REVIEW
Thermoelectrics
A Brief Review on Measuring Methods of Thermal
Conductivity of Organic and Hybrid Thermoelectric
Materials
Hanfu Wang,* Weiguo Chu,* and Guangming Chen*
Organic and hybrid thermoelectric (OHT) materials have attracted increasing
research interest over the past decade. Thermal conductivity measurement
plays a critical role in evaluating and improving the thermoelectric perfor-
mance of various types of these novel materials, ranging from bulks to low-
dimensional structures. Commonly used and newly developed techniques
for thermal conductivity measurement, most of which have been applied to
OHT materials in recent years, are reviewed. They are categorized as steady-
state methods, time-domain methods, or frequency-domain methods. The
operating principles, merits and limitations, technical issues, and application
examples for each technique are also discussed.
1. Introduction
In recent years, organic and hybrid thermoelectric (OHT) mate-
rials have attracted tremendous attention due to their easy
process ability, low cost, and low thermal conductivity.[1–6] The
thermoelectric performance is generally described by a dimen-
sionless thermoelectric figure of merit ZT
S 2σ T
ZT = (1)
κ sion coefficient associated with the polymer materials[9] can
where S, σ, and κ are the Seebeck coefficient, electrical con-
ductivity, and thermal conductivity, respectively; T is the tem-
perature. A good thermoelectric material should possess a high
power factor (S2σ) and a low thermal conductivity. Reliable
evaluation of these properties with proper characterizing tech-
niques is crucial for developing advanced thermoelectric mate-
rials. Tremendous efforts have been paid to improve the existing
Prof. H. Wang, Prof. W. Chu
CAS Key Laboratory of Nanosystem and Hierarchical Fabrication
CAS Center of Excellence for Nanoscience
National Center for Nanoscience and Technology
Beijing 100190, P. R. China
E-mail: wanghf@nanoctr.cn; wgchu@nanoctr.cn
Prof. G. Chen
College of Materials Science and Engineering
Shenzhen University
Shenzhen 518055, P. R. China
E-mail: chengm@szu.edu.cn
The ORCID identification number(s) for the author(s) of this article
can be found under https://doi.org/10.1002/aelm.201900167.
DOI: 10.1002/aelm.201900167
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measurement methods and to invent new
strategies to fulfill the needs of character-
izing diverse samples ranging from bulk
materials to low dimensional structures.[7,8]
For the three properties that are used to
determine the ZT value, the characteriza-
tion of the thermal conductivity usually
poses a substantial challenge. This is mainly
due to the fact that unwanted heat losses
(e.g., from blackbody radiation) and thermal
contact resistance (e.g., from the interface
between the sample and the temperature
sensor) can more or less bring extra errors
to the final results. Measures must be taken
to reduce or to quantify these influences.
The OHT materials generally share same characterization
methods of the thermal conductivity with their inorganic
counterparts, except that the measurement temperature for
the OHT materials is usually lower than 473 K. However,
special attention should be paid when applying these tech-
niques to the OHT materials due to the fact that the meas-
urement accuracy and reliability are significantly affected by
their unique mechanical, morphological, thermal, and optical
properties. For example, the relatively large thermal expan-
cause thermal contact problem in the steady-state methods,[10]
especially when a large temperature difference is exerted. It
is also known that certain polymers and polymer composites
may become mechanically unstable at cryogenic tempera-
tures.[11] Hence, one should make sure that measurements at
very low temperatures do not cause the samples to deteriorate
physically (i.e., generating cracks or fallen pieces[12]). Surface
roughness of the OHT materials is another concern, which
is usually not easy to control in the fabrication step. It may
eventually bring difficulty to the sample preparations for the
conventional 3ω[13] or the time-domain thermoreflectance
(TDTR)/frequency-domain thermoreflectance (FDTR) meas-
urements.[14] Similar technical issues which are relevant to
the characterizations of the OHT materials will be discussed
briefly in this paper. On the other hand, among these tech-
niques some appear to be more critical to the understanding
of the thermal transport in the OHT materials. For example,
one important feature associated with the OHT materials is
the thermal conductivity anisotropy, which has become an
important research subject in the OHT community.[4,6] There-
fore, this review will also put special emphasis on the tech-
niques capable of measuring the in-plane and cross-plane
thermal conductivity of the samples.
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Based on the time dependence of the heating sources, the

techniques for charactering the thermal conductivity can be Hanfu Wang obtained his
categorized into two major groups, i.e., steady-state methods Ph.D. from the University of
and transient methods.[15] For the steady methods, a con- Minnesota at Minneapolis,
stant temperature gradient is created along the sample by USA in 2001 and pursued his
applying a time-independent heat flow. The thermal conduc- postdoctoral work at Pacific
tivity is then deduced with the knowledge of the amount of Northwest National Laboratory,
heat conducted through the sample, the resulted tempera- USA from 2001 to 2004. He
ture difference, and the sample dimensions. As for the tran- joined the National Center for
sient methods, a time-dependent heat flow is imposed on the Nanoscience and Technology,
sample and the corresponding thermal response is measured. China as an associate pro-
The transient methods can be further divided into two sub- fessor in 2004. His major
categories: time-domain methods and frequency-domain research interest is thermoelec-
methods. In the time-domain methods, the thermal response tric materials and devices.
is recorded and analyzed as a function of time right after the
sample being perturbed by a heating pulse. Unlike the time-
Weiguo Chu obtained his
domain method, the frequency-domain methods usually
Ph.D. in 2000 from Harbin
exert periodic thermal perturbation which in turn produces a
Institute of Technology. In
periodic signal whose phase and amplitude will be analyzed.
2004, he joined the National
Some transient methods (such as laser flash method) do not
Center for Nanoscience and
directly measure the thermal conductivity due to the difficul-
Technology, China. Currently,
ties of accurately measuring the heat flow conducted through
his research interests are
the sample. In these cases, it is often convenient to measure
quite broad, including energy-
the thermal diffusivity α or thermal effusivity e instead. The
related nanomaterials and
thermal diffusivity of a material measures the rate of the heat
devices, optical metasurfaces,
transfer in response to a temperature change, while the effu-
nanosensors, and micro/
sivity characterizes its ability to exchange thermal energy with
nanofabrication technologies.
its surroundings.[15] The relation of the three transport proper-
ties is expressed as
Guangming Chen obtained
κ = C Vα (2)
his Ph.D. in 2000 from
e = κ CV (3) Institute of Chemistry,
Chinese Academy of Sciences
(ICCAS) and pursued his
κ =e α (4)
postdoctoral work at National
Institute for Materials
where CV is volumetric heat capacity (J m−3 K−1), which can Science, Japan (NIMS) from
be determined from density ρ (kg m−3) and specific heat Cp 2000 to 2002. He worked
(J kg−1 K−1) through CV = ρCp. Therefore, κ can be determined at ICCAS between 2002
if any two quantities among α, e, and CV are known. and 2018. He then joined
The measurement techniques for the thermal conduc- Shenzhen University as a
tivity can also be divided into contact methods and noncon- distinguished professor. His current research interest is
tact methods, according to whether the sample is directly thermoelectric composites.
contacted with the heat source and the temperature sen-
sors. The noncontact methods generally involve with optical
heating and optical sensing. An advantage of the noncon-
tact methods is that the thermal contact resistance between 2. Steady-State Methods
the sample and the heat source/temperature sensors is
eliminated, which makes the high-accuracy measurement This section will cover six measurement techniques, namely,
possible. the absolute method, the parallel thermal conductance method,
In this work, we review commonly used and newly devel- the comparative method, the Völklein method, the method
oped techniques for the thermal conductivity measurement. based on microfabricated suspended devices, and the steady-
Most of them have been applied to the OHT materials in state infrared (IR) thermography. The bulk samples can be
recent years. The review is divided into three main sections measured by the former three techniques, while the in-plane
focused on steady-state, time-domain, and frequency-domain thermal conductivity of the thin films by the latter three ones.
methods. The operating principles, merits and limitations, Among these methods, the infrared thermography is a noncon-
technical issues, and application examples related spe- tact absolute method, while all others are usually configured as
cifically to the measurement of the OHT materials will be the contact methods. The advantages and limitations of these
discussed. techniques are summarized in Table 1.

