GURU NANAK DEV ENGINEERING COLLEGE

DEPARTMENT OF MECHANICAL ENGINEERING

SYNOPSIS

THERMAL CONDUCTIVITY OF SOLID INSULATING

MATERIAL BY HOT-GUARDED PLATE METHOD

SUBMITTED TO: SUBMITTED BY:

Mr.DEEPAK DHAND SHIVAM BHANDARI-1411506
SHIVAM SEHGAL-1411507
SUSHANT KUMAR-1411526
SUVRAT JAIN-1411527
Table of contents
INTRODUCTION

1.1 THERMAL CONDUCTIVITY

Thermal conduction is the transfer of heat from one part of a body to another with which
it is in contact. Thermal conductivity is defined as ability of material to transmit heat
and it is measured in watts per square meter of surface area for a temperature gradient of
1 K per unit thickness of 1 metre.The thermal conductivity is not always constant. The
main factors affected the thermal conductivity are the density of material, moisture of
material and ambient temperature. With increasing density, moisture and temperature the
thermal conductivity increases too. Thermal conductance of a material is the heat flow
rate per unit area between two parallel surfaces of a body under steady state condition
when there is unit temperature difference between the two surfaces. Heat flow rate per
unit area between fluid on one side of the barrier to the fluid on other side under steady
state condition gives over all thermal transmittance value, when unit temperature
difference between the fluid of both side is maintained, thermal conductance is one of the
important properties of thermal insulating material, from energy saving application point
of view. A new apparatus for determining thermal conductance of building and insulating
material has been proposed, which is based upon the comparison method and depeds on
the fact that rate of heat flow across a material with high conductance will be higher than
a material with low conductance.

The determination of the thermal conductivity of building materials is fundamental for

solving problems related to building performance and user comfort. A variety of organic
insulation products have been recently promoted for their sustainability, which includes
crop-based materials. Among these some require a great thickness of implementation,
either because their very nature requires it, like for straw bales construction, or to
compensate for their lower thermal conductivity relatively to high performance inorganic
insulation materials. There are many methods for measuring the thermal conductivity of
materials, both in steady state and transient conditions. The stationary methods such as
the so-called 'guarded hot plate technique' require thermal equilibrium and thus a
significant measurement time. The boundary conditions imposed on the sample need also
to be controlled precisely. However, if these boundary conditions are met, the results
obtained by these methods are often very accurate. The transient methods provide
generally faster results and can be used on smaller samples but at the cost of lower
accuracy.

The work presented here was directed towards the conception of an apparatus for thermal
conductivity measurement in steady state, capable of performing over a wide range of
thickness. More specifically it's expected to provide reliable results on an entire straw
bale. This would be particularly useful to assess the effect of actual straws particles
orientation in the bale on final thermal conductivity. This information might be
particularly relevant for producers targeting the construction sector.
Much research has already been conducted on the thermal conductivity of straw bales.
The effect of the direction of heat flow relatively to fibers orientation has already been
highlighted. It is accepted that the more the flow is parallel to the fibers, the greater the
thermal conductivity. It is important to note however that most of available data drives
either from transient methods, from steady-state methods performed on lower thickness
re-built bales or from compressed loose material. Absolute thermal conductivity
measurements on an entire two-wired straw bale are thus still missing. The rearrangement
of the samples often observed in literature for steady-state measurement is required by
the low thickness generally imposed by commercial guarded-hot plate or heat flow meter
apparatus. As the straw particle length can generally extend to 50cm, resetting lower
thickness samples from original bale could lead to changes in structure the impact of
which is hard to quantify.
The guarded hot plate prototype presented here allows measurements on thick specimens
and offers the possibility to assess the thermal conductivity of non-altered straw bales
samples. The approach is thus complementary to existing data. It offers the possibility of
direct and easy comparison of bales from different origins or manufacturing. The original
device is described in this paper along with particular design details and challenges
encountered. Its performance will be assessed by performing the necessary numerical and
experimental tests.

