Thermoelectric transport properties of polycrystalline SnSe alloyed with PbSe

Tian-Ran Wei, Gangjian Tan, Chao-Feng Wu, Cheng Chang, Li-Dong Zhao, Jing-Feng Li, G. Jeffrey Snyder, and
Mercouri G. Kanatzidis

Citation: Appl. Phys. Lett. 110, 053901 (2017); doi: 10.1063/1.4975603

View online: http://dx.doi.org/10.1063/1.4975603
View Table of Contents: http://aip.scitation.org/toc/apl/110/5
Published by the American Institute of Physics

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 APPLIED PHYSICS LETTERS 110, 053901 (2017)

Thermoelectric transport properties of polycrystalline SnSe alloyed

with PbSe
Tian-Ran Wei,1 Gangjian Tan,2 Chao-Feng Wu,1 Cheng Chang,3 Li-Dong Zhao,3
Jing-Feng Li,1,a) G. Jeffrey Snyder,4 and Mercouri G. Kanatzidis2
1
State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering,
Tsinghua University, Beijing 100084, China
2
Department of Chemistry, Northwestern University, Evanston, Illinois 60208, USA
3
School of Materials Science and Engineering, Beihang University, Beijing 100191, China
4
Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208, USA
(Received 29 November 2016; accepted 23 January 2017; published online 3 February 2017)
Single-crystal SnSe has been found to exhibit exceptional thermoelectric performance, but the
efficiency of polycrystalline samples is still far from satisfactory. In this work, with an intention to
effectively suppress heat conduction and minimally affect hole transport, we alloyed p-type
polycrystalline SnSe with PbSe. Single-phase Sn1xPbxSe solid solutions were formed up to
x  0.12. The lattice thermal conductivity was reduced from 1.4 to 0.85 W m1 K1 by 12 at. %
PbSe alloying due to strain and mass fluctuations. Interestingly, the Seebeck coefficient and carrier
concentration were nearly unchanged by Pb substitution, indicating a constant effective mass and
an undisrupted valence band maximum. A peak figure of merit (ZT) of 0.85 at 800 K was obtained
in the x ¼ 0 sample, and relatively high performance was also achieved in solid solutions. A concise
model was developed involving multiple carrier scattering mechanisms, capturing the dependence
of the mobility on composition and temperature. Published by AIP Publishing.
[http://dx.doi.org/10.1063/1.4975603]