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Table 1. Summary of the steady-states methods presented in this review for measuring the thermal transport properties of the OHT materials.
Methods Measured quantities
Absolute method Thermal conductivity of bulk materials
Parallel thermal Thermal conductivity of bulk materials
­conductance method
Comparative method Thermal conductivity of bulk materials
Völklein method In-plane thermal conductivity of films
Microfabricated Thermal conductivity of nanowires or
­suspended device nanotubes along their axial direction,
or thin film stripes along their in-plane
direction
Steady-state infrared Thermal conductivity of films along the
thermography in-plane direction
2.1. Absolute Method
Figure 1 illustrates a typical experimental configuration of the
absolute method for measuring the thermal conductivity of
bulk materials in low temperature region. The bar-like or rod-
like sample is attached with a heater at one end, while another
end of the sample is anchored to a heat sink. Two temperature
sensors, which could be thermocouples or resistance thermom-
eters, are placed along the sample to measure the temperature
difference ΔT. The sample is heated by a constant heating
power. When the temperature distribution along the sample
reaches the steady state, ΔT is recorded and the thermal con-
ductivity κ is calculated by
∆T
qs = κ A
L
where qs is the heat flow through the sample, A is the cross-
sectional area of the sample. L is the distance between the two
temperature sensing locations.
Since heat exchanges between the sample and surround-
ings can happen through radiation, gas convection, and con-
duction (e.g., through lead wires), the heat power dissipated
from the heater may significantly differ from qs. Proper steps
should be taken in order to minimize the parasitic heat losses.
For example, a thermal shielding is often installed around the
sample to reduce the radiation exchange. To minimize the gas
convection, the test setup is often installed in a vacuum envi-
ronment. To reduce the heat losses due to conduction, it is
preferable to use long and thin lead wires made of low thermal
conductivity materials for the heaters and temperature sensors.
The thermal contact resistances between the sample and the
heater/sink as well as between the sample and the temperature
sensors should be minimized.[16]
It has been found that the radiation heat losses may cause
substantial measurement errors at higher temperatures (e.g.,
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Merits Limitations
Easy implementation; Can obtain κ; Possible to Heat losses and thermal contact resistances need
be measured with S and σ to be considered
Can obtain κ; Easy implementation The thermal conductance of the sample holder
needs to be small; Issue of thermal contact
resistance
Can obtain κ; No need for measuring heat flow; Heat losses and thermal contact resistances need
Possible to be measured with S and σ to be considered
Substrate effect eliminated; Prefabricated metal The thermal conductance of the bare membrane
stripes and insulation layers; Compatible with needs to be small when compared to that of the
various film deposition techniques; Can obtain κ sample
directly; Possible to be measured with S and σ
Capable of characterizing the nanoscale or Extensive microfabrication works; Difficulty in
microscale samples; Substrate effect eliminated; transferring as-prepared sample to the device;
Can obtain κ directly; Possible to be measured Issues of thermal contact resistance and measure-
with S and σ ment sensitivity need to be considered
Rapid and noncontact; Can obtain κ directly; Needs sample with substantial optical absorptance
Applicable to sub-micrometer thick films and large emissivity; Extensive calibrations of the
experimental setup
(5)
Figure 1. A typical experimental configuration of the absolute method
for measuring the thermal conductivity of bulk materials in the low-­
temperature region.
above 200 K).[17–19] Therefore, careful calibrations of the
apparatus or proper corrections of the radiation heat losses
are essential for reliable measurements. With the configura-
tion shown in Figure 1, Kovalsky et al. have measured the
thermal conductivity of an organic–inorganic hybrid perov-
skite CH3NH3PbI3 from 7 to 300 K.[20] The sample was in the
form of pellet mechanically pressed from the CH3NH3PbI3
powders. The data at temperatures above 50 K are in rea-
sonable agreement with those of a similar polycrystalline
sample measured by Pisoni et al. with the steady-state com-
parative method that will be discussed in Section 2.3.[21] In
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Figure 2. Two configurations for thermal conductivity measurement according to the ASTM
D5470 standard.
both studies, the thermal conductivity at room temperature is
around 0.3 W m−1 K−1.
Efforts have been made to carry out the thermal conductivity
measurement above room temperature with the same experi-
mental configuration. Zaitsev et al. have demonstrated an appa-
ratus which employed a radiation shield thermally anchored
to both the heater and the heat sink to simulate a t­emperature
gradient that existed in the sample.[22] To further reduce the
radiation heat loss, the space between sample and the heat
shield was filled with thermally insulating powder. With this
setup, the authors were able to simultaneously determine the
thermal conductivity, electrical conductivity, and Seebeck coef-
ficient of Mg2Si1−xSnx solid solution in a temperature range of
300–870 K.[22]
Another absolute steady-state method relies on test stacks
constructed from metal bars. The related test apparatus
and test procedures have been specialized in ASTM D5470
standard.[23] Figure 2 shows two test configurations based on
this method. In the first configuration, the sample is pressed
between two metal bars (also known as meter bars) which are
made from highly thermally conductive materials with well-
documented thermal conductivity (Figure 2a). A linear array
of temperature sensors is placed in each metal bar. When the
steady-state heat flow is reached, the heat flow through the
sample can be measured by the metal bars. The interfacial
temperatures between the sample and the metal bar (Th and Tc)
are extrapolated from the linear temperature distributions on
both hot side and cold side.[24] In the second ­configuration,
a guard heater is installed around the main heater in order
to significantly reduce the heat leakage from the latter one[25]
(Figure 2b). In this case, qs can be deduced from the power
dissipated from the heater with necessary corrections for the
heat losses.[25] Th and Tc are obtained from the temperature
sensors that are installed in extreme proximity to the inter-
faces between the sample and the metal bars. In both con-
figurations, compressive load and thermal interface materials
such as thermal grease could be applied to minimize the
thermal contact resistances between the sample and the metal
bars.[23]
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The thermal resistance Rs of the sample is
given by
Th − Tc
Rs = (6)
qs
In principle, several samples with different
thickness d should be tested in order to elim-
inate the thermal contact resistance Rcontact
between the sample and the metal bars.[23,25]
The thermal conductivity of the sample can
be derived from the slope of Rs versus d
curve as
d
Rs = + Rcontact (7)
Aκ
In recent years, the methods based on the
ASTM D5470 standard have been used to
measure the thermal conductivity of several
thermoelectric carbon nanotube (CNT)/polymer nanocompos-
ites.[24,26–29] The thickness of the specimens ranged typically
from several tens of micrometers to hundreds of micrometers.
It has been found that the polymer composites with randomly
distributed CNTs demonstrate fairly low thermal conductivities.
For example, Yu et al. prepared a series of samples by mixing
single-wall carbon nanotube (SWCNT) with poly(3,4-ethylen
edioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) and/
or polyvinyl acetate polymers. The thermal conductivities for
the composites with 60 wt% CNT were found to be 0.2–0.4 W
m−1 K−1 at room temperature.[28] The values are close to those
reported for multiwalled carbon nanotube (MWCNT)/polyani-
line (PANI) composites, which lie between 0.4–0.5 W m−1 K−1
when the MWCNT content was varied from 20 to 80 wt%.[27]
In general, the absolute method is relatively easy to imple-
ment. By properly setting up the experimental apparatus, it is
possible to measure the thermal conductivity along with the
electrical conductivity and the seebeck coefficient for the bulk
samples.[22] On the other hand, the heat losses and the thermal
contact resistance are two major concerns when carrying out
the absolute method. For the measurement of the OHT mate-
rials, how to effectively reduce the thermal contact resistance
between the sample surface and testing components (e.g.,
meter bars, heater, heat sink, temperature sensors, etc.) is
especially critical, since the polymer or other organic mate-
rials usually possess relatively large thermal expansion coef-
ficient which may be as high as 1.2 × 10−4 K−1.[9] To elucidate
the problems caused by the samples with the large thermal
expansion coefficient, it can be assumed that the sample is
measured by the ASTM D5470 apparatus and the temperature
difference across the sample is large (e.g., >30 K). Under such
a scenario, the thermal expansion at the hot surface of the
sample may be significantly larger than that at the cold sur-
face. This could cause the sample to bow and to generate gaps
at the interfaces between the sample and the metal bars.[10]
The formation of the gaps leads to an increase of the thermal
contact resistance which may eventually deteriorate the quality
of the measurement . Therefore, to measure the OHT mate-
rials with relatively large thermal expansion c­oefficients, the
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temperature difference should be carefully kept at a level (e.g.,
several Kelvins[24]) that is small enough to avoid the formation
of the gaps but is still large enough for carrying out reliable
measurements.
2.2. Parallel Thermal Conductance Method
The parallel conductance method was developed by Tritt and
co-workers for measuring small bulk samples at the millimeter
scale which often bring about difficulties to the temperature
and heat flow measurements.[30] As shown in Figure 3a, the
sample holder consists of a heater (hot end) and a heat sink
(cold end), which are connected by a supporting post with low
thermal conductance. A differential thermocouple is used to
measure the temperature difference between the hot end and
the cold end. The measurement is carried out in two steps. In
the first step, a baseline thermal conductance Gbaseline is meas-
ured for the empty sample holder, which accounts for the heat
losses associated with the sample holder itself. To do this, mul-
tiple DC heating currents (I’s) are applied to the heater suc-
cessively to generate corresponding steady-state temperature
differences (ΔT’s) across the supporting post. The heating
power P varies linearly with ΔT as denoted by the following
equation
P = I 2Re,H = Gbaseline ∆T (8)
where Re,H is the resistance of the heater. Gbaseline is extracted
from the slope of the P ~ ΔT plot. The sample is then attached
to the sample holder, and the total thermal conductance Gtotal is
measured in a similar way
P = I 2Re,H = Gtotal ∆T (9)
Both Gbaseline and Gtotal are measured in a high vacuum envi-
ronment to reduce the convective heat losses.[31] The thermal
conductivity κ of the sample is determined from the following
equation
κ = (Gtotal − Gbaseline ) L/A (10)
Figure 3. Schematic diagram of the parallel thermal conductance method.
a) Empty sample holder. b) Sample holder attached with a sample.
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where L and A are the length and the cross-sectional area of the
sample, respectively.
The technique is capable of obtaining the thermal conduc-
tivity of the small bulk samples with a relatively simple experi-
mental setup. It does not require special sample treatments
and the sample mounting is simple and rapid. Recently, Wan
et al. have applied this method to obtain the in-plane thermal
conductivities of TiS2 single crystal and an inorganic/organic
superlattice material TiS2[(HA)0.08(H2O)0.22(DMSO)0.03]
at room temperature, which were found to be 4.45 and
0.69 W m−1 K−1, respectively.[31] The value of the TiS2 single
crystal is close in magnitude to the result previously reported
by Imai et al.[32] Varghese et al. have measured the in-plane
thermal conductivity of an ≈100 µm thick free-standing ther-
moelectric film made by screen printing colloidal inks com-
posed of Bi2Te2.8Se0.2 nanocrystals. The value (≈0.56 W m−1 K−1
at room temperature) is within 5% of the cross-plane thermal
conductivity determined by the laser flash method, which indi-
cates the isotropic nature of the sample.[33]
Two issues should be paid attention when implementing the
technique. First of all, to maintain a reasonably high measure-
ment sensitivity, the baseline thermal conductance associated
with the sample holder Gbaseline needs to be made as low as
possible.[30] Second, the thermal contact resistance between the
specimen and the sample holder should be kept much smaller
than the thermal resistance of the specimen itself to ensure the
accuracy of the measurement.
2.3. Comparative Method
The comparative method determines the thermal conductivity
of bulk materials without measuring the heat flow through
the sample qs. In this method, a reference sample with known
thermal conductivity is thermally connected in series with the
specimen to be investigated. The stack structure is sandwiched
between the heater and the heat sink. Two or more temperature
sensors are arranged along the test sample and the reference
sample, respectively (Figure 4). Under the steady-state condi-
tion, the heat flow through the sample should be equal to that
Figure 4. Schematic of the experimental setup for the comparative
method.
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through the reference sample. The thermal conductivity of the
sample is then given by
 A ∆T L 
κ s = κ ref  ref ref s 
 As ∆TsLref 
where subscripts “s” and “ref” denote the specimen to be tested
and the reference sample, respectively. The method achieves
the best accuracy if the thermal conductivity of the sample is
comparable with that of the reference sample.[34]
Test standards like ASTM E1225[35] and ASTM E1530[36]
describe the relevant apparatuses and test procedures for the
comparative method. When applying this method to the OHT
materials, the influence of the uneven thermal expansions
on the thermal contact resistance should be minimized[10] as
for the absolute method discussed in Section 2.1. Marconnet
et al. have characterized the thermal conductivity of aligned
CNT-thermoset epoxy composites using a setup conforming
to the ASTM E1225 standard.[37] In this study, the tempera-
ture sensing was carried out with an IR microscope instead
of thermocouples. The axial thermal conductivity of the com-
posites was found to increase from 0.46 to 4.87 W m−1 K−1 as
the volume fraction of CNT varied from 1 to 16.7 vol%, which
is comparable with that of unfilled and aligned CNT arrays
investigated in the same study. On the other hand, as men-
tioned in Section 2.1, Pisoni et al. have measured the tem-
perature-dependent thermal conductivity of the CH3NH3PbI3
sample[21] by adopting the experimental configuration shown in
Figure 4 and the obtained results were confirmed later by other
authors.[20]
Verebelyi has extended this method to measure the
thermal conductivity of Pb-doped Bi2Sr2Ca1Cu2Ox whisker
with d­ imensions less than 1000 × 100 × 100 µm3 within a
­temperature range of 30–200 K.[38] The measurement error
for such a small sample was estimated to be less than 25%
with the application of the temperature matching shielding
and micro-thermocouples. Later, Yoshino et al. have applied
this method to measure the thermal conductivity of mil-
limeter-sized organic crystals. By properly designing the
sample holder, they were able to simultaneously obtain the
values of the thermal conductivity, the Seebeck coefficient,
and the electrical conductivity from the same sample.[39–41]
The capability of measuring κ together with S and σ is
Figure 5. a) Schematic illustration of the measurement chip used in the Völklein method. b) Deposition of the thermoelectric film on top of the
­suspended membrane.
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considered to be a merit for this modification. However, sig-
nificant error in measuring κ has been found in their studies
presumably due to high residual gas pressure remained in
their measurement chamber.[40] This implies that the issues
(11)
such as heat losses and thermal contact resistance require
extremely careful handling when characterizing the small
samples.[38]
2.4. Völklein Method
Völklein et al. have developed a chip-based method to measure
the in-plane thermal conductivity of the sub-micrometer thick