At the turn of the 20th century the refrigeration industry in the United States was
becoming a commercial reality. Mechanical refrigeration technology had achieved
economic viability as a means of producing ice for cooling and was on the threshold of
moving into households as an everyday appliance. Advances were underway to provide
mechanical air conditioning for public buildings, such as theaters, department stores,
and skyscrapers. In general, the early 1900s saw the evolution of a scientific approach to
refrigeration through company sponsored research and development. It was the technical
progress in the area of cooling and heating for industrial processes and thermal comfort
that stimulated the development of thermal insulation standards at NIST.

As described in Measures for Progress: A History of the National Bureau of Standards,

Congress, at the request of the refrigeration industry, appropriated funding in 1913 for
investigation of physical constants involved in the construction and operation of large-
scale refrigeration machinery. Under Hobart C. Dickinson, D. R. Harper 3rd, and N. S.
Osborne, studies were conducted that included the investigation of insulating materials
used in the construction of large scale refrigeration structures. Of particular interest to the
mechanical engineer was the development of usable data pertaining to heat transmission
in thermal insulation needed for design purposes. For this purpose, Dickinson is credited
with independently developing an absolute method of measurement called the guarded
hot plate for homogenous slab-like materials.
LITERATURE

Dickinson and fellow NBS colleague Milton S. Van Dusen published The Testing of
Thermal Insulators [1], a classic description of an NBS study to identify the causes of
discordant experimental results for heat transfer through homogeneous solid materials
and engineering systems. The publication contained accurate determinations of heat flow
through air spaces and through 30 insulating materials; it also promoted the usage of
standard terminology for thermal conductivity measurements obtained for solid materials
and compound walls. Shortly after their first publication, Van Dusen published The
Thermal Conductivity of Heat Insulators [2], which provided detailed information on the
design and theory of operation of the apparatus, as well as additional thermal
conductivity measurements of insulating materials. Important and insightful publications
in their day, these papers are still considered recommended reading for all students of
heat transfer through thermal insulation.

At NBS the guarded hot plate quickly became the foundation for thermal conductivity
measurements of heat insulators, and this encouraged the development of other apparatus
for the measurement of thermal conductivity of solids, not only for building materials but
also for metals, refractories, and ceramics. In fact, one might argue that either directly or
indirectly the apparatus has motivated nearly eight decades of thermal conductivity work
on solids at NBS/NIST. An early spin-off was the development of the guarded hot box,
which was based on similar principles of operation and was utilized for heat transmission
measurements of simple and compound walls.

Dickinson and Van Dusen 1928:

The guarded hot plate originally developed by Dickinson and Van Dusen was refined
over several years, and about 1928 Van Dusen [4] constructed a version of the apparatus
that operated consistently until 1983. The thermal conductivity data obtained from this
apparatus, along with the data from the early NBS publications [1,2], were aggregated
with other data and tabulated in handbooks as design heat transmission coefficients for
the engineer. These design data have served the engineering community effectively for
several decades. In recent years, most of the original NBS data has been compiled in
electronic format and will be available in NIST Standard Reference Database 81, Heat
Transmission Properties of Insulating and Building Materials. However, the single most
important impact of the guarded hot plate technology was the standardization of the test
method in North America. This remarkable step has been extremely effective in reducing
the differences among laboratories with respect to thermal testing.

Henry E. Robinson 1942:

After many years of effort, NBS researcher Henry E. Robinson and others produced a
tentative edition of the test method in 1942. By joint action, the American Society of
Heating and Ventilating Engineers (ASHVE), American Society for Testing and Materials
(ASTM), American Society for Refrigeration Engineers (ASRE), and the National
Research Council (NRC) produced a Standard Method of Test for Thermal Conductivity
of Materials by Means of the Guarded Hot Plate.
In 1945, the method was formally adopted as a standard and designated ASTM Test
Method C 177. The code set up the requirements for conducting tests and for construction
of a guarded hot plate apparatus. It is interesting to note that the standards adjunct still
contains the design drawings for the 1929 version of the NBS guarded hot plate
apparatus. ASTM Test Method C 177 became the cornerstone for all thermal insulation
testing in North