Thermoelectric materials are of widespread interest for
direct conversion between heat and electricity, offering a
prospect for the sustainable utilization of energy and the
effective control of greenhouse gas emissions.1 Searching
for promising materials, not only with a high ZT (defined as
ZT ¼ S2T/(qj), where S, T, q, and j are the Seebeck coeffi-
cient, absolute temperature, electrical resistivity, and thermal
conductivity, respectively) but also composed of earth-
abundant constituents, has become a popular trend in this
field.2 Recently, the binary compound tin selenide (SnSe)
was discovered to possess an ultrahigh ZT in single crys-
tals.3–5 Since then, more attention has been switched to the
polycrystalline counterparts with better machinability,6,7 but
their performance is still inferior to that of single crystals.
The unexpectedly higher thermal conductivity and impaired
mobility are likely to be the bottleneck.8,9
Alloying is an effective approach to impede phonon
transport and also to modify the electronic band structure.10
For SnSe, alloying with SnS11 and SnTe12 remarkably fur-
ther reduces the already low thermal conductivity.
Compared to the anion-site studies, alloying at cation site
seems more attractive for p-type SnSe, which is expected to
leave the valence band maximum (VBM, composed mainly
of anion orbitals13) less disturbed,14,15 thus giving a possibil-
ity of the decoupling charge and phonon transport.
Nonetheless, related reports focus on either phase-separated
composites16 or n-type SnSe;17 systematic studies on cation-
alloyed p-type SnSe with insight into the structural variation
and transport mechanisms are rather scarce so far. In this
work, we alloyed Na-doped SnSe with PbSe, a promising
a)
jingfeng@mail.tsinghua.edu.cn
thermoelectric material from the same IV–VI family with a
large and heavy cation, cubic structure, and high mobility.18
We find that PbSe alloying effectively lowers the thermal
conductivity, and more importantly, leaves VBM essentially
unperturbed, which provides a useful platform for separately
tuning electrical and thermal properties in thermoelectric
SnSe.
Polycrystalline (Sn1xPbx)0.99Na0.01Se (x ¼ 0–0.2) sam-
ples were fabricated via melting, annealing, and pulverizing
followed by spark plasma sintering (SPS) as described else-
where.9 Stoichiometric ratios of the elements were loaded
into a carbon-coated double quartz tube that was evacuated
and flame-sealed, melted at 1223 K for 10 h, and annealed at
873 K for 48 h. The obtained ingot was ground in air into
powders that were densified at 873 K under 50 MPa for 5 min
by SPS. The phase purity and structure were investigated by
Rigaku X-ray diffraction (XRD). Morphologies of samples
were examined by Zeiss field emission scanning electron
microscopy (FE-SEM). Elemental distribution was mapped
using the electronic probe microscopic analysis (EPMA,
JEOL). The Seebeck coefficient (S) and electrical resistivity
(q) were measured using ZEM-3 from Ulvac-Riko. Hall
measurements were conducted by a commercial system
(ResiTest 8340DC, Toyo). Thermal conductivity (j) was cal-
culated via j ¼ D  CP  d, where D is the thermal diffusiv-
ity (Netsch LFA457), CP is the heat capacity, and d is the
density measured by the Archimedes methods. Considering
the anisotropy, transport parameters were measured per-
pendicular to the SPS pressure direction (i.e., “in-plane”
measurements). S, q, and D were also measured in a heat-
ing-and-cooling cycle for two samples (Figure S1 of the
supplementary material).

0003-6951/2017/110(5)/053901/5/$30.00 110, 053901-1 Published by AIP Publishing.

053901-2 Wei et al. Appl. Phys. Lett. 110, 053901 (2017)