thin film.[42–46] The chip (known as λ-chip) includes a rectan-
gular suspended dielectric (e.g., SiNx) membrane with a thick-
ness of 50 to 100 nm, on which the film specimen can be
deposited (Figure 5a). A thin metal stripe is created along the
long axis of the membrane which serves as both a heater and
thermometer. The silicon rim surrounding the membrane acts
as a heat sink. All measurements should be conducted in the
vacuum environment. The thermal conductivity of the bare
membrane needs to be determined first. To do this, a dc cur-
rent is applied to the metal stripe and the resulted heat will
flow through the membrane to the heat sink. At the same time,
radiation heat loss will occur from the surfaces of the mem-
brane and the metal stripe. From the temperature rise and
the input electrical power, an apparent thermal conductance
associated with the chip (G) can be calculated. With certain
approximations, it can be shown that the thermal conductance
of the membrane due to heat conduction and radiation (GM)
is roughly equal to G.[44] Since GM is a function of unknown
thermal conductivity κM,∥ and emissivity ε of the membrane,
it is necessary to carry out two measurements with two dif-
ferent membrane geometries so that one may obtain κM,∥ and ε
simultaneously.[44]
The thermoelectric thin film to be tested can be deposited
on the top side (top configuration)[46] or bottom side (bottom
configuration)[45] of the membrane through various vapor dep-
osition procedures such as thermal evaporation, magnetron
sputtering, atomic layer deposition, etc. If the film is depos-
ited on the top side of the membrane, the metal stripe should
be covered with a thin insulating layer in order to avoid elec-
trical shortcuts (Figure 5b). The top configuration allows one to
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prepare the OHT samples by different kinds of solution-based
methods such as spin-coating, dip-coating, drop casting, ink-jet
printing, etc.[47,48]
To obtain the in-plane thermal conductivity of the depos-
ited film (κf,∥), the thermal conductivity of the composite
layer (including the test film and the supporting mem-
brane) κC,∥ is measured by employing the same procedure
of obtaining κM,∥. κf,∥ is subsequently extracted from the fol-
lowing equation[44,45]
κ C, dC − κ M, dM
κ f , =
df
where df, dM, dC are the thicknesses of the thin film, the mem-
brane, and the composite layer, respectively. By applying this
method, Linceis et al. have recently measured κf,∥ for a 110 nm
thick Bi87Sb13 film over a temperature range of 120–450 K,[45]
which shows good agreement with previously published
results.[49]
The use of the ultrathin suspended membrane is a major
advantage of this method, since the parasitic heat transfer from
the sample into the substrate is eliminated,[43] which is critical to
achieving reliable measurements on the sub-micrometer thick
thermoelectric films.[44,45] Additionally, the insulation layer
and metal stripes are prefabricated on the test chip, which not
only significantly simplifies the sample preparations but also
prevents the samples from undergoing harsh environments
of depositing the insulation layer or performing lithography
process. This is very important for the characterization of the
vulnerable OHT materials.[13] Moreover, the current experi-
mental configuration has been integrated with measurement
techniques of the other TE properties on a single chip, there-
fore all quantities needed for calculating the in-plane ZT-value
can be obtained from the same sample in one measurement
run.[45]
On the other hand, it should be noted that the method is
incapable of measuring the cross-plane thermal conductivity of
the thin films. The measurement must be carried out in the
vacuum environment. The measurement accuracy depends on
the relative magnitudes of the thermal conductance associated
with the deposited film and the bare membrane. If possible, the
thermal conductance of the bare membrane should be made
smaller than that of the deposited film (κM,∥dM < κf,∥df).
Figure 6. a) Schematic illustration of the experimental configuration proposed by Shi et al.[50] b) Another configuration proposed by Sultan et al.[53]
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2.5. Microfabricated Suspended Device
Aiming for eliminating the parasitic heat transfer from the
sample into the substrate, another steady-state method based
on microfabricated suspended devices (MFSD) has been devel-
oped to measure the thermal conductivity of nanowires or
nanotubes along their axial direction or narrow thin film stripes
along their in-plane direction.[50–54] The temperature sensing of
this technique is performed at both ends of the sample and all
measurements are carried out in the vacuum environment to
reduce the convective heat loss. Two typical configurations will
(12) be reviewed in this paper.
One configuration proposed by Shi et al.[50] is schematically
shown in Figure 6a in which the test platform consists of two
adjacent suspended SiNx membranes each supported by five
identical long and thin SiNx beams. A platinum resistance ther-
mometer (PRT) is fabricated on each membrane to serve as the
heater or the thermometer. The sample is transferred onto the
device to bridge the two membranes. One membrane is used as
heating membrane on which the PRT is heated by a dc current,
while another one is used as sensing membrane. It is assumed
that the temperature rise on both membranes is uniform and
the heat losses due to gas flow, convection, and radiation can
be neglected. The Joule heat generated by the heater and the
two Pt current leads on the heating membrane are PH and 2PL,
respectively. A certain amount of the generated heat is trans-
ferred from the heating membrane directly to the environment
through the five beams. The rest heat flows into the sensing
membrane through the sample and is further conducted to
the environment through the five beams connected with the
sensing membrane. It can be shown that the measured thermal
conductance of the sample Gs is expressed as[50]
∆Tc (PH + PL )
Gs = (13)
∆Th2 − ∆Tc2
where ΔTh and ΔTc are the temperature rise at the heating
membrane and the sensing membrane, respectively. Both
ΔTh and ΔTc can be measured from the resistance change of
the PRT. On the other hand, the measured thermal resistance
(i.e., Gs−1) consists of the intrinsic thermal resistance of the sample
Rn, and the thermal contact resistance between the sample and
the two membranes, Rcontact
Gs−1 = R n + Rcontact (14)
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Only if Rcontact is small enough, the thermal conductivity of the
sample κ can be calculated directly from Gs−1 by
L L
κ = s ≈ −1s (15)
Rn As Gs As
where Ls and As are the length and cross-sectional area of the
sample, respectively. Therefore, how to reduce Rcontact is one of
major concerns when applying this technique. In practice, Rcontact
can be reduced by metal or amorphous carbon deposition at
the locations where the sample is contacted with the mem-
branes.[50] Alternatively, new techniques have been invented
later to explicitly obtain the thermal contact resistance and
the intrinsic thermal resistance of the sample by, for example,
making use of the thermoelectric voltage of the sample to deter-
mine the temperature drops at the contacts.[51,55]
Figure 6b illustrates another experimental configuration pro-
posed by Sultan et al. in which two identical suspended SiNx
membranes each equipped with the heater and thermometer
and supported by four legs are linked together by a narrow SiNx
bridge.[53,54,56] One membrane is used as the heating mem-
brane excited by a dc current, while another one as the sensing
membrane. It can be demonstrated that the steady-state tem-
perature rises on the two membranes are related to the heating
power P by[53]
GL + GB
∆Th = P (16)
(2GB + GL )GL
GB
∆Tc = P (17)
( 2GB + GL )GL
where GB and GL are the thermal conductances of the bridge
and the supporting legs, respectively. GB and GL can be solved
from the slopes of the ΔTh ∼ P and ΔTc ∼ P straight lines. Before
transferring the test sample onto the bridge, the thermal con-
ductance of the bare bridge GB,Si-N needs to be measured first.
Then the thermal conductance GB,C of the composite structure
consisting of the sample and the SiNx bridge is measured in the
same manner. The difference between GB,C and GB,Si-N is used
to compute the thermal conductivity of the sample. It should
be noticed that thermal contact resistance between the sample
and the two membranes should also be kept as low as possible.
Besides the thermal contact resistance, another impor-
tant issue associated with the MFSD method is the measure-
ment sensitivity of the device, which sets the lower limit of the
thermal conductance that can be measured for a sample.[8] This
value is around 1 nW K−1 for a typical device with the configu-
ration shown in Figure 6a.[50] The measurement sensitivity is
limited by several factors, including the heat transfer through
residual gas molecules, the radiation from the membranes,
and temperature fluctuation of the sample environment.[57]
Recently, significant progresses have been made to increase
the measurement sensitivity, it is now possible to measure the
sample with a low thermal conductance at the order of 10−10
or 10−11 W K−1.[57,58] For the configuration shown in Figure 6b,
the major factor that affects the measurement sensitivity is the
background thermal conductance of the bridge.
Both configurations have been used to measure the thermal
conductivity of polymer or OHT materials in recent years,
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including oxidized polyacetylene nanofibers (74–126 nm
in diameter),[59] amorphous polythiophene nanofibers
(71–245 nm in diameter),[60] PEDOT:PSS and PEDOT:Tosylate
(Tos) films (130–230 nm thick),[61] and polymer treated CNT
films or polymer:CNT hybrid films (≈90 nm thick in ref. [62]
and 80–110 nm thick in ref. [64]).[62–64] Among these studies,
Weathers et al. have systematically investigated the in-
plane thermal conductivities of a series of PEDOT:PSS and
PEDOT:Tos films, which demonstrated an obvious correlation
with the in-plane electrical conductivity σ∥. As σ∥ changed from
20 to 500 S cm−1, the thermal conductivity could vary from
about 0.5 W m−1 K−1 to as high as 1.8 W m−1 K−1 at 300 K.[61]
The value of 0.5 W m−1 K−1 is close to the in-plane thermal con-
ductivity (≈0.58 W m−1 K−1) for a low-σ∥ PEDOT:Tos film meas-
ured by Ushirokita and Tada using a chip-based 3ω method that
will be discussed in Section 4.3.[65]
It is also worth mentioning that the test platforms can be
designed to couple with the characterizations of the Seebeck
coefficient and the electrical conductivity of the same sample.[61]
On the other hand, the SiNx bridge in Figure 6b allows direct
depositions of the films on it by various physical vapor deposi-
tion (PVD) techniques[53,54] as well as solution-based ultrasonic
spray (UP) process.[62,63] The combination of the MFSD with
the UP process will facilitate the measurements of those solu-
tion- processable OHT films.[62,63]
The major drawbacks associated with the method are that
it requires extensive microfabrication works and the transfer
of as-prepared samples to the microdevices could be chal-
lenging. The thermal contact resistance and the measure-
ment sensitivity are also critical issues that needed to be
carefully considered. Since the measurement needs to be car-
ried out under the high vacuum condition, the technique is
not applicable to the humidity-controlled tests for the OHT
materials.[66]
2.6. Steady-State Infrared Thermography
The steady-state infrared thermography has been employed
to determine the in-pane thermal conductivity of the free-
standing PEDOT:PSS film[67] and PEDOT:PSS/Si nanoparticle
composite films.[68] As shown in Figure 7, the thin film sample
is suspended over a cavity in an opaque substrate with high
thermal conductivity. The sample is homogenously illuminated
from below by visible light with an absorbed power density QA
Figure 7. Schematic of steady-state infrared thermography.
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in a vacuum chamber. The wavelength of the light is carefully
selected to cause strong optical absorptance for generating sub-
stantial heating. The substrate serves both as a shadow mask
for the illumination and as a heat sink for the heat flow. The
temperature distribution is recorded by an infrared camera.
Theoretically, the temperature at a distance r from the cavity
center is given by[67]
QA QA
T (r ) = − r2 + r02 + T0
4κ f , df 4κ f , df
where r0 is the radius of the cavity. κf,∥ and df are the in-
plane thermal conductivity and the thickness of the film,
­respectively. T0 is the temperature of the heat sink. Since the
last two terms in Equation (18) are just constants, κf,∥ can
be deduced from the parabolic temperature distribution near
the center of the cavity, the absorbed power density, and the
film thickness.
The steady-state infrared thermography represents a non-
contact absolute method which can directly yield the in-plane
thermal conductivity of the sub-micrometer thick thin films.
However, extensive calibrations of the light source and the IR
camera are required for performing the measurements. In
order to apply the method to the OHT materials, it is neces-
sary for the samples to have a substantial absorptance at the
illuminating wavelength and a relatively large emissivity for
the IR detection.[67] In ref. [67], the 250 nm thick PEDOT:PSS
film (σ∥ = 720 S cm−1) post-treated by ethylene glycol (EG)
was found to have an in-plane thermal conductivity of
1.00 W m−1 K−1 at room temperature, which is comparable
with the literature data for highly electrically conductive sam-
ples such as dimethyl sulfoxide (DMSO)-mixed PEDOT:PSS
film (κf,∥ is estimated to be 1.05 W m−1 K−1 at σ∥ ≈ 520 S cm−1)
measured by the TDTR method[69] and EG-mixed PEDOT:PSS
sample (κf,∥ = 0.84 W m−1 K−1 at σ∥ = 820 S cm−1) character-
ized by the laser flash method.[70]
3. Time-Domain Methods
This section reviews three time-domain methods, including
two noncontact methods (i.e., the laser flash method and the
time-domain thermoreflectance method) and one contact
method (i.e., the hot-disk method). The laser flash method
and the hot disk method are commonly used to measure the
Table 2. Summary of the time-domain methods presented in this review for measuring the thermal transport properties of the OHT materials.
Methods Measured quantities
Laser flash method Cross-plane thermal diffusivity of bulk
materials mainly
Time-domain Thermal conductivity in the cross-plane
thermoreflectance direction mainly, possible in the in-plane
(TDTR) method direction
Hot-disk method Cross-plane thermal diffusivity and
thermal conductivity of bulk materials
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thermal diffusivity and the thermal conductivity of the bulk
samples, ­respectively. The time-domain thermoreflectance
method, on the other hand, is suitable for characterizing the
samples ranging from the bulks to sub-micrometer thick films.
Table 2 summarizes the major merits and limitations of these
three methods.
3.1. Laser Flash Method
(18)
The laser flash method was first introduced by Parker et al. in
1961 and has gained widespread acceptance since then.[71] It
is a noncontact technique for characterizing the thermal dif-
fusivity of the solid materials.[7,72,73] In this method, the front
surface of the sample is irritated uniformly by a short laser
pulse, the instantaneous temperature rise on the rear side
sample is recorded by a fast detector (e.g., infrared detector)
as a function of time. The use of the infrared thermographic
technique avoids the thermal contact resistance that will exist
between the sample and a conventional thermometer such as
the thermocouple.
A very thin layer of graphite or other high emissivity coating
is usually applied on both sides of the sample to enhance
the light absorption on the front surface of the sample and
infrared emission on the rear side of the sample.[74] If the
heat conduction from the front surface to the rear surface
is assumed to be 1D and heat losses from the sample are
neglected, the thermal diffusivity of a homogenous sample
can be expressed as[7]
 d2 
α = 1.37  2
(19)
 t1/2π 
where d is the thickness of the sample. t1/2 is the time needed
for the temperature on the rear surface (T(t)) to reach half of
its maximum temperature rise (Tmax ), which is schematically
illustrated in Figure 8.
The major advantage of the method is that it allows the
thermal conductivity being measured rapidly and reliably over a
wide temperature range (148–3073 K),[15] provided that the den-
sity and the specific heat of the sample have been obtained sep-
arately. On the other hand, the method requires surface coating
which prevents the sample from being used for other test pur-
poses. Also, it is not capable of measuring the sub-micrometer
thick thin films as the thickness for the sample that can be
Merits Limitations
Rapid and noncontact; Needs Cp and ρ;
wide temperature range Thickness limitation for the conventional laser flash
method; Surface coating needed