Robinson and Thomas W. Watson 1947:

Robinson and colleague Thomas W. Watson in 1947, extended the temperature range of
Van Dusens guarded hot plate apparatus. A few years later, NBS completed one of the
first published laboratory inter comparisons of thermal conductivity tests of insulation
[5]. America. Over the decades, the standard test method has achieved international
acceptance as the most accurate absolute test method for the measurement of thermal
conductivity of heat insulators.This series of tests clearly demonstrated the need for
suitable means to calibrate the apparatus at industrial and other laboratories. Shortly
thereafter, a program was devised for supplying to industry measured samples of suitable
insulating materials for calibration purposes.

Dickinson 1948:
Dickinson developed a relatively simple steady-state method for thermal conductivity
measurements of refractory solids. The apparatus employed a steam calorimeter for
measuring the thermal conductivity of refractory solids from 400 C to 1500 C [3].

Robinson 1964:
In 1964, Robinson presented an elegant modification of the test method. The basic design
of a line-heatsource guarded hot plate was presented to a thermal conductivity conference
sponsored by the National Physical Laboratory in England. The design was reported in
Nature [6] as follows:
H. E. Robinson (U.S. National Bureau of Standards) discussed forms of line heat sources
that could be used as heaters in apparatus for measurements at lower temperatures on
insulating materials in disk and slab form. These new configurations lend themselves
more readily to mathematical analysis, they are more simple to use and would appear to
be able to yield more accurate results.The design was novel. In contrast to a
(conventional) guarded hot plate that used uniformly distributed circular line-heat sources
at precisely specified locations. By proper location of the line-heat-source(s), the
temperature at the edge of the meter plate can be made equal to the mean temperature of
the meter plate, thereby facilitating temperature measurements and thermal guarding. The
benefits offered by a line-heatsource guarded hot plate included simpler methods of
construction; improved accuracy; simplified mathematical analyses for calculating the
mean surface temperature of the plate as well as determining the errors resulting from
heat gains or losses at the edges of the specimens; and superior operation under vacuum
conditions.

M. H. Hahn 1971:
After Robinson, another generation of NBS researchers continued development of the
line-heatsource technology. In 1971, M. H. Hahn [7] conducted an in-depth analysis of
the line-heat-source concept and investigated several design options. The design,
mathematical analysis, and uncertainty analysis for a prototype line-heat-source guarded
hot plate were published in 1974 by Hahn, Robinson (posthumously), and D. R. Flynn
[8]. Construction of the prototype apparatus was completed in 1978 [9]. Because of the
promising results from the prototype, NIST began plans for a second, larger line-heat-
source guarded hot plate apparatus. In 1980, a ruling by the U.S. Federal Trade
Commission concerning the labeling and advertising of home insulation dramatically
accelerated the construction of this apparatus.

By 1977 more than 300 laboratories had been served, resulting in considerable
improvement in the quality of thermal conductivity data on insulating and building
materials reported in technical journals and handbooks. In 1977 the ASTM Committee C-
16 on Thermal and Cryogenic Insulating Materials recommended that this program
become an official part of the NBS Standard Reference Materials Program. Presently,
NIST provides the thermal testing community with several thermal insulation SRMs for
thermal resistance.

Hahn, B. A. Peavy, F. J. Powell, and others 1980:

With the energy crisis in the 1970s, there was growing demand for thick insulation and a
resulting concern from the Federal Trade Commission that the existing standards for
insulation measurement, based on 25 mm thick specimens, were not protecting
consumers interests. In response to concerns from industry and the Federal Trade
Commission, NBS expedited development of the one-meter line-heat-source guarded hot
plate. Near the end of 1980, the second line-heat-source guarded hot plate apparatus was
completed with the efforts of Hahn, B. A. Peavy, F. J. Powell, and others [10]. Industry
subsequently testified to Congress [11] that the improved accuracy provided savings of
$90 million per year to consumers in insulation costs alone. It is not surprising that NIST
now plans to continue developing the measurement technique into the 21st century with a
new design that will extend the current temperature range.
PROBLEM FORMULATION
1.1 GUARDED HOT PLATE

