Journal of ELECTRONIC MATERIALS, Vol. 39, No.

9, 2010
DOI: 10.1007/s11664-010-1265-6
Ó 2010 TMS

Thermal Conductivity Measurements on Challenging Samples

by the 3 Omega Method

A. JACQUOT,1,2 F. VOLLMER,1 B. BAYER,1 M. JAEGLE,1 D.G. EBLING,1

and H. BÖTTNER1

1.—Department of Thermoelectric Systems, Fraunhofer-Institut für Physikalische Messtechnik IPM,

Heidenhofstraße 8, 79110 Freiburg, Germany. 2.—e-mail: alexandre.jacquot@ipm.fraunhofer.de

The 3 omega method is the best established method for measuring the thermal
properties of thin films (>100 nm) and nanowires. Theoretically, the method
could be applied to many more types of samples, leading to new knowledge,
but to date little effort has been made to extend its applicability. An enabling
set of technologies has been tested at the Fraunhofer-IPM. The technologies
developed encompass a new design of microheater, the measurement of bulk
samples with a prefabricated microheater on adhesive tapes and polymer
sheets, the measurement of tiny bulk samples glued to the underside of
polymer sheets, a fully automated experimental setup, and a new numerical
tool adapted to the new type of heater. The new design of microheater and
software were validated using float glass as a reference material. A micro-
heater on adhesive tape was used to measure accurately the thermal prop-
erties of sintered thermoelectric materials. The thermal conductivity of a very
small melt-spun nanocomposite sample glued to the underside of a Kaptonä
sheet was measured. The potential of the new design of microheater to mea-
sure very thin (nm) films is discussed.

Key words: 3 Omega, thermal properties measurement, thermal

conductivity, heat capacity, SPS materials, bismuth telluride,
bismuth antimony telluride

INTRODUCTION almost impossible to isolate the microheater prop-

erly from the sample. Practicable ways of making
Since Cahill pioneered the 3 omega method for
the insulating layer are by sol–gel techniques or by
measuring bulk insulating material about 20 years
using postbaked photoresists, but these films do not
ago,1 it may be pointed out that very few bulk
reliably prevent leakage. If the insulating film is
thermoelectric materials have been measured using
made thicker, a lower frequency (1 Hz) has to be
it. The major field of application for the 3 omega
used so that the thermal wave penetrates deep into
method is rather the measurement of relatively thin
the thermoelectric material, making the contribu-
films or superlattices2–4 and nanowires,5 where its
tion of the insulating film to the temperature rise
accuracy is undisputed. Still, the 3 omega method is
smaller. In fact, nobody uses low frequencies, not
very appealing for measurements in a cryostat,
because it is experimentally impossible, but because
because the method uses between two and up to four
in this case, the thermal wavelength may be com-
electrical contacts to measure the thermal proper-
parable or larger than the microheater length itself.
ties, a record in simplicity that remains unbeaten to
In this case, the assumption that under the heater
this day. If the 3 omega method is not the work-
the heat transfer is two dimensional is no longer
horse for the measurement of thermal conductivity
valid. Recently, a microheater approximately in the
of bulk thermoelectric materials, it is because it is
form of a spiral was presented, but the numerical
tools failed to account for all the features of the
(Received July 10, 2009; accepted May 3, 2010; phase and amplitude plotted as a function of fre-
published online May 25, 2010) quency.6 In this article the heat transfer below the