Rapid and noncontact; Complicated experimental setup; Sophisticated data
May obtain κ without knowing CV; Applicable reduction procedure;
to samples ranging from sub-micrometer Large uncertainty for κ∥ when κ∥ < 5 W m−1 K−1; Smooth
thick films to bulks sample surface needed; Needs surface coating
Nondestructive and rapid; Inapplicable to sub-micrometer thick films;
Can obtain α and κ simultaneously over a wide Questionable for the measurements of low density
temperature range materials
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Figure 8. Schematic of the laser flash method.
measured is limited by the pulse width of the heating laser and
the response speed of the detector. The commercial i­ nstruments
generally require the thickness of the sample to be larger than
100 µm.[74] Therefore, many OHT materials investigated by the
laser flash method are made in the form of bulk.[75–79] Ao et al.
have applied the method to measure the thermal conductivity
of Bi2Te3/polythiophene composites, which shows a weak tem-
perature dependence. For example, the thermal conductivity
of the composite with 30 wt% polythiophene was found to be
around 0.33 W m−1 K−1 in a temperature range of 300–473 K.[76]
A similar observation has been made for Sb2Te3/PEDOT com-
posite, which demonstrates a nearly constant value around 0.15
W m−1 K−1 between 300 and 523 K.[78] Yao et al. have shown that
the thermal conductivity of the SWCNT/PANI composite varies
from ≈0.34 to 0. 48 W m−1 K−1 as the SWCNT content increases
from 30 to 89 wt.%,[80] which is in reasonable agreement with
the results previously obtained by the absolute steady method
for the MWCNT/PANI composites.[27]
To extend the measurement capability of the conventional
laser flash method into the thin film region, a new technique
known as ultrafast laser flash method has been developed by
using the picosecond laser as the light source and the thermore-
flectance as the temperature sensing mechanism.[81] Unlike the
TDTR or FDTR methods which use the front heating/front
detection configuration (please refer to Sections 3.2 and 4.7),
the ultrafast laser flash method uses the rear heating/front
detection configuration which can be viewed as a natural exten-
sion of the conventional laser flash method.[81]
Figure 9. a) Schematic of the temporal evolution of the thermoreflectance signal. b) Sketch of the TDTR experimental setup based on an
­ultrafast-pulsed-laser system.
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3.2. Time-Domain Thermoreflectance Method
The TDTR method is an optical pump–probe technique for
measuring the thermal conductivity and interfacial thermal
conductance of thin films and bulk materials.[74,82–84] In this
method, a pump laser pulse at a fixed wavelength irradiates
the sample surface to generate a transient change in tem-
perature, which consequently causes a change in surface
reflectance that can be detected by a probe laser. The sample
surface is usually coated with a thin metallic film (i.e., trans-
ducer layer) whose reflectance changes with the temperature
rise at the wavelength of the probe laser. The temporal evo-
lution the thermoreflectance signal is schematically displayed
in Figure 9a. After ­initially heated by the short laser pulse,
a sudden jump in surface temperature is followed by a slow
cooling process from which the thermal properties of the
sample can by extracted by comparing with suitable theoret-
ical models.[74,85,86]
Depending on the pulse width of the pump laser and the
time scale for data acquisition, the TDTR methods can be
performed in the nanosecond domain for characterizing
the thermal properties of thin films,[87–91] in the picosecond
domain for measuring the thermal properties of thin films
and their ­interfacial properties,[82,92] and in the femtosecond
regime for investigating electron and phonon processes.[90,93,94]
If the thermoreflectance technique is applied in the nano-
second domain, a continuous wave (CW) laser can be used as
the probe laser.[87–91] On the other hand, when working in the
picosecond or femtosecond domain, an ultrafast pulsed laser
system should be used as the light source for fulfilling the
pumping and probing purposes.[74,84,95] Figure 9b schemati-
cally depicts such an experimental setup in which an ultrafast
pulsed laser light is split into the pump beam and the probe
beam by a polarizing beam splitter (PBS). By varying the time
delay between the probe pulse and the pump pulse using a
mechanical delay stage, the information of the temporal evolu-
tion of the surface temperature can be recorded. In order to
increase the signal to noise ratio, the train of the pump pulses
is modulated at frequency f mod by an electric-optic modulator
(EOM) so that the thermal response signals can be detected
by a lock-in amplifier.[96] The modulation frequency f mod typ-
ically ranges from 1 MHz to around 10 MHz, which makes
it possible to constrain the thermal penetration depth within
the sub-micrometer range.[84,86] Hence, the TDTR method
has become an attractive tool in characterizing the thermal
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conductivity of the sub-micrometer thick thin films, since the
influences from the substrate can be eliminated.[97] Depending
on the implementation strategies of the method, the extraction
of the thermal conductivity from the measurement data may or
may not require that the volumetric capacity CV of the sample
be predetermined.[98–102] In fact, it is possible to measure κ
and CV simultaneously by using a frequency-dependent TDTR
method.[101,102] Though the TDTR method was originally devel-
oped to measure the cross-plane thermal conductivity κ⊥, κ∥
may be measured by orientating the sample in such a way
that the incident laser beam is parallel to the in-plane direc-
tion of the sample.[69,103] Alternatively, the TDTR method can
be extended to characterize κ∥ by adopting variable spot size
configuration or beam-offset configuration.[14,96,104]
The TDTR method provides a rapid and noncontact way
to obtain the thermal conductivity for the materials ranging
from sub-micrometer thick films to bulks with a high lateral
spatial resolution.[103] It is not involved with the complicated
sample preparation process as required by the conventional
3ω method that will be discussed Section 4.1. The method
has attracted much attention in recent years as an important
technique for characterizing the thermal conductivity of var-
ious OHT materials including PEDOT:PSS films (100–400 nm
thick in ref. [99], 2.5 µm thick in ref. [100], and 80 nm thick
in ref. [105]),[69,99,100,105] poly(3-hexylthiophene-2,5-diyl) (P3HT)
thin films (77–200 nm thick),[98] graphene based organic nano-
composite (65 nm thick),[106] and tetracyanoquinodimethane
incorporated Cu3(BTC)2 (BTC = benzene tricarboxylate) metal–
organic framework films (200 nm thick).[101] With this method,
Liu et al. have observed that the cross-plane thermal conduc-
tivity κ⊥ of the drop-cast DMSO-mixed PEDOT:PSS films
does not change with the in-plane electrical conductivity σ∥ at
≈325 K.[69] The average value of κ⊥ is about 0.3 W m−1 K−1,
which is consistent with the data obtained by the conven-
tional 3ω technique.[107] In the same study, the authors were
able to obtain κ∥ for the PEDOT:PSS films by properly ori-
entating the sample embedded in an epoxy matrix with
respect to the direction of the laser beam.[69] The κ∥ value
demonstrates an increasing trend with σ∥, which has also
been observed by Weathers et al. via the MFSD technique
for the suspended PEDOT:Tos films prepared by vacuum
vapor phase polymerization and chemical polymerization.[61]
The κ∥ value estimated from the published data in ref. [69]
is ≈1.05 W m−1 K−1 for σ∥ ≈ 520 S cm−1, while κ∥ in ref. [61]
Figure 10. a) The bifilar spiral structure of a hot-disk sensor. b) Cross-sectional view of the diffusivity of the sample and tmax is the max-
experimental setup for the hot-disk method.
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could reach 1.8 W m−1 K−1 when σ∥ is around 400–500 S
cm−1. The difference might be attributed to the fact that the
PEDOT samples in both studies have been prepared in dif-
ferent manners.
The major limitations of the TDTR method include its
complicated experimental setup and sophisticated data-
reduction procedure as well as the surface coating. More-
over, to perform the TDTR measurement, the surface of
the sample needs to be smooth in order to minimize diffuse
reflections.[14] The requirement may bring challenge to the
sample preparations for certain OHT materials whose sur-
face roughness might be difficult to control. For example,
undulations or striations can naturally occur on the surface
of spin-coated or casted polymer films.[13] The OHT materials
can also possess strong anisotropy in thermal conductivity.
To properly extract the cross-plane thermal conductivity of
the anisotropic materials, it has been suggested that a large
spot size of the laser and high modulation frequency should
be used to eliminate radial heat transport.[96] The measure-
ment of the in-plane thermal conductivity based on variable
spot size configuration or beam-offset configuration[14,96,104]
seems even more challenging, since more complicated experi-
mental setup and data reduction models are involved. Jiang
et al. have suggested that it is difficult to measure the in-
plane thermal conductivity that is less than 5 W m−1 K−1 by
using the configurations mentioned above due to limits in
the lowest modulation frequency and the smallest spot size
of the laser used in the current TDTR setups.[14] Although
it is technically possible to further reduce the low limit of
the modulation frequency and the laser spot size in the
future,[14] the application of these configurations in meas-
uring the in-plane thermal conductivity of the OHT materials
may be limited at this moment, since many OHT materials
of interest have an in-plane thermal conductivity less than
5 W m−1 K−1.[47,61,63,64,67]
3.3. Hot Disk Method
The hot disk method, also known as transient plane source
(TPS) method,[108–111] uses a thin metal strip or a metal disk
(usually with a bifilar spiral pattern as shown in Figure 10a)
as a plane heat source which is sealed between two thin insu-
lating polymer films. To perform the measurement, the encap-
sulated hot disk is sandwiched between two
identical samples and a constant electrical
current is applied to the heater (Figure 10b).
The temperature rise is monitored by meas-
uring the resistance change of the heater
as a function of time. To ensure that the
sample can be treated as thermally infinite-
size solid, a criterion has been put forward
as a guideline for preparing the sample with
proper dimensions, which states that the
distance from the sensor edge to the nearest
free boundary of the sample should be
larger than 2 α tmax , where α is the thermal
imum transient recording time.[109,110,112]
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Theoretically, the temperature increase detected by the bifilar
spiral sensor is given by[109]
P
∆T (τ ) = D (τ ) (20)
π 3/2rsenκ
αt
τ= (21)
rsen
where P is the output power of the heater; rsen is the radius
of the sensor; t is the time and τ is a dimensionless quantity
known as characteristic time ratio; D(τ) is a complicated dimen-
sionless time-function that can be evaluated numerically.[112]
An advantage of the hot disk method is that both thermal
conductivity κ and the thermal diffusivity α can be obtained
from a single transient recording.[109,110] Hence, the volumetric
specific heat can be obtained at the same time according to
Equation (2). One way of extracting the thermal transport prop-
erties from the raw data is given as follows. α is varied as a trial
parameter to yield a series of ΔT(τ) versus D(τ) plots. The cor-
rect value of α corresponds to the plot that ΔT(τ) varies linearly
with D(τ). From the slope of the ΔT(τ) versus D(τ) curve (i.e.,
P/π3/2rsenκ), one may immediately obtain the thermal conduc-
tivity κ.[112] To improve the accuracy of the result, Equation (20)
can be further modified by including a number of factors such
as the heat capacity of the probe, the thermal resistance due
to the insulation layer of the sensor, resistance change of the
sensor with temperature, and so on.[109,112,113] An inconven-
ience associated with the usual hot disk method is that the
measurement requires two pieces of samples each with an
identical planar surface. Recently, a new technique known as
modified transient plane source method has been introduced
to address this issue. The new method is based on one-sided
sensor, which allows one to carry out the test with one single
piece of sample.[114–118]
The technique provides a nondestructive and rapid tool to
investigate the thermal conductivity and thermal diffusivity of
various materials over a wide temperature range.[119] Compared
with the steady state methods, the size of the sample could be
significantly small and the sample with irregular shape can be
accepted. During the test, the temperature rise caused by
the transient heating is typically less 5 K,[111] which represents
a small temperature perturbation imposed on the sample. This
will benefit the measurement of the OHT materials which may
suffer mechanical instability caused by the uneven thermal
expansion under a large temperature difference as discussed
in Section 2.1. In recent several years, the technique has been
extensively used for characterizing the thermal conductivity of
the OHT materials with a thickness ranging from several hun-
dred micrometers to 1–2 millimeters.[115–118,120–123] Unfortunately,
the method is not applicable to measuring the thermal conduc-
tivity of sub-micrometer thick films. With this technique, Wu
et al. measured the thermal conductivity of pellet samples (σ is
around 0.2–0.8 S cm−1) mechanically pressed from p-toluenesul-
fonic ­acid-doped PANI nanowires or nanorods.[117] The thermal
conductivity is about 0.3–0.4 W m−1 K−1 at 300 K, which is
in good agreement with that measured via the absolute
steady-state method for a PANI sample (κ ≈ 0.38 W m−1 K−1 at
σ = 0.45 S cm−1) prepared in a similar fashion.[27]
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It should be mentioned that Coquard et al. recently
s­uggested that the accuracy of the TPS method becomes
questionable when it is applied to low density materials
(such as polymer foams) due to the fact that their thermal
inertia is usually two orders of magnitude smaller than
that of the probe.[119] Therefore, if the method is applied to
aerogel-based or polymer foam-based OHT materials,[123,124] it
might be a good idea to crosscheck the results with another
method.[125,126]
4. Frequency-Domain Methods
In the frequency-domain methods, the periodic thermal per-
turbations are often created by the resistive Joule heating or
laser heating. The thermal responses captured by various
types of sensors (e.g., the resistive thermometer, thermo-
couple, IR sensor, photodiode, acoustic sensor, etc.) are usu-
ally fed into lock-in amplifiers to improve the signal-to-noise
ratio. In this section, we will review eleven frequency-domain
methods, including eight contact methods and three noncon-
tact methods. The contact methods include the traditional 3ω
method, the self-heating 3ω method, the 3ω method based
on the suspended ultrathin dielectric membranes, the scan-
ning thermal microscopy (SThM)-3ω method, the Ångström’s
method, the temperature wave analysis method, the light
irradiated ac-calorimetric method, and the photo-thermoelec-
tric method, while the frequency-domain thermoreflectance
method, the modulated photothermal radiometry, and the
photoacoustic method belong to the noncontact methods. The
merits and disadvantages of these methods are summarized in
Table 3.
4.1. Traditional 3ω Method
The traditional 3ω method developed by Cahill and Pohl in
1980s was initially used to measure the thermal conductivity
of bulk materials and thick films.[127,128] It was later extended
to measure the cross-plane thermal conductivity of the thin
films on substrate.[129,130] The technique utilizes a thin metal
stripe (with a width ranging from several micrometers to
tens of micrometers) deposited on top of the specimen to
serve as both a heater and thermometer. For electrically
conductive specimens, a thin insulation layer is needed to
separate the metal stripe from the sample (Figure 11). An
ac current at frequency ω in the form of I(t) = I0cos(ωt) is
injected into the heater/sensor to create the Joule heating at
frequency 2ω
I 02Re,H
P(t ) =
2
(1 + cos(2ω t)) (22)
where I0 is the amplitude of the ac current and Re,H is the
resistance of the metal stripe. A temperature oscillation at
­frequency 2ω (ΔT2ω) arises in response to the ac heating, which
in turn brings about a resistance fluctuation at the same fre-
quency. Multiplication of the 2ω resistance change by the ac
driving current gives rise to a small 3ω voltage component that
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Table 3. Summary of the frequency-domain methods presented in this review for measuring the thermal transport properties of the OHT materials.