The guarded hot plate (GHP) apparatus is traditionally recognized as the only absolute
method for thermal conductivity measurement in steady-state of homogeneous materials
able to achieve a global measurement uncertainty below 2% . Its principle is to reproduce
the uniform, unidirectional and constant thermal flux density existing through an infinite
homogeneous slab-shaped specimen caught between two infinite isothermal planes. The
method is defined in an international standard under the designation 'Thermal insulation -
Determination of steady-state thermal resistance and related properties - Guarded hot
plate apparatus.

The device developed in this research is based on the single specimen apparatus(Fig.2).
their principle is the following:

The analyzed specimen is sandwiched between an electrically-heated hot plate

maintained at temperature Th and a cold plate maintained at a lower temperature Tc. The
heat dissipated by the Joule effect in the hot plate would travel to the cold plate through
the sample, but also backwards and laterally on the edges of the hot plate. Back and
lateral guard zones are then necessary to neutralize these leaks. By maintaining the
different guard zones at the same temperature Th with precise control, all unwanted
thermal transfers are indeed canceled. The hot plate is thus separated in two parts: A
heater zone (or measurement zone) of known area and heated electricity and an adjacent
guard ring heated with a different circuit. A small gap separates the two zones and a
thermopile is often used to control the temperature difference between these. The back
face of the hot plate is provided with an additional guard plate with identical dimensions
providing protection from backwards thermal fluxes. This back guard plate also has its
own heating system and is associated with appropriate temperature differential control as
in lateral gap.

Fig. 3.1. Single specimen GHP

When working well, with all three elements at exactly the same temperature th the heat
produced in the measurement plate will flow unidirectionally towards the cold plate. All
the others heat fluxes are supposed to be eliminated. An equation originally developed by
Fourier for conduction of heat in one dimension:

Where,

The thermal conductivity (W/mK)

Q heat flow or power supplied (W)
ThTc mean difference in temperature between the plates (K)
A the cross-sectional area of the plates (m2)
l the mean thickness of the specimens (m)
METHODOLOGY TO BE USED

5.1 THERMAL CONDUCTIVITY MEASUREMENT TECHNOLOGIES

The continuous desire for increasing heat transfer for various applications is one of the
most difficult challenges faced by thermal engineers. With the advancement of
technologies, heat transfer at higher rates and efficiency from small cross section areas or
over low temperature difference are causing a rise in demands. As a consequence of the
wide range of thermal properties there is no single measure method which can be used for
all thermal conductivity measurements. Desired temperature range, sample size, required
accuracy and thermal conductivity range all need to be considered when designing a
measurement apparatus (insulation materials and foams require different methods than
for materials like metals). Consequently, over the past decades a wide variety of
techniques for the enhancement of heat transfer has been suggested, where the most well-
known and promising methods are briefly described in this chapter. The emphasis will be
on techniques for thermal conductivity measurements of poorly conduction materials.

5.2 THERMAL CONDUCTIVITY MEASUREMENTS

As a definition, thermal conductivity, k, is the property of a materials ability to conduct

heat. To quantify the heat transfer process for heat conduction, the rate equation Fouriers
Law is used.

The heat flux, Q [W/m2], is the heat transfer per unit area, T/x [W/m] is the
temperature gradient and k is the transport property known as the thermal conductivity
[W/(m*K)]. The minus sign is due to the fact that the heat transfer is in the direction of
decreasing temperature [3]. Methods for measuring thermal conductivity are divided into
two different groups, namely steady-state methods and transient methods. Steady state
conditions refer to constant temperature at each point of the sample, i.e. not a function of
time. The transient methods are used to record measurements during the process of
heating up or cooling down a material or fluid. These methods have the advantage of
giving quicker measurements than the steady state methods.