1621
1622
Fig. 1. Exploded assembly drawing of the spiral-like microheater on its substrate, design of the microheater, and cross-sectional view of the finite
elements (meshing) used to calculate the heat transfer beneath the microheater. The four pads are the connections for current leads (I+,I) and
voltage leads (V+,V). The hatched area of the exploded view is the plane of the cross-sectional view of the meshing.
spiral-like heater is simulated by the heat transfer
below concentric rings instead of modeling the
spiral-like heater as a disk. Since a ring has an axis
of symmetry and since the asymmetry of the spiral-
like heater is negligible, this symmetry can be used
to calculate the three-dimensional (3D) heat trans-
fer using a two-dimensional (2D) mesh (Fig. 1), and
the numerical simulation of Jacquot et al.7 can be
easily extended. The method will be designated the
concentric 3 omega method. The concentric method
is tested on float glass and then used to measure the
thermal conductivity of melt-spun spark plasma
sintered (SPS) (Bi,Sb)2Te3. Since there is a demand
for measurement systems and methods for mea-
suring small samples, the Fraunhofer-IPM
extended the on-membrane method introduced by
Jacquot et al.8 by using an alternating current (AC)
instead of a direct current (DC) in the microheater.
Preliminary results of measurements on Kaptonä
sheet, Polyamide films, and melt-spun (Bi,Sb)2Te3-2
mol% PbTe nanocomposite are presented.9,10
EXPERIMENTAL PROCEDURES
The measurement system used for this work
is a further development of a previously presented
system.11 Validation was carried out by measur-
ing the thermal conductivity of quartz glass
(1.31 W m1 K1) from Schott Lithotec (Lithosilä).
The system can perform highly automated mea-
surements. The instrumentation is used together
with a cryostat from Cryovac, thus enabling mea-
surements between 70 K and 700 K. The sample
holder for the cryostat was developed at the
Fraunhofer-IPM. Measurement of the cross-plane
Jacquot, Vollmer, Bayer, Jaegle, Ebling, and Böttner
Seebeck coefficient is also possible with this mea-
surement system.12 For room-temperature mea-
surements, the Fraunhofer-IPM uses a sample
holder with Peltier elements for temperature regu-
lation. In this case the temperature does not change
by more than 1 mK and stabilizes very quickly.*
Measurements are made in vacuum. This is impor-
tant when the measurement is done on membranes
or at high temperatures. The numerical tool that
comes with the measurement system is an improved
version of the Windows-based software developed by
Jacquot et al.7 The material properties used in the
numerical simulation are listed in Table I.
CONCENTRIC METHOD
Validation
A bolometer with the shape shown in Fig. 1 was
fabricated by photolithography on a sample made of
float glass. The diameter of the spiral-like heater,
the strip width, and strip separation were 920 lm,
20 lm, and 40 lm, respectively. The temperature
amplitude (a) and phase (b) were measured with a
power per unit area of 7521 W m2 and plotted as a
function of the inverse square root of frequency
(Fig. 2). The agreement between experiment and
the simulation done with the meshing shown in
Fig. 1 is very good over the whole frequency range
for both amplitude and phase. Hence, it can be
*The temperature controller is a Thorlab TED350. Depending on
the temperature sensor used, temperature stability is better than
1 mK over 24 h, and measurement resolution of 0.001°C and
temperature accuracy of ±0.1°C are achievable (see technical
data of the TED350 available online).
Thermal Conductivity Measurements on Challenging Samples by the 3 Omega Method
Table I. Thermophysical properties at room temperature of materials used in the numerical simulations
Thickness
(lm)
Float glass 1000
Kaptonc 25
Siliconc 500
Adhesive film 15
Meltspun-SPS-(Bi,Sb)2Te3 1500
Polyamidee 10
(Bi,Sb)2Te3 films 1.1
Nanocomposite (Bi,Sb)2Te3-2 mol% PbTe 40
a
The density and heat capacity of float glass are assumed to be not far from the properties of LithosilTM quartz glass; bOur work (best
curve fitting); cData from Ref. 7; cData taken from www.MatWeb.com and assumed to be the same as the properties of the silicone-based
fluid Durathermä; dData taken from www.MatWeb.com and assumed to be the same as those of Bi2Te3; eData from Ref. 6.
Fig. 2. Amplitude (j) and phase (d) measured at room temperature
with a spiral-like microheater on float glass. The solid lines are cal-
culated with the data of Table I.
concluded that it is correct to simulate the heat
transfer of a microheater in the form shown in
Fig. 1 with concentric rings. This is a remarkable
result since the spiral-like heater is not perfectly
symmetric whereas concentric rings are. Neverthe-
less, taking into account eight rings and taking the
average diameter of the spiral-like heater seems to
be sufficient. The new microheater design and
numerical tool may also simplify and greatly
improve the accuracy of the measurement of ther-
mal properties (heat capacity and thermal conduc-
tivity) of solids and liquids.13,14 The measurement of
a liquid by the 3 omega method as proposed by
Birge and Nagel13 will be more accurate with a
spiral-like heater because of the decoupling between
the microheater width, necessarily large to measure
the heat capacity accurately, and the electrical
resistance of the microheater, which should be kept
to a reasonable level (larger than 10 Ohm). Since it
is possible in the simulation to put the microheater
between the material labeled 2 and 3 in Fig. 1, the
simulation can be used for the interpretation of
1623
Density Thermal Conductivity Heat Capacity
(kg m23) (W m21 K21) (J kg21 K21)
2450a 1.07b 790a
1090 0.28 1420
2330 150 711