Methods Measured quantities Merits Limitations

Traditional 3ω method Thermal conductivity of bulk materials;
Thermal conductivity of thin films in
the cross-plane direction mainly, also
possible in the in-plane direction
Self-heating 3ω method Thermal conductivity of the fibers or
nanowires along their axial direction,
or the thin film stripes along their
in-plane direction
3ω method based on In-plane thermal conductivity of films
the suspended ultrathin
dielectric membranes
Can obtain κ directly; Possible to be measured with S and σ
SThM-3ω method Thermal conductivity of bulks, thin films,
or nanostructures
Ångström’s method Thermal diffusivity of bulk materials
Temperature wave Cross-plane thermal diffusivity of bulk
analysis (TWA) method materials
Frequency-domain ther- Thermal conductivity in the
moreflectance cross-plane direction, possible in the
(FDTR) method in-plane direction
Light irradiated In-plane and cross-plane thermal
ac-calorimetric method ­diffusivity of thin plate samples
Modulated photothermal Cross-plane thermal diffusivity and
radiometry (PTR) thermal conductivity of bulk materials;
Possible to obtain in-plane thermal
diffusivity or thermal conductivity of
thin plate-like or filament-like sample.
Photoacoustic (PA) Cross-plane thermal diffusivity and
method thermal conductivity of bulk materials
and thin films
Photo-thermoelectric Cross-plane thermal diffusivity and
method thermal conductivity of bulk materials
Can obtain κ directly;
Applicable to sub-micrometer thick thin films;
Insensitive to the radiation and convective heat losses
Can obtain κ directly; Possible to be measured with
S and σ
Substrate effect eliminated;
Prefabricated metal stripes and insulation layers;
Compatible with various film deposition techniques;
Can obtain κ;
Minimum sample preparations;
High spatial resolution;
Applicable in ambient condition
Easy implementation;
Simple sample preparations
Easy implementation;
Simple sample preparations
Rapid and noncontact;
Applicable to both sub-micrometer thick thin films
and bulk materials; Easier instrumentation than TDTR
Easy implementation;
Possible to measure the in-plane and cross-plane
thermal diffusivity from the same sample
Noncontact method;
Can obtain κ
Noncontact method;
Can obtain κ; Inexpensive detection system;
Toleration for surface roughness
Easy implementation
Can obatain κ; Applicable to thermoelectric liquid
Microfabrication of the metal stripe;
Needs good insulation layer for the
electrically conductive samples
Needs electrically conductive sample
with a substantial TCR; The resistance
should at least locally vary linearly with
temperature. The sample needs to be
stable in the vacuum
The thermal conductance of the bare
membrane needs to be small when
compared to that of the sample
Sophisticated models and extensive
calibrations needed
Needs Cp and ρ
Needs Cp and ρ;
Samples should be thermally thick;
Needs good thermal contact between
sample and heater/sensor
Sophisticated data reduction
procedure; May need CV to extract
κ⊥; Large uncertainty for κ∥ when
κ∥ < 5 W m−1 K−1; Smooth sample
surface needed; Needs surface coating
Needs Cp and ρ;
Contact method
Complicated normalization
procedures are necessary;
Needs surface coating
Needs surface coating;
Extensive calibration and
normalization procedures
The sample may need a substantial
Seebeck coefficient

can be detected by the lock-in amplifier. The 3ω voltage signal tance that heat diffuses within the sample during one cycle of
V3ω is given by[131] the ac power heating period[127]) is much larger than the half-
width of the metal stripe b, the metal strip can be treated as a
1
V3ω = I 0 Re,H ∆T2ω β H (23) line source. The complex temperature rise of the metal stripe
2 can be approximated by[127,129,131]
 1 dR 
where βH  βH = e,H
is the temperature coefficient of Pl  1 1  αs  π
 Re,H dT  ∆Ts =  − ln(2ω ) + ln  2  + η − i  (24)
resistance (TCR) of the metal stripe. The thermophysical prop- πκ s 2 2 b 4
erties such as the thermal conductivity of the sample can be
retrieved by fitting proper theoretical transport models to the where κs is the thermal conductivity of the solid and b is the
ΔT2ω data.[127,132] half-width of the metal stripe. Pl is the amplitude of the ac
For a semi-infinite isotropic solid with a thermal diffusivity heating power per unit length dissipated by the metal stripe.
αs, if its thermal penetration depth LP = α s /2ω (i.e., the dis- η is a constant. Equation (24) demonstrates that the thermal

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Figure 11. Schematic of the experimental configuration for the traditional
3ω method.
­conductivity of the isotropic substrate κs can be obtained from
the slope of the in-phase component of ΔTs as a function of log-
arithm frequency.
To measure the cross-plane thermal conductivity of an insu-
lating layer on the substrate as shown in Figure 11, the width of
the stripe is made to be much larger than the thickness of the
films so that one may assume that the heat flow through the
film is 1D. Since the film thickness is much smaller than
the thermal penetration depth of the substrate, the measured
thermal response by the stripe (ΔTsub+f) is just the temperature
rise of the substrate (ΔTsub) added by a frequency independent
temperature rise across the film (ΔTf)[129]
∆Tsub+f = ∆Tsub + ∆Tf (25)
One may directly calculate ΔTsub from Equation (24), provided
that the thermophysical properties of the substrate have been
determined separately. When ΔTf is known, the cross-plane
thermal conductivity of the film κf,⊥ is calculated by[129]
Pl df
κ f ,⊥ = (26)
2b∆Tf
where df is the thickness of the thin film. It should be empha-
sized that the thermal contact resistances between the film and
the substrate as well as between the metal stripe and the film
have been assumed to be negligible here.
The thermal conductivity measurement of the TE films often
involves multiple-layer structures. For example, for the TE film
deposited on a SiO2/Si wafer and capped with a SiNx insulation
layer, there are totally four layers with different thermophysical
properties. Theoretically, the temperature rises associated with
the Si wafer and the SiO2 and SiNx layers can be measured sep-
arately. But this will often bring about “stacking errors” to the
final result.[131] One reliable way to subtract the contributions
of the substrate and the dielectric layers is known as the “differ-
ential method,” in which metal stripes with same dimensions
are patterned onto the specimen and a “blank sample” without
the film of interest.[132] The temperature rises are measured
as a function of the heating frequency with same input power
for both samples. ΔTf is then taken from the temperature-rise
­difference between the two samples.
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The 3ω method has been extended by Ju et al. to measure
the in-plane thermal conductivity κf,∥ of films by utilizing a very
narrow metal stripe (around several micrometer wide) which is
sensitive to the heat transfer in both in-plane and cross-plane
directions.[133] It can be shown that ΔTf under such a circum-
stance can be written as[74,132]
Pl  1 
1/2
∞ sin 2 λ   df   κ f , 
1/2

∆Tf =
π  κ f ,⊥κ f ,  ∫ λ3
tanh  λ 
 b  
 κ f ,⊥ 
 dλ (27)
 
0
where κf,⊥ is measured separately by using a much wider metal
stripe. In principle, κf,∥ can be readily obtained by fitting the
2D model to the ΔTf data. However, it has been reported by See
et al. in their studies on polymer-nanocrystal hybrid thermoelec-
trics that errors associated with the measurements of the TCR
and the width of the heater line as well as the film thickness
propagate highly nonlinearly to cause an uncertainty around
70% for the fitted κf,∥. Therefore, conclusive results for κf,∥ were
not reached in their studies.[134] In fact, for the thermal conduc-
tivity measurement on the anisotropic ­materials (including the
anisotropic OHT materials), it is desirable to measure κ⊥ and
κ∥ independently as in the 2D model the propagation of the
uncertainty in κ⊥ (κ∥) can lead to growth of the uncertainty in
κ∥(κ⊥) as well.[135] Hence, further comparison of the 3ω method
with alternative techniques may be necessary regarding the
measurement of the in-plane thermal conductivity of the aniso-
tropic materials.[61]
Up to date the method has been extensively used to
measure the thermal conductivity of a variety of OHT mate-
rials, including the conductive polymer films,[65,66,107,136,137]
the small molecule organic semiconductors,[138–140] the
organic/inorganic composites,[134,141,142] etc. The thickness
of the OHT samples prepared for the cross-plane thermal
conductivity measurements range typically from 100–200
nm[107,138] to several micrometers.[136,138,142] Among these
studies, Bubnova et al. reported a room temperature κ⊥ value
of 0.33 W m−1 K−1 for the PEDOT:Tos film,[137] which was con-
sistent with the results measured on similar samples via the
conventional 3ω[66,107] or TDTR[69,105] techniques. Rausch et al.
reported a room temperature κ⊥ value of 0.19 W m−1 K−1 for
the sub-micrometer thick P3HT film,[143] which is also in good
agreement with the TDTR[98] and other conventional 3ω[65]
measurements.
A major advantage of the 3ω method is that it is insensi-
tive to the radiation and convective heat losses, since the
thermal ­penetration depth associated with the ac heating is
usually small and the heat losses during the measurement
occur mainly from a small area surrounding the heating
stripe.[127,144] Therefore, the method can be applied in both
vacuum and ambient. Kim et al. have found that the ther-
moelectric properties of PEDOT doped by different amounts
of hydrophilic PSS can be tuned by varying humidity con-
ditions.[66] In their studies, the traditional 3ω method was
employed to perform the thermal conductivity measurements
in a humidity-controlled environment.
Although the method is relatively easy to implement, the
necessity of microfabricating the metal stripe makes the meas-
urement somehow time-consuming. In some cases, it is also
challenging to fabricate the thin insulation layer with good
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quality for isolating the electrically conducting materials to be
measured from the metal stripe.[131,145] To apply the traditional
3ω method on the OHT materials, more precautions should
be taken for the sample preparations due to the fact that some
OHT materials are vulnerable to the relatively high processing
temperature (e.g., 573 K in a typical plasma enhanced chemical
vapor deposition (PECVD) process for depositing the insula-
tion layer[13]), and the harsh chemicals used in the lithography
procedure. In order to address the issues mentioned above,
Kaul et al. have developed a sample preparation methodology
which included a low temperature PECVD procedure for fab-
ricating the insulation layer and utilization of shadow masks
for creating the metal stripe.[13] The recipe has been success-
fully applied to the measurements of 110 nm and 5 µm thick
­polyaniline films.
4.2. Self-Heating 3ω Method
In the self-heating 3ω method,[146,147] the sample itself acts as
a heater and temperature sensor, therefore it is required to be
electrically conductive with a substantial TCR βs. As shown in
Figure 12, the measurement is performed with a four-probe
configuration. Two outer electrical contacts are used to feed
the electrical current, while the electrical voltages are extracted
from two inner electrical contacts. The central portion of the
sample between the two voltage contacts is suspended to avoid
the parasitic heat flow entering into the substrate. The test
platform is placed in a vacuum chamber to avoid convective
heat losses. When a sinusoidal electric current at frequency ω
is passed through the sample, the resistance fluctuation at fre-
quency 2ω is generated in response to the temperature fluctua-
tion at the same frequency. Consequently a small 3ω voltage
signal will be produced which is encoded with information
of the thermophysical properties of the sample. Lu et al. have
shown that the amplitude of 3ω voltage signal can be written
as[146]
3
4I RMS 2
LRe,s βs
V3ω ,RMS = (28)
π κ s As 1 + (2ωγ t )2
4
where V3ω,RMS and IRMS are the root-mean-square (RMS) ampli-
tude of the 3ω voltage and the exciting current, respectively. L
is the length of the sample between the two inner contacts. κs,
Re,s, and As are the thermal conductivity, the resistance, and the
cross-sectional area of the sample, respectively. γt = L2/π2αs is
a characteristic thermal time constant associated with the heat
transfer along the axial direction, where αs is the thermal dif-
fusivity of the sample. Based on Equation (28), it is possible to
Figure 12. Schematic of the experimental setup for the self-heating 3ω
method.
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simultaneously obtain the thermal conductivity and the thermal
diffusivity (or volumetric capacity) of the sample by performing
proper data fittings.
On the other hand, when the measurement is carried out at
the low frequency limit ωγt → 0, V3ω,RMS is almost independent
on frequency
3
4I RMS 2
LRe,s βs
V3ω ,RMS = (29)
π κ s As
4
In this scenario, the thermal conductivity can be simply found
by solving Equation (29).
The self-heating 3ω method provides a simple way to
measure the thermal conductivity of the electrically conductive
materials, including carbon nanotube,[148] inorganic semicon-
ductor nanowires or nanoribbons,[149–151] metal nanowires,[152]
and semiconductor nanocrystal coated glass fibers.[153] In
recent years, the method has been applied to characterize
highly ­conductive organic/inorganic nanocomposites[154] and
OHT materials such as poly(nickel-ethylenetetrathiolate)[155]
and polythiophene[156] films, which were usually several
micrometers to several tens of micrometers thick. In ref. [156],
Zhang et al. reported a room temperature thermal conductivity
of 0.22 W m−1 K−1 for a polythiophene sample prepared by
­electrochemical polymerization with a low electrical conduc-
tivity (σ = 44 S cm−1). The result is very close to the bulk value
of 0.19 W m−1 K−1 measured by the photoacoustic method for
another electrodeposited polythiophene sample.[60] Huewe
et al. have integrated the self-heating 3ω technique into a mul-
tipurpose sample holder capable of characterizing all three
thermoelectric quantities (S, σ, and κ) on the same sample of
crystalline organic semiconductors.[157] Their studies yielded a
thermal conductivity of 1.73 W m−1 K−1 at room temperature
for a DCNQI2Cu (DCNQI = dimethyl-dicyanoquinonediimine)
organic crystal along its axial direction, which agrees in mag-
nitude with literature data for similar quasi-1D organic single
crystals.[158]
Since the sample itself is used as the thermometer, its resist-
ance should vary linearly with temperature, at least within
small temperature range around the measurement tempera-
ture. Its electrical and thermal properties need to be stable
under vacuum condition, especially when the sample is made
from the OHT materials. For the OHT materials with humidity-
dependent electrical and thermal properties,[66] the calibration
of the TCR should be carried out in vacuum environment along
with the 3ω measurement in order to maintain consistency of
the data.
4.3. 3ω Method Based on the Suspended Ultrathin Dielectric
Membranes
The 3ω method can also be coupled with the suspended
ultrathin dielectric membranes to measure the in-plane thermal
conductivity of the films.[44,47,48,65,159,160] One way to achieve this
is to use the λ-chip in the Völklein method (Figure 5a) as the
measurement platform.[44,47,48,159,160] By injecting an ac cur-
rent I(ω) = I0cos(ωt) into the central metal stripe, the gener-
ated thermal wave will flow from the heat source toward the
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heat sink (i.e., silicon chip) through the suspended membrane The in-plane thermal conductivity is measured for both
(bare dielectric membrane or composite layer composed of the the bare dielectric membrane and the composite structure
dielectric membrane and deposited film). By measuring the 3ω deposited with the film of interest. The thermal conductivity
voltage V3ω across the metal stripe, the 2ω temperature oscil- of the deposited film can be subsequently deduced from
lation ΔT2ω at the location where the stripe is located can be Equation (12).
given by[44] Linseis et al. have applied this method to measure the
temperature-dependent in-plane thermal conductivity of
2V3ω the PEDOT:PSS films with a thickness ranging from sub-
∆T2ω = (30)
I 0 Re,H β H micrometers (100–383 nm)[47] to 15 µm.[48] In ref. [47], the
error bar range associated with the measurement increases
where βH and Re,H are the TCR and electrical resistance of the with decreasing the film thickness and the results for the
metal stripe, respectively. 100 nm thick film demonstrate a high degree of uncertainty.
In order to establish the relationship between V3ω and the The thermal conductivities of the 276 and 383 nm thick
thermophysical properties of the membrane, a 1D transient samples (σ∥ < 20 S cm−1) vary approximately from 0.39 to
heat transfer equation has been solved by imposing proper 0.54 W m−1 K−1 at room temperature, which are comparable
boundary conditions.[159] The amplitude of V3ω in the low fre- with those of the low-σ∥ samples measured by the MFSD[61]
quency limit can be written as[48] and TDTR[69] techniques. On the other hand, the in-plane
thermal conductivity of the 15 µm thick film (σ∥ ≈ 200 S cm−1)
β HRe,H
2
I 03 prepared by drop casting was determined to be ≈0.35 W m−1
V3ω = (31)
4K P K−1 at room temperature,[48] which is smaller than that of the
sub-micrometer thick samples with low σ∥.[47] However, the
2κ  dLM value is very close to the κ⊥ value of the PEDOT:PSS films
KP = (32)
w which has been found to be independent on σ∥.[69] The low κ∥
value of the thick film probably reflects the isotropic nature of
where w and LM are the width and length of the mem- the sample.
brane as defined in Figure 5a. κ∥ and d are the in-plane Ushirokita and Tada have taken another approach to com-
thermal conductivity and the thickness of the membrane, bine the 3ω technique with the suspended ultrathin mem-
respectively. brane.[65] Their test platform is based on a double stripe
It has been found that the values of κ∥ calculated from ­configuration[161–163] as shown in Figure 13. Two metal stripes
­Equations (31) and (32) are subject to errors caused by the (denoted as S1 and S2, respectively) are fabricated on top of a
radiation heat loss from the membrane surfaces.[48] Therefore, SiNx membrane window. A 50 nm thick SiO2 layer is depos-
a correction procedure based on two membranes with different ited on top of the stripes as an insulating layer for subsequent
dimensions has been proposed as follows, from which the deposition of the conducting sample. An ac current in the form
thermal conductivity κ∥ and emissivity ε of the membrane are of I(ω) = I0sin(ωt) is passed through the strip S1 to induce the
obtained together.[48] 2ω temperature oscillation. The heating frequency is selected
It can be shown that the thermal conductance associated to be high enough to make the thermal penetration length
with the two membranes due to heat conduction and heat radi- Lp inside the membrane much smaller than the width of the
ation is written as[44,48] membrane window. Under the 1D heat transfer approximation,
the amplitude of the temperature oscillation at S1 (|ΔTS1|) and
PAC,i  wi 
GM,i = = 2κ  dLM,i µ coth  µ  (33)
∆T2ω ,i  2