5.3 STEADY STATE MEATHOD

In practice, the temperature in a steady state system is maintained by an internal heat

source, typically an electrical heater. The temperature difference is determined between
two points with a separation distance, x, inside the test specimen. Methods are classified
by the cell geometry in which heat transfer is achieved, where axial and radial systems
are most commonly used. Axial flow methods have been long established and have
provided some of the most consistent results with the highest accuracy found in literature.
The most commonly used method for axial system is the parallel plate apparatus (also
called guarded hot plate apparatus), whereas the concentric cylinder is often used for
radial systems. Steady state measuring methods can provide accurate and reliable results;
however, they have the disadvantage of being time consuming.

5.3.1 GUARDED HOT PLATE METHOD

The guarded hot plate method is versatile and commonly used method for determining
the thermal conductivity of nonmetals such as glass, ceramics, polymers and insulation
materials. There are two different types of the guarded hot plate instrument: single
specimen and two-specimen apparatus as shown in Figure 1. They are both able to
operate between 80 K to 800 K and uncertainty related to thermal conductivity
measurements of is 2% [4]. The guarded hot plate apparatus is made up by one or two
cold plates, a hot plate, a system of guard heaters and thermal insulation. The hot plate is
surrounded by guard heaters and insulation to make sure that the heat from the hot plate
only passes through the test specimen. This method is an absolute method of
measurement and it requires: i) steady-state establishment, and ii) accurate measurements
of the relevant parameters which may affect the unidirectional heat flux through the
metered area of the test specimen (e.g. heat flux in metered section, thickness of
specimen and temperatures at hot and cold surfaces).

An advantage of using a two-specimen apparatus is that an effective control of the heat

losses is achieved because of the symmetric specimen arrangement. In the single-
specimen arrangement apparatus the heat flows through the specimen and the back of the
main heater acts as a guard plane, resulting in an adiabatic environment [4]. Even though
the guarded hot plate can be effective for many practical conductivity tests, it is difficult
to carry out tests of powders. Containing the powder within the apparatus is much more
challenging compared to solid materials. Heat leaks to mechanical supports containing
the powder would make the thermal conductivity much harder to determine.

Figure 5.1: Principle sketch of guarded hot plate methods, a) two-specimen

apparatus. b) single specimen apparatus
5.3..2. AXIAL FLOW METHOD

Axial flow methods have been long established and have provided some of the most
consistent and high accuracy results reported in literature. The method is the most widely
used method for thermal conductivity measurements for temperatures below 100 K due to
minimal heat losses at low temperatures for this method. The axial flow method is most
suitable for small specimens with thermal conductivities greater than 1 W/(m*K) and for
investigations where simultaneous measurements of other transport properties are
required. The key measurement issue for this method is to reduce the radial heat losses in
the axial heat flow developed [5]. For this technique, a test specimen of unknown thermal
conductivity is sandwiched between two reference specimens of known thermal
conductivity, forming the sample column. A heater at one end of the sample column and a
heat sink in the other end, creates a temperature gradient measured through the test
specimen [5]. For an idealized case of perfect axial heat flow (no heat losses), the cross
section of the specimen and the effective separation of temperature sensors, x, is of
importance. The cross section can easily be found, however the determination of x is
more complicated due to the geometrical location of the sensor position. In most cases
the heat flow will not purely axial, and corrections for peripheral losses have to be made.
The temperature range for the axial heat flow method

