlung der wärmeleitgfähigkeit

plattenförmiger stoffe”, zeitschrift des vereines deutscher ingenieure 56, 1912.

6 M. M. Fulk, “Evacuated powder insulation for low temperatures”, Progress in

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 BIOGRAPHICAL SKETCH

Name of Author: Matthew Nicklas Barrios

Place of Birth: Metairie, LA
Date of Birth: January 15, 1982

Education
Master of Science, 2006, Florida State University
Bachelor of Science, 2004, Louisiana Tech University

Research Interests
Heat and mass transfer in cryogenic engineering
Cryogenic insulation testing

Professional Experience
Research assistant, 2004-2006, National High Magnetic Field Laboratory
Engineering assistant, 2003, Audubon Engineering

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