8εγ T03
µ2 = (34)
κ d
where PAC,i and |ΔT2ω,i| are the amplitude of the ac heating
power and amplitude of the temperature rise associated with
the ith (i = 1,2) membrane, respectively. γ is the Stefan–Boltz-
mann constant and T0 is the temperature of the heat sink. The
ratio of the thermal conductance of the two membranes is con-
sequently given by[48]

LM,1 coth  µ 1 
w
GM,1  2
= (35)
LM,2 coth  µ 2 
GM,2 w
 2

By numerically solving Equation (35), the parameter μ can be

obtained readily. It is then straightforward to calculate κ∥ and ε Figure 13. The platform for measuring the thermal conductivity of a thin
from Equations (33) and (34). film using double metal stripes.

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the phase shift of the temperature oscillation at S2 (ΔϕS2) are
given by[65,161]
∆TS1 α 1 the bare membrane.[65] In contrary to the conventional 3ω tech-
= (36)
Pl 2 2dκ  ω
and
ω
∆ϕS2 = − L + ϕ0 (37)
α
respectively. Here, Pl is the amplitude of the ac heating power
per length. κ∥ and α∥ are the in-plane thermal conductivity and
thermal diffusivity of the suspended membrane, respectively.
d is the thickness of the membrane. L is the interval between
the two stripes and ϕ0 is a constant. |ΔTS1| is derived from the
­measurement of the 3ω voltage. To obtain ΔϕS2, a dc “probe”
current is passed through S2 to detect its resistance vari-
ation. Since the temperature rise of S2 has a 2ω component,
the resistance of S2 gains a small ac component of the same
frequency. The product of the ac resistance with the “probe”
current gives rise to a small voltage component oscillated at
2ω.[162,164] The phase shift of this small voltage signal is ΔϕS2
which can be measured by the lock-in amplifier. In the experi-
ment, both ΔϕS2 and |ΔTS1| are recorded as a function of ω. α∥
can be obtained by linearly fitting ΔϕS2 as a function of ω .
With known α∥, κ∥ is derived from the slope of the |ΔTS1| versus
ω−1/2 curve. Based on this configuration and Equation (12), the
thermal conductivity of poly(methyl methacrylate) (PMMA) and
several thin conjugated polymer films (200 nm–1 µm thick)
have been characterized at room temperature by Ushirokita and
Tada.[65] The room temperature value of the PMMA film was
found to be 0.17 W m−1 K−1, which is in good agreement with
the literature result.[88] They also reported a correlation between
κ∥ and the in-plane electrical conductivity σ∥ for the PEDOT:Tos
films, which confirms the previous observations made on the
PEDOT:PSS and PEDOT:Tos samples by applying the MFSD[61]
and TDTR[69] techniques. All these studies actually yield close
κ∥ values (around 0.5–0.7 W m−1 K−1) for the low-σ∥ samples
(σ∥ < 50 S cm−1).[61,65,69] The κ∥ value for the sample with
σ∥ = 240 S cm−1 was found to be 0.86 W m−1 K−1 in ref. [65],
which is coincident with the result (≈0.82 W m−1 K−1 at
σ∥ ≈ 250 S cm−1) obtained via the TDTR technique[69] and is
about 28% smaller than the value interpolated from the MFSD
data (≈1.2 W m−1 K−1).[61]
To summarize, the 3ω method based on the suspended
ultrathin membrane can be used to measure the in-plane
thermal conductivity of the films with various thicknesses of
sub-micrometers to more than ten micrometers by eliminating
the substrate effect. The chip-based measurement platform
has been designed to measure the Seebeck coefficient and
the electrical conductivity of the sample at the same time.[47]
Unlike the conventional 3ω method, this method utilizes the
prefabricated insulation layers and metal stripes, which is an
advantage for characterizing the OHT materials that may not
be able to sustain hostile processing conditions. The test-chip
is designed to allow facile sample deposition by PVD methods
(e.g., thermal evaporation and magnetron sputtering) and
solution-based techniques (e.g., spin coating, drop casting, or
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ink-jet printing).[48] On the other hand, to ensure a sufficient
measurement sensitivity, the thermal conductance of the test
film should be as large as possible when compared to that of
nique, this method should be conducted under the vacuum
environment, which precludes its use in exploring the thermal
conductivity of the OHT materials in ambient or humidity-con-
trolled conditions.[66]
4.4. SThM-3ω Method
SThM brings a microprobe which acts as thermometer and
heater to be in contact with or in close proximity to the sample
surface.[165–167] By delivering heat locally to the sample and
measuring corresponding thermal responses, it is possible to
probe the thermal conductivity of the sample with high lateral
resolution. More specifically, the probe could be a thermo-
couple junction[168,169] or a resistive metallic probe.[170–174] In
the latter case, the temperature variation is detected by meas-
uring the resistance change of the probe. If an ac current with
angular frequency ω is used to heat the resistive metallic probe,
the resulted 2ω temperature oscillation of the probe should be
proportional to its voltage rise in the third harmonic (i.e.,V3ω)
that can be detected by a lock-in amplifier. An experimental
setup adopted by Lefèvre and Volz for performing the SThM-3ω
measurement is schematically shown in Figure 14.[172]
In order to link the observable quantity V3ω with the thermal
conductivity, a number of analytical and numerical models
have been proposed, which take into accounts of various factors
such as the geometrical/dimensional parameters and mate-
rials properties of the probe, the effective thermal resistance
between the sample and the probe, the effective coefficient of
heat losses by the whole probe surface to its environment, and
so on.[171,172,175–178]
The technique allows relatively fast characterization of a
wide variety of sample types (including bulks, films, or nano-
structures)[166,172,176,178–181] and requires only minimal sample
preparations. It provides a high lateral spatial resolution[166]
that is not attainable by other techniques. For the bulk or ther-
mally thick films, the thermal conductivity can be derived by
treating the sample as a semi-infinite medium. If the film on
a ­substrate is thermally thin and heat spreading in the in-plane
directions is non-negligible, a 2D heat transfer model for a
multilayered system should be employed to obtain the thermal
Figure 14. Schematic of the experimental setup for the SThM-3ω
­measurement adopted by Lefèvre and Volz.[172]
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www.advancedsciencenews.com
c­ onductivity.[176] In recent years, the method has been used to
measure the thermal conductivity of several inorganic nano-
structures such as the nanowires of Si,[178,179] SiGe,[179] and
Bi2Te3,[180] and some OHT materials including P3HT nanow-
ires (100 µm long and 120–350 nm in diameter),[181,182] doped
and undoped poly[N-9′-heptadecanyl-2,7-carbazole-alt-5,5-(4′,7′-
di-2-thienyl-2′,1′,3′-benzothiadizole)] (PCDTBT) films (several
micrometers thick),[176,183] and so on. In order to evaluate the
reliability of the SThM-3ω technique, Wilson et al. carried out
characterizations on calibrated samples, including PANI com-
posites mixed with 5% and 7% graphene nanoplatelets,[176]
which have been investigated previously by the comparative
method.[184] The measured thermal conductivities were found
to be 0.47 and 0.68 W m−1 K−1, respectively, which are in good
agreement with the calibrated data. Since the SThM measure-
ments are usually performed in air condition, the method is
in principle applicable to the investigations of the humidity
dependent thermal conductivity[66] of the OHT ­materials. On
the other hand, in order to extract the value of the thermal con-
ductivity, the sophisticated models and extensive calibrations
are generally needed. The accuracy of the results relies on how
those effective parameters associated with the theoretical model
have been obtained.[171,172,175–178,185]
4.5. Ångström’s Method
The Ångström’s method is a widely accepted method for deter-
mining the thermal diffusivity of the solid materials.[7,186,187] In
this method, the sample is heated periodically at one end, while
the temperatures are measured at two locations along its length
(Figure 15). When the propagation of the thermal wave reaches
a steady state, temperature variations are recorded to calculate
the thermal diffusivity by[188]
π f mod L2
α= (38)
∆ϕ ln ( ∆Th / ∆Tc ) 2α
where f mod is the heating frequency. L is the distance between
xh and xc where two temperature sensors are located. |ΔTh| and
|ΔTc| are the measured amplitudes of the temperature wave at
xh and xc, respectively, while Δϕ is the phase lag between the
two locations.
The Ångström’s method is a traditional method for obtaining
the thermal diffusivity of the rod-like or stripe-like sample.
The implementation of the method is relatively easy and the
sample preparations are simple. It has been used to measure
the thermal diffusivity of the thermoelectric materials since
1960s.[188–190] Though many choices are available today for
Figure 15. The experimental configuration for Ångström’s method.
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characterizing the thermal transport properties of the bulk
thermoelectric materials, the Ångström’s method still remains
useful due to its simplicity and versatility. Recently, Shin
et al. have used this method to characterize the Bi0.5Sb1.5Te3
and Bi2Te2.7Se0.3 based samples prepared by a combination of
screen-printing and hot pressing procedures.[191] Tan et al. have
used this method to measure the thermal diffusivity of a kind
of carbon nanoparticle hybrid aerogel with extremely low den-
sity and high porosity.[124] The derived thermal conductivity for
the aerogel sample was about 0.02–0.03 W m−1 K−1, which is
comparable with that of a 3D CNT network measured via the
laser flash and hot disk methods at low air pressure (20 Pa).[126]
The main limitation of the Ångström’s method is that it does
not directly yield the value of κ, although certain attempt has
been made to modify the method in order to achieve a simulta-
neous measurement of α and κ.[186]
4.6. Temperature Wave Analysis Method
The temperature wave analysis (TWA) method is a contact
method for measuring the cross-plane thermal diffusivity of the
sample.
In this method, the sample of thickness d is sandwiched
between one heater and one resistive temperature sensor[192–194]
(Figure 16). The heater creates a thermal wave at the front sur-
face of the sample by the ac Joule heating at frequency f mod
( f mod = ω mod /2π ) , which diffuses toward the rear surface
along the thickness direction. The temperature oscillation at
the rear surface is measured by detecting the resistance varia-
tion of the sensor with the lock-in technique. If the sample is
thermally thick ( i.e., d π f mod /α  1), the phase lag of the tem-
perature variation between the front surface and the rear sur-
face, Δϕ, is approximated by[193,194]
ω mod π
∆ϕ = − d− (39)
4
The thermal diffusivity α is determined from the slope of Δϕ
versus ω mod plot.
The TWA method only needs simple instrumentation and
minimum sample handlings. The major limitation of the
Figure 16. The experimental setup for the temperature wave analysis
method.
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www.advancedsciencenews.com