5.3.3. CYLINDERICAL METHOD

The cylinder method, also referred to as the radial heat flow method, has proven to be
very successful in measurements of thermal conductivity. The concept of the technique is
to have heat flowing radially away from a central heater towards a heat sink, and from
this measure the temperature gradient inside the system.
In most cases the apparatus consists of an electrically heated wire or cylinder placed at
the central axis inside a hollow cylinder. The cylinder is typically liquid cooled. Between
the cylinder wall and the heater the specimen can be filled and, if desirable, evacuated to
a preferred pressure. Thermocouples are mounted in the specimen at least two radii near
the mid-section of the specimen. Determining the specimens thermal conductivity is
done by first passing a stable electric current through the core heater to generate a radial
heat flow outwards. This establishes a temperature difference between the thermocouples
placed in the specimen. When steady state is reached, the temperature measurements at
the thermocouples are recorded. cylinder apparatus. However, heat losses to the top and
bottom will affect temperature gradients in the specimen. These heat losses are
challenging to avoid, especially if the conductivity of the specimen is low. Therefore, a
key element for a concentric cylinder apparatus design is to make the cylinder long with
respect to the cylinder radius. This allows for a fairly uniform temperature profile to be
established in the mid-section of the cylinder, where measurements are done. However,
heat losses to the top and bottom of the cylinder should still be minimized or one should
at least be able to determine the magnitude of the losses. The main advantages of the
cylinder method are that the system can be operated with relatively simple
instrumentation as well as the wide range of applicability on specimens with both high
and low thermal conductivities. The greatest disadvantage however, is that to be able to
get as accurate measurements as possible, large specimen sizes should be used. This can
be costly and also requires longer running time to reach steady state conditions. [5] The
cylinder method can be used for temperatures in the range of 4 K to 1000 K, and
achievable uncertainty for the thermal conductivity measurements of 2% [4].

Figure 5.2: Basic elements for the cylinder method and the
temperature profile of a cross section

No standard for the cylinder method has been found. However, the International Standard
ISO 8497 [A6] covers relevant performance requirements and test procedure which can
be used for the cylinder method.

5.3.4. HEAT FLOW METER METHOD

The basic idea for the heat flow meter method is to determine the heat flux by measuring
the temperature difference across a thermal resistor during steady-state conditions. The
design of the heat flow meter method is quite similar to the single-specimen guarded hot
plate apparatus, with the difference that the main heater is exchanged with a heat flux
sensor. Heat flux sensors are thermal resistors with a series of thermocouples. In some
cases a heat flux sensor is placed at the cold plate to determine radial losses and reduce
the time duration of measurements. The method is mostly used for polymers and
insulation materials where the thermal conductivity is less than 0.3 W/(m*K) and an
uncertainty of 3% can be accomplished [4]. However, if losses in radial direction are
present the uncertainty increases rapidly. The conventional heat flow meter method
assumes one-dimensional conduction for heat transfer, i.e. no convection or radiation
present. This assumption is reasonable if the test specimen is thin in the direction of heat
flow and has a large cross-section area. The surface area for convection and radiation
becomes negligible compared to the conductive heat transfer through the specimen and
the method is suited for materials with low thermal conductivity. However, for materials
with high thermal conductivity, a thicker test specimen is required to be able to measure
the temperature difference. This results in doubt of the 8 accuracy of the measurements
since convection and radiation will then be present. Convective heat losses can be
minimized by performing the experiments under high vacuum conditions. The technique
is ideally suited for testing anisotropic specimens and is very accurate and reliable when
measuring thermal conductivity the direction on one dimensional heat flow [6].

Figure 5.3: Typical heat flux transducer heat flow meter apparatus

5.4. TRANSIENT METHOD

With the availability of modern computers and data analysis tools, transient methods for
measuring thermal conductivity have become increasingly popular. The transient methods
measures a response as a signal sent out to create heat in the test specimen. To start with,
the specimen is in thermal equilibrium with the surrounding atmosphere. Then, a short
heating pulse is given to the specimen. The change in temperature during the time of
measurement is recorded and further used for determining the thermal conductivity of the
test specimen [7]. The advantages of the transient techniques are that they generally
require much less precise alignment and dimensional and stability knowledge, but most
of all the reduced duration needed for the experiments. Typical measurement duration of
one hour for a steady-state measurement is reduced to a few minutes with a transient
method. The temperature measurement at two opposite surfaces in the specimen needed
for steady-state measurements is replaced by a temperature measurement as a function of
time at only one position for the transient methods. The design for the transient
measurement instruments are therefore quite straight forward and can also improve the
accuracy of the results. However, transient conductivity measurements typically involve
relatively complicated data analysis tools where advanced equipment is needed