830d 0.13b 1690d
7730d 1.00b 160d
1140 0.226 1500
7730d 2.06b 160d
7730d 1.80b 160d
measurement results done on liquids if the proper-
ties of the material labeled 1 and 2 are set to those
of the liquid. The measurement is simplified
because it is possible to measure not only the heat
capacity but also the thermal conductivity with the
same spiral-like heater. It was noticed in Ref. 6 that,
when the thermal wave penetration depth is much
smaller than the diameter of the spiral-like heater
and smaller than the distance between two rings,
the integral form of the Cahill formula gives a rea-
sonable value for the measured amplitude. This
means that, if the strip width of the spiral-like
heater is much smaller than the distance between
two rings, a frequency range exists where the line-
arized (Eq. 1) form of the Cahill formula may also
work quite well. In this case, the slope of the real
part of the temperature amplitude plotted as a
function of the logarithm of the frequency may be
used to extract the thermal conductivity. If the
thermal wave is much larger than the distance
between two rings but much smaller than the
diameter of the spiral-like heater, the product of
heat capacity and thermal conductivity can be
extracted by plotting the amplitude as a function of
the inverse square of frequency.13 To date, the state
of the art was to measure the heat capacity using a
wide heater and the thermal conductivity using a
much narrower heater,14 the equations used to
extract the heat capacity and the thermal properties
from the measurement results being only valid
in two extreme configurations and over a very
restricted frequency range almost impossible to
determine experimentally.
Melt-Spun SPS (Bi,Sb)2Te3
A bolometer in the shape shown in Fig. 1 was
fabricated by photolithography on a sample made of
Kapton adhesive tape. The microheater had the
same geometry as the one used for the measure-
ment done on float glass. The adhesive tape was
stuck to a silicon wafer, and the temperature
amplitude (Fig. 3a, curve S) and phase (Fig. 3b,
1624
Fig. 3. (a) Amplitude and (b) phase measured at room temperature
with an adhesive tape on which a spiral-like microheater was
microfabricated, when the adhesive tape is on a silicon wafer (S) or
SPS material (T).
curve S) were measured at a power per unit area of
3451 W m2 to obtain a comparison between the
experiment and simulation of the properties of the
adhesive film (glue underneath Kapton tape), since
the thermal properties of Kapton and silicon are
known (Table I). Then, the adhesive tape was stuck
to the sintered sample, and the temperature
amplitude (Fig. 3a, curve T) and phase (Fig. 3b,
curve T) were measured again. We emphasize that
just crude polishing of the sample is required. It is
not necessary to microfabricate the microheater on
the sample surface. When the frequency is lower
than 0.4 Hz, the difference between curves S and T
is large, especially for temperature amplitude. The
additional temperature rise of curve T compared
with curve S is a function of the thermal properties
of the sintered material. Using the 3 omega method,
a thermal conductivity of 1 W m1 K1 has been
measured, which is in very good agreement with a
result obtained by the laser-flash method by
Netzsch (1.03 W m1 K1). The 3 omega method
may offer the additional advantage of being able to
measure the anisotropy of the thermal conductivity
Jacquot, Vollmer, Bayer, Jaegle, Ebling, and Böttner
Sample
(1)
(3)
(2)
(4)
Fig. 4. (1) A supporting Kapton sheet with two integrated micro-
heaters (metal strips with four electrical contacts) prefabricated.
(2) The sample of which the thermal conductivity has to be measured
was glued with a polyamide film onto the underside of the Kapton
sheet just underneath one microheater. (3) The assembly (mem-
brane + sample) was then fixed with silver paint onto an aluminum
plate (frame) having two rectangular openings so that the metal
strips pass exactly across the middle of these openings. (4) The
comparison between the measurements made with both micro-
heaters enables the determination of the thermal conductivity of the
sample.
with only one sample, for example, by using two
spiral-like heaters of different diameter and/or by
making the measurement and interpreting the
results over a broad frequency range. Since the
diameter of the spiral-like heater may be much
smaller than the straight strip currently used
(length between 2 mm and 4 mm), much smaller
samples can be measured.
ON-MEMBRANE METHOD
Preliminarily results are presented for the first
measurements of thermal conductivity of a flake
(1.5 mm 9 2 mm 9 0.04 mm) of (Bi,Sb)2Te3-
2 mol%PbTe made by melt-spinning.9,10 A micro-
heater in the form of a metallic strip 5 mm long and of
width 10 lm has been microfabricated by photoli-
thography on a Kapton sheet 50 lm thick (Fig. 4).
The nanocomposite was glued with a polyamide
spray to the underside of the Kapton sheet. The sheet
was glued with silver paint onto a frame made of
aluminum with an opening of 4 mm 9 2 mm. The
distance between the voltage (1 mm) wires connected
to the microheater was chosen to be significantly
smaller than the length of the flake. The real part of
the amplitude and the phase shift were measured at a
heating power per unit length of 2 W m1 and are
shown in Fig. 5a and b. A Kapton sheet, a Kapton
sheet with a 10-lm- to 20-lm-thick polyamide film,
and a Kapton sheet with a 1.1-lm-thick (Bi,Sb)2Te3
film sputtered on the underside have also been mea-
sured (Fig. 5). The material underneath reduces the
temperature rise at low frequency (4 Hz). At higher
frequency, the thermal wavelength is smaller than
Thermal Conductivity Measurements on Challenging Samples by the 3 Omega Method 1625