Figure 17. Schematic of the FDTR system based on CW lasers proposed by Schmidt et al.[199] the TDTR system similar to the one shown
method is that one has to know the specific heat and density
of the sample in order to calculate the thermal conductivity.
To ensure measurement reliability, the sample should be ther-
mally thick and good thermal contacts should be achieved at
the sample/heater and the sample/sensor interfaces. The tech-
nique has been previously applied to measure the temperature
dependent cross-plane thermal diffusivity of nonconductive
polymer films, including aromatic polyolefins[193] and poly-
imide.[194] Morikawa and Hashimoto have measured the tem-
perature-dependent thermal diffusivity for 25 and 125 µm thick
polyimide (Kapton) films,[194] which demonstrated a good coin-
cidence with the laser flash results.[195]
Later, its application scope has been extended to OHT mate-
rials. With this technique, Hiroshige et al. investigated the
thermal diffusivity of pristine and iodine-doped copolymers of
phenylenevinylene with dialkoxyphenylenevinylene.[196] Zhang
et al. have measured the thermal diffusivity of PEDOT:S-PHE
(sulfated poly(β-hydroxyethers)) films prepared by electro-
chemical polymerization.[197] The room temperature thermal
diffusivity of these thermoelectric polymers was found to be
around 1–3 × 10−7 m2 s−1, which is of the same order as that
of the insulating Kapton films (≈1.2 × 10−7 m2 s−1).[194] By pre-
paring 0.74–0.84 mm thick SWCNT–polystyrene composites,
Suemori and Kamata were able to measure the thermal diffu-
sivity along both cross-plane and in-plane directions by proper
orientating the sample slices.[198] The derived thermal conduc-
tivities along the in-plane direction for the composites with 25
and 50 wt% SWCNTs are around 4 W m−1 K−1, which are about
5 times and 10 times larger than those along the cross-plane
direction due to the preferable orientation of SWCNTs in the
in-plane direction. The in-plane thermal conductivity is actually
comparable with the axial thermal conductivity of the aligned
CNT-thermoset epoxy composite with 16.7 vol% CNTs meas-
ured by Marconnet et al. using the comparative method
(4.87 W m−1 K−1).[37]
4.7. Frequency-Domain Thermoreflectance Method
The FDTR technique is a rapid and noncontact method for
measuring the thermal conductivity of both sub-micrometer
thick films and bulk materials. Like the TDTR method, the
FDTR method also uses the modulated pump laser to periodi-
cally heat the sample surface and detects the thermoreflectance
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change with the probe laser beam.[199,200]
However, in contrast to the TDTR method
in which the thermoreflectance change is
measured as a function of the delay time
between the probe beam and the pump
beam, the FDTR method records the output
signals as a function of modulated frequency.
Both the ultrafast pulsed laser and CW laser
can be used in this technique. Accordingly,
two major experimental setups have been
proposed by Schmidt et al. for carrying out
the FDTR measurements.[199] The first kind
of experimental setup is converted from
in Figure 9b by fixing the position of the
mechanical delay stage and varying the modulation frequency.
The second type of experimental setup is implemented by using
the CW lasers as the pump and probe beams (Figure 17). In
this case, the pump laser is externally modulated and the probe
beam is directed at the sample surface without passing through
the mechanical delay stage. Therefore, the setup can be built
in a less-expensive and less complicated way when compared
with the FDTR setup based on the ultrafast laser system and
the mechanical delay stage. To obtain the thermophysical prop-
erties, the amplitude and phase shift of the thermoreflectance
signals recorded by the lock-in amplifier should be analyzed
with proper heat transfer models.[74,85,199] In practice, the volu-
metric heat capacity CV of the sample is often used as one of
known input parameters to the models for deriving the thermal
conductivity value.[135,201,202]
The measurement sensitivity of the FDTR method is com-
pared with that of the TDTR method[199] and both methods
should be applicable to the small samples with dimensions
down to the order of 100 × 100 × 100 µm3.[201] Since the
thermal penetration depth of the FDTR method ranges typi-
cally from 200 nm to several micrometers at a modulation
frequency of 0.1–20 MHz, it is also regarded as a powerful
technique for probing the cross-plane thermal conductivity
of the nanoscale thin films.[86] Ong et al. have used FDTR to
measure the thermal conductivity a series of novel mate-
rials such as ligand-stabilized 3D inorganic nanocrystal
arrays (NCAs) layer (30–150 nm thick)[202] and supera-
tomic crystals (SACs).[201] These materials are expected to
serve as electronic, thermoelectric, and photonic materials
in the future. It was found that the thermal conductivities
of the NCAs and SACs are typically within a range of
0.1–0.3 W m−1 K−1 at room temperature. The FDTR technique
was able to reveal that the thermal conductivity of the NCAs
increases with increasing diameter of the nanocrystal core,
but is less sensitive to the thermal conductivity of the core
materials.[202] Malen et al. applied a fiber-aligned FDTR tech-
nique to measure the room-temperature thermal conductivity
of a 1.6 µm thick P3HT film.[203] The value was found to be
0.17 W m−1 K−1 which is in agreement with that obtained by the
conventional 3ω[65] or TDTR[98] methods.
The FDTR method is usually involved with the complicated
data reduction procedures. It also requires smooth sample
surface[14] and application of the metallic coating. Although
the method has been modified to characterize the in-plane
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thermal conductivity of the anisotropic materials by using the
beam-offset configuration, large uncertainty for measuring
the in-plane thermal conductivity below 5 W m−1 K−1 has been
observed.[135] This might bring difficulties to the reliable meas-
urement of the in-plane thermal conductivity of the OHT mate-
rials which is usually less than 5 W m−1 K−1.[47,61,63,64,67]
4.8. Light Irradiated ac-Calorimetric Method
In the light irradiated ac-calorimetric method, the sample is
periodically irradiated by a modulated light source and the
thermal response is measured by a thermocouple.[204,205] There-
fore, this method is essentially a contact method.
As will be shown later, the technique can be implemented in
several configurations. The primitive configuration proposed by
Hatta et al. in 1980s was aimed to measure the in-plane thermal
diffusivity of the thin plate samples.[204] In this configuration, a
modulated light source is used to irradiate the sample which is
partially blocked by a movable screen. The temperature oscilla-
tion on the rear side of the sample is monitored by a thermo-
couple (Figure 18). If the thickness d of the sample is assumed
to be much smaller than the thermal penetration depth, the
temperature gradient can be neglected in the film thickness
direction. The heat flow is then viewed as a 1D diffusion pro-
cess along the x-direction under the shadowed region. The ac
temperature rise measured by the thermocouple is related to
the distance x between the movable screen edge and tempera-
ture sensing location through[204]
QA
∆T ( x ) = e − kx − i (kx + π /2) (40)
2ω mod C V d
where ω mod(ω = 2π f mod ) is the angular modulation frequency,
k is the inverse thermal penetration length in the form of
k = π f mod /α , QA the absorbed power density (W m−2). The
thermal diffusivity can be retrieved from the amplitude |ΔT(x)|
or phase ϕ of the temperature oscillation as a function of the
screen offset x[206]
π f mod
αθ = (41)
(d ln ∆T ( x ) /dx )2
π f mod
αϕ = (42)
(dϕ /dx )2
where αθ and αϕ are the thermal diffusivity values extracted
from the amplitude and the phase signal, respectively.
The method was later modified by replacing the uniform
illumination by scanning line-shape and spot-like laser beam
on the sample surface.[205,207–210] Yu et al. have compared these
three configurations and suggested that the uniform illumina-
tion method is more susceptible to error than the other two
configurations.[206] On the other hand, the cross-plane thermal
diffusivity can be obtained if the spot-like light source which
excites the front surface of the sample is aligned with the
thermocouple on the opposite side of the sample,[208,209] or if
the whole front surface of the sample is homogenously irra-
diated.[158,211] It should be mentioned that the thermocouple
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Figure 18. Schematic of the experimental configuration for the light
­irradiated ac-calorimetric method proposed by Hatta et al.[204]
junction in some studies is formed between a sharp metal tip
and the metal layer coated on the backside of the sample, the
measurement technique in this case was thus named as photo-
thermoelectric method in order to emphasize the thermoelec-
tric nature of the temperature sensor.[209,210,212] It should not
be confused with the photo-thermoelectric method that will be
mentioned in Section 4.11, in which a transient thermoelectric
voltage generated from the sample itself is used to measure the
temperature rise.
In summary, the experimental apparatus for the light irra-
diated ac-calorimetric method is relatively easy to implement.
By employing the method, it is even possible to measure the
in-plane and cross-plane thermal diffusivity from the same
sample.[208] However, in order to calculate the thermal conduc-
tivity, the density and the specific heat should be determined
separately. Additional coating on the sample surface may be
necessary to enhance the light absorption.[208] The contact
resistance between the sample and the temperature sensor
(e.g., thermocouple) will also bring errors to the results.[210]
The method has been employed to characterize the in-plane
thermal diffusivity of several conducting polymer or organic
composite materials, including polypyrrole films (less than
120 µm thick),[213] nanofibrillated cellulose (NFC)/PEDOT:PSS
based mixed ion-electron conductor (30 µm thick),[214] NFC/
polystyrene sulfonate sodium based thermoelectric composite
(30 µm thick),[215] etc. In addition, Zhang et al. measured the
thermal diffusivity of a few millimeter-sized crystalline organic
semiconductors which have a transverse thickness in the range
of 300–610 µm.[158,211] The derived thermal conductivity along
growth axis for a needle- shaped 6,13-bis(triisopropylsilyleth
ynyl) pentacene crystal was found to be 1.6 W m−1 K−1 at room
temperature,[158] which is comparable with that of the quasi-1D
organic crystals consisting of segregated molecular stacks with
excellent p-orbital overlaps.[157]
4.9. Modulated Photothermal Radiometry
In the modulated photothermal radiometry (PTR), the
sample is illuminated by an intensity modulated light beam.
A monolithic Infrared detector coupled with a lock-in ampli-
fier is used to sense the temperature oscillation which can
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A linear fit of the phase (or the natural loga-

rithm of the amplitude) of Tn against f mod
results in a straight line with a slope of m
from which the thermal diffusivity is calcu-
lated as[219]
2
d
α =  π (46)
m