Figure 1(a) shows the XRD spectra of the pulverized
ingots. The main peaks are indexed to the orthorhombic
phase with a Pnma symmetry. Tiny amount of second phase
(marked by *) emerges when x reaches 0.12, and its presence
is more obvious in x ¼ 0.16 and 0.20 samples, which was
identified as the PbSe-based solid solution. This result sug-
gests that the samples have reached a two-phase region at
around x ¼ 0.12 that is close to the previously reported val-
ues (15–20%).19,20 Since PbSe has a smaller bandgap, ligh-
ter valence band, higher mobility and thermal conductivity
than SnSe matrix,18 the two-phase composites (x ¼ 0.16 and
0.20) are likely to exhibit different transport properties from
the single-phase solid solutions. Enlarged XRD patterns
(Figure 1(b)) show that with the increasing Pb content, the
(400) and (002) peaks shift to lower and higher 2h values,
respectively, indicating stretched a and compressed c. These
changes in lattice constants beyond x ¼ 0.12 indicate a con-
tinued increase in the Pb content for the main SnSe-based
phase. The true maximum solubility of Pb in the ternary Pb-
Sn-Se system (or quaternary Na-Pb-Sn-Se) can vary depend-
ing on the Se content as demonstrated in filled skutterudite
ACo4Sb12 (Ref. 21) and could be determined by phase
boundary mapping.
As is intuitively expected, when a larger atom (Pb)
replaces a smaller one (Sn), the lattice will expand accord-
ingly, which is the case of a and b, but not c (Figure 1(c)),
and similar results have also been found by Chang et al.17 It
is interesting to note that this trend is analogous to the one
caused by the increasing temperature, that is, the displacive
Pnma-Cmcm phase transition.22–24 Here, the alloying-
induced structural variation can be understood from the per-
spective of the lone pair. In Pnma-SnSe, there exists a lone
pair (Sn 5 s electrons) that is stereochemically expressed,14,25
forming a distorted SnSe6 octahedron. For Fm3m-PbSe, the
lone pair visually disappears (aside from the entropic behav-
ior),26 and the cation bonds equally with six anions, exhibit-
ing a perfect octahedron coordination. The Cmcm structure
possesses an intermediate degree of symmetry: the lone pair
is partly expressed, and the bonds become undistinguishable
to each other in the a-c plane, yielding a less distorted octa-
hedron. Therefore, we tentatively conclude that PbSe alloy-
ing is likely to promote such a transition from a low- to a
high-symmetry structure, where the “fade-out” of the lone
pair is important.
Polycrystalline Sn1-xPbxSe samples with high densities
(Table I, >95% of the theoretical one, 6.19 g cm3) exhibit a
layered microstructure (Figure 2(a)) that stems from the
quasi-two-dimensional crystal structure. Within the solubil-
ity, a homogeneous distribution of main elements was
observed down to 100 nm (Figures 2(c)–2(e)), again con-
firming that SnSe-based solid solutions have been formed,
and the samples are of good quality for the following trans-
port analysis.
Consistent with our expectation, Pb substitution is effec-
tive in suppressing heat transport for x ¼ 0–0.12, as shown in
Figures 3(a). Higher j values are seen in two-phase compo-
sites for x ¼ 0.16 and 0.20 probably due to the existence of
high-j PbSe-based phase as well as the narrowed bandgap
(Figure S2 of the supplementary material). The lattice ther-
mal conductivity (jL ¼ j  LT/q, where L is the Lorenz num-
ber) decreases from 1.4 W m1 K1 for x ¼ 0 to 0.85 W m1
K1 for x ¼ 0.12 at room temperature (RT). It is also seen
that jL in this work is higher than that of single crystals3,4 but
comparable with other polycrystalline samples,6,7,9,12 which
may be related to defects, off-stoichiometry, and air oxidation
(samples were ground in air) that are commonly found in
SnSe polycrystals.27 In order to reveal the effect of alloying
on blocking phonon transport, Debye approximation was
employed to model the data. jL can be written as
 3 ð h =T
kB kB T a
e z z4
jL ¼ 2 sðzÞ dz; (1)
2p v h 0 ðez  1Þ2
where v is the average sound speed, ha is the average acous-
tic Debye temperature, z ¼ hx=kB T is the reduced phonon
energy, and s(z) is the relaxation time.28 The overall phonon-
scattering frequency is the sum of the interaction rate for
each mechanism: s1 ¼ s1 1
U þ sPD , where the subscripts U
and PD refer to the Umklapp process and the point-defect
scattering, respectively. Here, the Normal (N-) process was
not taken into account considering the high temperature and
abundant defects.29 Also, phonon scattering by voids and
boundaries is not important due to the large size of these
defects.12
For U-process, we adopted the following expression:30

kB 2 c2 2 3 ha =3T
s1
U ðzÞ ¼ zT e ; (2)
hMv2 ha

TABLE I. Density and thermal transport parameters of Na-doped Sn1-xPbxSe

solid solutions (x  0.12) at room temperature.

x d (g cm3) jL (W m1 K1) C Cm Cs

0.00 5.94 1.39 0 0 0

0.04 5.97 1.07 0.057 0.015 0.042
FIG. 1. (a) Full-range and (b) enlarged powder-XRD patterns, and (c) lattice 0.08 6.06 0.971 0.088 0.027 0.061
parameters varying with the Pb content for Na-doped Sn1-xPbxSe ingots. “*” 0.12 6.12 0.852 0.165 0.038 0.127
in (a) and (b) denotes PbSe-based alloys as a secondary phase.
053901-3 Wei et al. Appl. Phys. Lett. 110, 053901 (2017)