5.4.1. HOT WIRE METHOD

The hot-wire method is a transient technique and is a modification of the steady-state

cylinder method geometry with radial heat flux. The method has made it possible to
measure small, transient resistance changes with high accuracy in duration of less than
one second. The hot-wire technique is based on a linear heat source with infinite length
(the hotwire) and infinitesimal diameter embedded in a test material. The hot-wire serves
as a temperature sensor as well as a heater with a constant output ensured by a power
supply (see Figure 4).An electric current of fixed intensity is generated in the wire, and
the thermal conductivity is determined from the slope from the linear temperature profile
as a function of time established from the measurement [8]. The transient hot-wire
technique has the advantages of simplicity, the ability to measure thin material sizes, the
short exposure of specimen to a high temperature and the possibility of good accuracy for
measurements. In good experimental conditions, an accuracy of less than 5% can be
achieved for conductivity measurements [7]. Furthermore, the exact dimensions of the
equipment are less important compared to other thermal conductivity measurement
techniques. Despite these advantages, the hot-wire method for thermal conductivity
measurements is rarely used for commercial tests because of the delicacy of the very thin
wire which easily snaps, especially when dealing with fluids and solids [8].

Figure 5.4: Principle sketch of the hot-wire method

5.4.2. NEEDLE PROBE

The needle probe method, also referred to as the Line-Source Method, is a variant of the
hot wire method and is capable of very fast measurements. It is suitable for both melt and
solidstate thermal conductivity measurements; however, it is not suited for directional
solid-state property measurements in anisotropic materials [9]. A needle probe is located
at the center of the test specimen, both kept at constant initial temperature. When running
experiments, a known amount of heat is produced in the needle, creating a heat wave
linearly with the logarithm of time, and this relationship can be used directly to calculate
the thermal conductivity of the test specimen. Small test samples makes it possible to
subject the samples to a wide variety of test conditions; the method can cover a
temperature range from 233 K to 673 K on materials with thermal conductivity between
0.08 to 2 W/(m*K). However, the standard for this test method, ASTM D 5930 [A13],
does not contain numerical precision and bias statement and therefore it should not be
used as a reference test method in case of dispute.

DESIGN CRITERIA

The basic design requirements for the proposed apparatus were to

Ensure solid insulations and refractories having thicknesses in the range 2550
mm,
Measure materials with thermal conductivities of up to 1 W m1 K1 and thermal
resistances from 0.05 to 3.2 m2 K W1,
Cover the temperature range from 100 to 850 C
Obtain a measurement uncertainty of about 5% over the whole range of
temperature and thermal resistance and
Fully automate the apparatus.

6.1 DESIGN AND CONSTRUCTION DETAILS

A cylindrical double sided design of 305 mm diameter was chosen in preference to a

conventional square design used near ambient temperatures. The radial symmetry of the
apparatus greatly simplifies the design of the lateral guard and the edge-guard system
required to minimize edge heat losses at high temperatures. In addition, the number of
power supply units and temperature controllers is significantly reduced, lowering
construction costs. Figure 3 shows a line drawing of the basic design for the high
temperature guarded hot plate.

The guarded heater plate consists of two 305mmdiameter plates about 10 mm thick
bolted together. The plates are machined from Inconel 600, a high temperature nickel
alloy with very good dimensional stability at temperatures up to at least 900 C. As with
the heated cold plates, one plate is machined with grooves to provide a location for the
guard and metering area heating elements. The second plate has shallow grooves cut into
one face to allow a thin wire, differential thermocouple to be wound across the guard
metering gap. The central metering area of the plates is separated from the concentric
guard area by a 2 mm gap cut through the plates centered on a 150 mm diameter circle,
three small bridging pieces being left in position to provide mechanical support for the
metering area. The outer surface of each plate is machined flat to within better than 0.05
mm across the whole face. Grooves are machined into the faces to take sheathed mineral
insulated thermocouples.