Fig. 5. (a) Amplitude and (b) phase measured at room temperature and calculated (c and d) with the data of Table I in the case of the
microheater on a membrane. The materials underneath the membrane are listed in the insert to (a).

the thickness of the Kapton sheet, so the thermal
wave is not affected by the material underneath. The
1.1-lm sputtered film cannot be measured accurately
with the experimental configuration used here
because of the large difference in thickness between
the Kapton sheet (50 lm) and the sputtered layer
(1.1 lm). This conclusion is also valid for the poly-
amide film. Since the thickness of the flake of nano-
composite is comparable to the thickness of the
Kapton sheet, it decreases the temperature ampli-
tude significantly enough to be measured with good
accuracy. Numerical simulations have been per-
formed to obtain greater insight into these experi-
mental results (Fig. 5c and d). There is good
semiquantitative agreement between experiment
and simulation for frequencies down to 0.1 Hz. The
thermal conductivity obtained (1.8 W m1 K1) is
just slightly lower than that measured on SPS
material of the same composition.10
Below 0.1 Hz the thermal wavelength is compa-
rable to the size of the opening. There is heat flow
along the length of the membrane that is not taken
into account in the numerical simulation. Heat loss
by radiation could also decrease the temperature
amplitude, since the amplitude measured at low
frequency is rather high. Obviously, better experi-
mental conditions can be found for this pioneering
experiment.
DISCUSSION OF THE MEASUREMENT
OF NANOMETER-THICK FILMS
The effect of the width of a microheater in the
form of a strip on the measurement accuracy of thin
films can be illustrated by the effect of a change in
microheater width on the real part of the complex
temperature rise ðDTÞ~ arising from the substrate (1)
and from the film (2)1,11,15:
1626
 
Pl 1 1 k the form of sintered materials or tiny flakes. Pho-
~
ReðDTÞ ¼  lnð4pf Þ þ ln þ 0:92 ; (1)
pk 2 2 qcp b2
Pl  e
ReðDT~F Þ ¼ ; (2)
2b  kF
where Pl is the heating power per unit length, k is
the thermal conductivity of the substrate, f is the
frequency of the current in the microheater, 2b is
the strip width, q and cp are the density and heat
capacity of the substrate, e is the film thickness, and
kF is the cross-plane thermal conductivity of the
film.
The temperature rises in the substrate and film
are functions of the strip width and increase
when the strip width decreases. Nevertheless, the
increase of temperature in the substrate is a loga-
rithmic function of the width, whereas the temper-
ature rise in the film is a much stronger (1/2b)
function of the width. As a rule of thumb, the best
accuracy is obtained with a narrow strip as long as
it is possible to make a narrow strip. By photoli-
thography, it is possible to make strips with well-
defined widths equal to or larger than 10 lm. Very
accurate (5%) measurements can be done in this
case when the film is no thinner than 100 nm. By
e-beam lithography it is possible to make the strip
100 times narrower. Truly nanometer-thick films
should be measurable with very good accuracy. If
this has not been done up to now, it is because it was
not possible to make the microheater long enough for
the heat transfer to be two dimensional. In addition,
the electrical resistance of the microheater would
have been much too high. A microheater in the form
of a ring can be easily made by e-beam lithography,
and the measurement results can be easily inter-
preted with the numerical tool presented in this
article. The resistance of the microheater may be
easily tuned by varying the diameter of the ring.
CONCLUSIONS
It has been demonstrated experimentally that the
3 omega method can be used to measure the ther-
mal properties of bulk thermoelectric materials in
Jacquot, Vollmer, Bayer, Jaegle, Ebling, and Böttner
tolithography is no longer needed by the end-user,
and there is no longer any need for electrical insu-
lation directly on measured materials even if the
materials are electrically conducting. This should
increase interest in the 3 omega method and enable
measurement of thermal properties from low to
moderate temperatures and at lower cost. Micro-
heaters in the form of rings and the numerical tool
presented herein may enable measurement of
extremely thin films or very small samples in the
very near future.
ACKNOWLEDGEMENTS
This work was supported by the German Federal
Ministry of Education and Research (BMBF) within
the Joint Project VEKTRA and by the Fraunhofer-
Gesellschaft, Grant Number: WISA 815 020.
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