 2 .
MSn  MPb
C m ¼ x ð1  x Þ 2; (4)
M

and Cs was set as a fitting value considering the large ambi-

FIG. 2. (a) Fractured and (b) polished surface morphologies of x ¼ 0.12 sam-
ple with a homogeneous distribution of (c) Sn, (d) Pb, and (e) Se.
where M is the average mass per atom and c is the Gr€uneisen
parameter. Here, ha ¼ 107 K, v ¼ 1634 m s1, and c ¼ 2.7
were taken from our previous report.12 The frequency of
point-defect scattering was given as31
kB 4 Vatom C 4 4
s1
PD ðzÞ ¼ z T ;
4ph4 v3
where C ¼ Cm þ Cs quantifies the fluctuations in mass and
strain introduced by impurity atoms. For Sn1xPbxSe solid
solutions, Cm was calculated via32
guity in ionic/atomic size and the phenomenological parame-
ter e.33 The dependence of jL on T is shown in Figure 3(b)
using the above equations, and jL as a function of x was also
plotted in Figure 3(f) using C ¼ 1:45xð1  xÞ, where the pre-
factor 1.45 is a fitting value combining the mass and strain
disorder. As seen from modeling parameters in Table I, the
strain fluctuations have a dominant role in alloy scattering of
phonons, but the contribution from mass fluctuations is also
significant due to the large mass difference between Sn
(118.7 g mol1) and Pb (207.2 g mol1) when compared to
the Te-substituted case.12
Despite the lowered thermal conductivity, the ZT value
is not enhanced by alloying as depicted in Figure 3(c). This
is attributed to the greatly decreased carrier mobility which
leads to increased electrical resistivity, q (Figure 3(d)). As
shown in Figure 3(f), the drop of lH with x outweighs the
decrease in jL, while the density-of-state effective mass,
md*, remains relatively constant as (1.0 6 0.05) m0 (m0 is the
mass of one free electron). Therefore, the thermoelectric
quality factor b / m3=2 lT=jL (Ref. 34) of the alloys is not
enhanced, implying that reoptimization of the carrier con-
centration (the Na doping concentration) is not likely to
change the conclusion. In the following discussion, we will
illustrate in detail the effect of alloying on electrical trans-
port and give insight into the band structure and various scat-
(3) tering mechanisms.
It is interesting to find that md* is unchanged by alloying
as shown in Figure 3(f), which derives from the nearly
composition-independent S and nH (Figure 4(a)) under the
approximation of an equivalent single parabolic band