The two chilled plates act as heat sinks for heat flowing through the specimen. Each
consists of a 30 mm thick aluminum alloy plate with cooling channels cut concentrically
into the top surface. Fluid from a temperature controlled bath is pumped through the
channels to maintain the temperature of the plate at 20 C. Heated cold plates are
separated from the chilled cold plates by a thick block of calcium silicate insulation.
Since the chilled cold plate runs at 20 C, the thermal conductivity of insulation and
specimen and the temperature drop through the specimen determine the lower
temperature limit of the heated cold plate. The two heated cold plates are made to a

Figure 6.1: The NPL 305 mm diameter high temperature guarded hot-plate apparatus.

guarded design with the central area surrounded by a concentric lateral guard area. The
10 mm thick plates are made from Inconel alloy. Sheathed heating elements are set into
grooves machined into the back surface of each plate both in the central area and in the
guard section. The surface adjacent to the specimen is machined flat to within better than
0.05 mm across the face and has grooves to take four mineral insulated NicrosilNisil
(Type N) thermocouples and a differential thermocouple.
 The edge-guard assembly consists of two semi-cylindrical Inconel 600 plates that
surround the specimen stack to leave a gap of about 25 mm between the specimens and
the edge guard. The edge-guard plates extend at least 30 mm beyond the heated cold
plates when 50 mm thick specimens are being measured, the overlap obviously being
greater for thinner specimens. Separate heating elements are wound onto the outside of
each guard plate and connected in series to a power supply. The outer surfaces of the
guard plates are insulated with micro-porous insulation encased in a stainless steel lining,
the thickness of insulation being sufficient to keep the temperature of the stainless steel
below about 60 C when the edge guard is at 850 C.

Type N thermocouples are used throughout the apparatus in the form of mineral insulated
thermocouple wire in a NiCroSil sheath of 1.5 mm diameter and of sufficient length to
allow the sheath terminations to be made at room temperature. Samples from the batch of
sheathed thermocouples were calibrated by the NPL Temperature Standards section. The
data acquisition and temperature control systems and software routines are similar to
those already described above for the 610 mm guarded hot plate.

The edge-guard assembly incorporates a hinge system that allows the two semi-
cylindrical parts of the guard to swing open for easy access to the specimen stack for
changing specimens. When it has been assembled, the cold and chilled plate assembly
rests on top of the specimen stack and moves up and down with the expansion and
contraction of the apparatus during a measurement. Movement of the upper chilled plate
is monitored with reference to the base plate of the apparatus using three linear
displacement transducers. The transducer system is calibrated to give the thermal
expansion of the specimens by calibrating out the expansion of the apparatus using
micro-porous silica glass specimens that have a comparatively low coefficient of
expansion. Checks are made using specimens whose coefficients of expansion are known
and it is found that the method provides a good first-order correction to take into account
the expansion of the specimens.
PROCEDURE

The specimens are placed on either side of the heating plate assembly, Uniformly
touching the cooling plates. Then the outer container is fitted with loose fill
insulation such as glass wool supplied in small cloth packets.

Connect the power supply to the unit. Turn the regulator knob clockwise to power
the main heater to any desired value.

Adjust the guard heaters regulator so that the main heater temperature is less than
or equal to the guard heater temperature.

The cooling circuit is started. Allow water through the cold plate at steady rate.
Note the temperatures at different locations when the unit reaches steady state.
The steady state is defined, as the temperature gradient across the plate remains
same at different time intervals.

Calculated input is given to central and guard heaters through separate single
phase supply lines with a dimmer state in each line desired temperature.

Allow 30 60 minutes for the temperatures to stabilize.

The guard heater input is adjusted in such a way that there is no radial heat flow
which is checked from thermocouple readings and is adjusted accordingly. The
input to the central heater (current and voltage or watts) and the thermocouple
readings are recorded every 10 minutes till a reasonably steady state condition is
reached. The readings are recorded in the observation table.

The final steady state values are taken for calculations.