On the other hand, when the sample is semi-

Figure 19. Schematic sketch of the experimental setup for modulated photothermal radiometry.
a) Front-side detection configuration. b) Rear-side detection configuration.
be used to deduce the thermal transport properties of the
sample.[216–219]
This technique can be applied in either the front-side detec-
tion configuration (Figure 19a) or the rear-side detection config-
uration (Figure 19b) depending on whether the thermal emis-
sion is recorded from the irradiated surface or from the oppo-
site-side surface of the sample. The rear-side detection configu-
ration is often used to characterize the thermal diffusivity of the
solid materials. [219,220] Assuming that a sample with thickness
d is homogeneously heated by a monochromatic light beam of
intensity Iv0 at a modulation frequency ω mod(ω = 2π f mod ) from
the front surface, the light intensity at a certain position inside
the sample is expressed as I v ( x ) = I v 0 (1 − R v )e −α v x, where x is the
distance from the front surface to this location. Rv and αv are
the optical reflection coefficient and the absorption coefficient Ysb = (es /e b ) − 1
of the sample at the wavelength of the incident light, respec-
tively. By neglecting heat losses, the ac component of the tem-
perature rise inside the sample is given by[219]
I v 0 (1 − R v )α v2  (e −α d − e − q d )e q x + (e −α d − e q d )e − q x + (q k /α v )(e q d − e − q d )e −α x 
v k k v k k
∆T ( x ) =  
2κ q k (q k2 − α v2 )  e qk d − e − qk d
(43)
where q k = iω mod /α is the thermal wave vector, κ and α are
the thermal conductivity and thermal diffusivity of the sample,
respectively.
In the PTR method, in order to eliminate the instrumental
influence, normalization procedures are needed. One way of
achieving this is to normalize the signals detected at the rear
surface ΔT(d) to those recorded at the front surface ΔT(0)[219]
∆T (d ) (e −α v d − e − qk d )e qk d + (e −α v d − e qk d )e − qk d + (q k /α v )(e qk d − e − qk d )e −α v d
Tn = =
∆T (0) 2e −α v d − e qk d − e − qk d + (q k /α v )(e qk d − e − qk d )
(44)
where Tn is the normalized temperature.
Equation (44) suggests that Tn does not rely on κ, but
depends on d/ α and αvd. If one further assumes that the
sample is opaque (αvd → ∞) and thermally thick d/ α → ∞ ,
Equation (44) is reduced to[219]
π f mod π f mod
− d −i d (45)
Tn ≈ 2e − qk d = 2e α
e α
transparent, both α and αv can be simulta-
neously obtained by fitting the experimental
data to Equation (44).
In contrast to the rear-side detection con-
figuration, the front-side detection configura-
tion can be used to simultaneously retrieve
the thermal diffusivity and effusivity of the sample.[218,221,222] Its
normalization procedure involves with getting the ratio of the
frequency dependent PTR signals collected from the sample
with the backing substrate and without the backing substrate.
When the substrate is thermally thick, the normalized signal Sn
is expressed as[218]
1 + (Ysb − 1)exp( −2q k d )
Sn = (47)
1 − (Ysb − 1)exp( −2q k d )
Here, Ysb is the reflection coefficient of the thermal waves at
the interface between the sample and the substrate. It can be
written as[218]
(48)
(es /e b ) + 1
where es and eb are the thermal effusivities of the sample and
the substrate, respectively. It can be further shown that the
k k v
thermal diffusivity of the sample is expressed as[218]

4 f mod ,0 d 2
α= (49)
π
where f mod ,0 corresponds to the smallest frequency where the
phase of Sn becomes zero. Once α has been obtained, Ysb can
be calculated from the phase of the Sn data. Since eb is a known
value, one may directly calculate es by Equation (48)[218] and the
thermal conductivity of the sample by Equation (4).
If the infrared detector is replaced by a fast infrared video
camera with a high lateral resolution, the technique is termed
as lock-in infrared thermography which can be employed to
obtain the in-plane thermal diffusivity or thermal conductivity
of thin plate-like or filament-like samples.[223–226]
In summary, the modulated PTR technique is a well-­
established noncontact method for obtaining the thermal
diffusivity and thermal conductivity of the bulk materials.
­
However, the implementation of the technique involves the
( ) complicated normalization procedures.[218,219] To enhance the
light absorption, the surface coating is usually applied, which
may restrict the reuse of the sample for other test purposes. In
very recent years, the method has been employed to measure
the thermal conductivity of bulk PANI,[227] PANI/reduced

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graphene oxide composite,[227] and PANI/silver composite,[228]
as well as the transverse thermal diffusivity of millimeter-sized
organic semiconductors (up to 600 µm thick in the transverse
direction).[229] The thermal conductivity of the PANI sample
could be used as a benchmark for verifying the reliability
of the measurements. With the PTR technique. Islam
et al.[227] reported a room temperature thermal conductivity of
≈0.44 W m−1 K−1 for a PANI sample with an electrical conduc-
tivity of less than 0.1 S cm−1, which is consistent with that of
the low-σ sample (0.46 W m−1 K−1 at σ = 0.48 S cm−1) meas-
ured by the comparative method by Abad et al.[184] The result
is also comparable with the cross-plane thermal conductivity
of 0.59 W m−1 K−1 measured by the conventional 3ω tech-
nique for a 5 µm thick PANI film with an electrical conduc-
tivity of 93 S cm−1.[13]
4.10. Photoacoustic (PA) Method
In the PA method,[230–232] an intensity modulated radiation
heats a sample located in a closed gas cell (PA cell). A gas layer
in contact with the sample surface is heated periodically and
is driven to expand and contract like a thermal piston. The
periodic change of pressure produces an acoustic wave that is
detected by a microphone, which can be used to derive the ther-
mophysical properties of the sample.
The PA effect was first theoretically explained by Rosencwaig
and Gersho who revealed that the PA signal (or the variations
of the gas pressure) is given by[230]
γ g µgPg,0θ i(ω mod t − π4 )
∆Pg (t ) = e (50)
2LgT0
where Pg,0 is the static pressure and ω mod is the angular modu-
lation frequency. μg(µg = 2α g /ω mod , where αg is the thermal
diffusivity of the gas) and γg are the thermal diffusion depth
and the ratio of specific heats of the gas, respectively. T0 is
the average temperature. Lg is the gas column length. θ is a
complex expression for the temperature oscillation at the gas/
sample interface.
The theory was soon extended by McDonald and Wetsel
who suggested that mechanical vibration of the sample sur-
face due to thermal expansion exerts work and subsequently
causes additional temperature change on the gas medium.[231]
Recently, Hu et al. proposed a generalized expression for the
PA effect in a multilayer system.[233]
Figure 20. Schematic sketch of the photoacoustic measurement setup. a) Front-side detection configuration. b) Rear-side detection configuration.
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Experimentally, the PA signal can be recorded with the front-
side detection configuration (Figure 20a) and the rear-side
detection configuration (Figure 20b). In order to eliminate the
frequency dependence of the instrumental responses and non-
essential signal-related proportionality factors, normalization
of the PA signals is typically needed. For example, in order to
measure the thermal diffusivity of the solids, several normaliza-
tion procedures have been proposed. Pessoa et al. performed
the normalization by taking the signal’s ratio in the rear-side
and front-side detection configurations for one-single layered
sample at a single modulation frequency.[234] Balderas-López
took the signal ratio from the investigated sample and a refer-
ence sample which were both measured in the rear-side detec-
tion configuration.[235] Alternatively, the test sample can be
measured in the rear-side detection configuration, while the
reference sample in the front-side configuration.[236]
In principle, the thermal conductivity of the bulk sample can
be determined by, for instance, putting the sample in thermally
contacted with a backing materials whose thermophysical prop-
erties have been known.[237] On the other hand, by performing
the measurements at a frequency up to 20 kHz and applying
the advanced multilayer model[233] for data reduction, the tech-
nique has been extended to measure the thermal conductivity
of the thin film with sub-micrometer thickness.[238,239]
The PA technique is a noncontact method featured with
a unique and inexpensive detecting system. It can actually
measure the cross-plane thermal conductivity of the films and
the bulk samples with rough surfaces.[238] The toleration of the
method for the surface conditions may allow one to measure
the thermal conductivity of those OHT materials whose sur-
faces are so rough that the use of the techniques such as the
conventional 3ω method and the TDTR (or FDTR) method
should be precluded. A disadvantage of this technique is that
it needs extensive calibration and normalization procedures
to eliminate the PA signal distortions caused by the electronic
circuitry.[234–236,238,240] Additionally, the surface coating for the
sample is needed to enhance the laser power absorption, which
will limit the use the sample for other purposes. To date, the
method has been utilized to measure the thermal conductivity
of several OHT materials including undoped PCDTBT film,[183]
Bi2Te3 nanowire array/SU-8 epoxy resin nanocomposite,[241]
poly(3-octylthiophene-2,5 diyl) (P3OT) film and MWCNT/P3OT
composites,[242] polythiophene film and nanofibre arrays,[60]
as well as P3HT nanotube array,[243] etc. The thickness of the
OHT samples usually ranges from several micrometers[183] to
several tens of micrometers.[241–243] Among these materials,
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www.advancedsciencenews.com
the P3OT film was found to have a thermal conductivity
of 0.21 W m−1 K−1,[242] which is in agreement with the values
reported for structurally similar polymers such as P3HT.[98,143]
The value of the undoped PCDTBT film was measured to be
0.20 W m−1 K−1, which is in reasonable agreement with the result
obtained from the SThM-3ω measurement (0.25 W m−1 K−1).[183]
4.11. Photo-Thermoelectric Method
The photo-thermoelectric method was proposed by Kuria-
kose et al.[244,245] who used the transient photo-thermoelectric
response of the sample as a probe to explore its own thermo-
physical properties. The experimental setup is schematically
illustrated in Figure 21. The top and bottom surfaces of the ther-
moelectric sample are covered with thin metal electrodes for
extracting the thermoelectric voltage. The bottom of the sample
is thermally contact with a substrate with known thermal dif-
fusivity and thermal effusivity. The top surface of the sample is
heated by a modulated laser beam. At a fixed modulation fre-
quency, the thermoelectric signal ΔVth obtained with presence
of the substrate is normalized by the signal ΔVth,0 obtained with
air as the backing material[244]
∆Vth
Vn =
∆Vth,0
where Vn is the normalized signal. By fitting Vn to a theoretical
model,[244] both thermal diffusivity α and thermal effusivity e
of the sample can be calculated. By applying Equation (4), the
thermal conductivity κ of the sample is determined.
The method provides a simple and rapid way to measure
the thermal diffusivity and thermal conductivity for the bulk
thermoelectric sample. The OHT materials such as 6.6 wt%
oxidized SWNTs/doped PANI composite have been tested
by this method. Its thermal conductivity was measured to be
0.83 W m−1 K−1, which agrees well with that obtained from the
conventional photothermal radiometry.[244] Another interesting
feature of this method is that it can be adapted to measure the
thermal conductivity of thermoelectric liquids, such as tetrado-
decylammonium nitrate salt/1-octanol mixture.[245] It should be
noted that the sample should possess a relatively large ­Seebeck
Figure 21. Schematic illustration of the photothermoelectric experimental
setup proposed by Kuriakose et al.[244]
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coefficient in order to achieve a high measurement accuracy,
although the samples with a Seebeck coefficient as low as
5.8 µV K−1 were still measurable.[244]
5. Summary
This paper presents a brief review on the commonly used and
newly developed techniques that can be used for characterizing
the thermal conductivity of the OHT materials. Each individual
technique mentioned above has its own merits and l­imitations.
A suitable method is selected primarily based on the factors such
as the characteristics of the sample (e.g., dimensionality, size,
morphology, mechanical properties, optical properties, thermal
properties, etc.), the temperature range of the measurement,
the required measurement accuracy, and so on. When a specific
method has been selected, it is crucial to understand its theo-
retical backgrounds and possible error sources. Careful sample
preparations or instrumentation calibrations are also important
for carrying out reliable measurements. To further ensure the
accuracy and creditability of the results, some researchers prefer
to crosscheck their results by different techniques.[126,183,244]
With the continuing development of the novel OHT materials,
some measurement techniques may receive more attention in
the future. For example, the characterization of the ­anisotropic
(51)
thermal conductivity has become an important topic in the OHT
community. The combined use of the relevant tools (such as the
various 3ω techniques, the thermoreflectance ­techniques, the
light irradiated ac-calorimetric method, the modulated photo-
thermal radiometry, etc.) might be helpful for tackling the issue.
On the other hand, it has been shown in many studies that the
thermal conductivity can be simultaneously measured with the
Seebeck coefficient and the electrical conductivity on the same
sample.[22,61,157] This feature is highly desirable, since calculating
the ZT value from the TE properties measured on different sam-
ples may cause errors. This is due to the fact that the samples
are usually more or less inhomogeneous even when they are
chosen from the same batch.[34]
Acknowledgements
The authors would like to acknowledge the financial supports from
the National Natural Science Foundation of China under grant nos.
51573190 and 61176083, and the State Key Development Program for
Basic Research of China under grant no. 2011CB932801.
Conflict of Interest
The authors declare no conflict of interest.
Keywords
hybrid thermoelectric materials, organic thermoelectric materials,
thermal conductivity measurement
Received: February 13, 2019
Revised: May 15, 2019
Published online:
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