FIG. 3. Thermoelectric properties of Na-doped Sn1-xPbxSe alloys: (a) thermal conductivity, (b) lattice thermal conductivity, (c) ZT, (d) electrical resistivity, and
(e) the Seebeck coefficient as a function of temperature; (f) mobility and lattice thermal conductivity normalized to the x ¼ 0 sample and density-of-state effec-
tive mass (inset) as a function of Pb content at 300 K. Curves in (b) and (f) are calculation results; dashed lines are used for the two-phase region (x > 0.12).
Error bars in (b) represent 7% uncertainty including measurement and calculation of the Lorenz number, and those in (c) denote 20% uncertainty for ZT.
053901-4 Wei et al.
(SPB).9,35 This is a clear indication that the configuration of
the equivalent VBM is well preserved in Sn1xPbxSe solid
solutions, which is consistent with the theoretical calcula-
tions. The latter indicate that the VBM of SnSe comes
mainly from anion orbitals (Se 4p),13 so alloying at cation
site can help maintain the VBM structure.
The Hall mobility, lH, decreases from 13 to 4.2 cm2
1 1
V s with x (x ¼ 0–0.12) at RT, accounting for the
increased q. For x ¼ 0.16 and 0.20, lH turns to increase as
shown in Table S1 of the supplementary material, which is
also related to the PbSe-based secondary phase with a small
effective mass and high mobility. Since m* of the solid solu-
tions is unchanged by Pb substitution as shown above, the
mobility can be written in the form similar to that of relaxa-
tion time (s) limited by various scattering processes, i.e.,
acoustic-phonon (AP) scattering, grain-boundary (GB) scat-
tering, and point-defect (PD) scattering of carriers
l1 ¼ l1 1 1
AP þ lGB þ lPD : (5)
GB scattering is proposed here in association with energy
barriers formed at the grain (or sub-grain) boundaries due to
the air oxidation and crystal defects. This type of scattering
has been found suitable for understanding electrical transport
in polycrystalline SnSe samples.8,9,12 If we focus solely on
the alloying effect, the first two terms in Eq. (5) can be tenta-
tively combined as l0 that is independent of Pb content. Or
more simply, l0 can be treated as the mobility of the x ¼ 0
sample. Then, the mobility is
1 l0
l¼ ¼ : (6)
l1
0 þ l1
PD 1 þ l0 =lPD
The PD scattering rate is proportional to the mole ratio of
guest and host atoms,36,37 so we can write
l0
l¼ ; (7)
1 þ Axð1  xÞ
where A is the relative intensity of alloy scattering that is
related to intrinsic material parameters but independent of
the alloy atom content. Using l0 ¼ lx ¼ 0 ¼ 13 cm2 V1 s1
and A ¼ 21.5 as the fitting value, the decreasing trend of
mobility with x is well captured by the model as shown in
Figures 3(f) and 4(b). Various carrier scattering mechanisms
are further clarified in the T-dependent data (Figure 4(c)).
Here, we assume the mobilities limited by AP, GB, and
PD are proportional to T3/2 (Ref. 35), T1/2 exp(EB/kBT)
Appl. Phys. Lett. 110, 053901 (2017)
FIG. 4. (a) The Hall carrier concentra-
tion (red, left axis), the Seebeck coeffi-
cient (blue, right axis), and (b) the Hall
mobility as a function of the Pb content
at RT; (c) mobility limited by various
carrier scattering mechanisms: acoustic
phonons (AP), grain boundaries (GB),
point defects (PD), and their combined
effects. The lines in (b) and (c) are cal-
culation results. Error bars of S, nH,
and lH represent 5%, 10%, and 10%
uncertainty, respectively.
(Refs. 12 and 38), and T1/2 (Ref. 36) respectively, which
are depicted as the dashed lines. By using Eq. (5)–(7) with
fitted pre-factors, the calculation (solid lines) closely
matches our experimental data for both pristine and alloyed
samples. The consistency demonstrated in Figures 4(b) and
4(c) indicates that the drop of mobility is caused only by
alloying-induced random disorder, again confirming the
argument that the equivalent VBM of SnSe was not signifi-
cantly disrupted by Pb substitution.
In summary, thermoelectric transport properties of Pb-
substituted SnSe alloys were studied. Single-phase Sn1xPbxSe
solid solutions were formed for x ¼ 0–0.12. PbSe alloying was
found to facilitate a structural transition to high symmetry pos-
sibly due to the fading steric activity of the lone pair. A 39%
reduction in lattice thermal conductivity was realized by 12%
PbSe alloying through intensified alloy scattering of phonons.
Meanwhile, the equivalent valence band maximum of SnSe
appears to be unperturbed by the cation-site substitution. This
is likely because the VBM is composed predominantly of Se-
based p orbital states and has a minor contribution from the
metal orbital states.13 This is different from the situation in
rock salt PbQ (Q ¼ S, Se, Te) and SnTe systems, where the
VBM has a significant contribution from lone electron pair s
states. A maximum ZT ¼ 0.85 was achieved in the x ¼ 0 sam-
ple at 800 K, and no significant enhancement was realized by
alloying due to the impaired mobility that was quantitatively
described by a mixed carrier scattering process involving
acoustic phonons, grain boundaries, and point defects. The
findings in this work should help further understand and ratio-
nally tune electrical and thermal transport properties in poly-
crystalline SnSe.
See supplementary material for electrical transport prop-
erties of all the compositions, optical absorption spectra, and
thermoelectric properties measured in a heating-and-cooling
cycle.
This work was supported by NNSF (No. 11474176) and
973 Program (No. 2013CB632503) of China. At
Northwestern University, this work was also supported by
DOE of U.S. under Award No. DE-SC0014520 (G.T. and
M.G.K.), and S3TEC funded by DOE under Award No. DE-
SC0001299 (G.J.S.).
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