Author’s Accepted Manuscript

Bi2Te3-MWCNT nanocomposite: An efficient

thermoelectric material

Sunil Kumar, Deepti Chaudhary, Punit Kumar

Dhawan, R.R. Yadav, Neeraj Khare

www.elsevier.com/locate/ceri

PII: S0272-8842(17)31708-X
DOI: http://dx.doi.org/10.1016/j.ceramint.2017.08.017
Reference: CERI15971
To appear in: Ceramics International
Received date: 14 July 2017
Accepted date: 2 August 2017
Cite this article as: Sunil Kumar, Deepti Chaudhary, Punit Kumar Dhawan, R.R.
Yadav and Neeraj Khare, Bi 2Te3-MWCNT nanocomposite: An efficient
thermoelectric material, Ceramics International,
http://dx.doi.org/10.1016/j.ceramint.2017.08.017
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Bi2Te3-MWCNT nanocomposite: An efficient thermoelectric material

Sunil Kumar1, Deepti Chaudhary1, Punit Kumar Dhawan2, R.R. Yadav2, Neeraj Khare1,*
1
Department of Physics, Indian Institute of Technology Delhi, Hauz Khas, New Delhi-

110016, India.
2
Department of Physics, University of Allahabad-211002, Uttar Pradesh, India.
*
Corresponding Author Electronic mail: nkhare@physics.iitd.ernet.in

Abstract

Bi2Te3–MWCNT nanocomposite has been synthesized by hydrothermal technique and

demonstrate the role of MWCNT for thermoelectric properties. Herein, MWCNT has been

used as conducting filler, which leads to the enhancement in the electrical conductivity in the

case of nanocomposite. Bi2Te3–MWCNT nanocomposite shows ~22% decrease in the

thermal conductivity as compared to Bi2Te3 nanostructures, which is attributed to the

enhanced phonon scattering at the interfaces of Bi2Te3–MWCNT nanocomposite. Due to the

increase in the electrical conductivity and decrease in the thermal conductivity, the overall

enhancement in the figure of merit is ~45% in Bi2Te3–MWCNT nanocomposite as compared

to Bi2Te3 nanostructures.

Key words: Electrical conductivity; Thermal conductivity; Bi2Te3; Nanocomposites

1. Introduction

In recent years, generation of green energy has attracted considerable attention to fulfil the

demand of energy and reduction of emission of harmful gases [1]. Thermal energy can be a

potential source of sustainable energy due to its abundance, environment friendly and its

conversion into electrical energy using a thermoelectric devices [2, 3]. The performance of

thermoelectric materials is quantified by figure of merit (ZT) [4],

S 2
ZT  T (1)


where S is the Seebeck coefficient,  is the electrical conductivity, κ is the thermal

conductivity and T is absolute temperature. S2 is defined as thermoelectric power factor

(TEP). To enhance the performance of a thermoelectric device, thermoelectric materials

needs to have a higher value of TEP, low thermal conductivity and high value of Seebeck

coefficient [5]. In order to reduce joule heating the electrical conductivity should be high [6].

However, Seebeck coefficient, thermal conductivity and electrical conductivity are dependent

to each other, therefore it is very difficult to achieve high conversion efficiency in bulk

materials [7]. The increase in the carrier concentration will increase the electrical

conductivity but decrease the value of Seebeck coefficient. Therefore, to achieve higher

value of TEP, the optimised value of carrier concentration is required [8]. Recently,

significant improvement has been observed in the thermal energy conversion efficiency of

nanocomposites by quantum confinement and charge carrier filtering to increase the Seebeck

coefficient without reducing the electrical conductivity [9, 10]. In the case of conducting

filler based thermoelectric materials, the carrier concentration can be optimized for

decoupling both the parameters (S and ) using interfaces [11]. At interfaces, low energy
charge carrier filter out and high energy charge carriers can travel through the conducting

path in the nanocomposites [12]. The work function of conducting filler and nanostructures

should be similar to transport high energy charge carriers across the interfaces and to

construct conducting channel and low energy filtering surface [13]. The conducting filler

introduces many conducting path between inorganic matrix and thereby increases the

mobility to promote S and  [14, 15]. In order to avoid thermal shorting, low thermal

conductivity can be achieved in the case of nanocomposite thermoelectric material in which

lattice scattering of phonons increases due to a large number of interfaces [1]. Ju et al. [16],

reported a significant reduction in thermal conductivity of Bi2Te3 nanowire/graphene

nanocomposite.

Generally, nanocomposites and superlattices are prepared at higher temperature using

molecular beam epitaxy, melt spinning techniques etc. [12, 17]. Recently, there have been a

lot of interest to develop a low cost and simple technique such as sol-gel, wet-chemical and

hydrothermal technique for the formation of nanocomposite materials [9, 13, 14].

Bismuth Telluride (Bi2Te3) is a promising thermoelectric material with superior energy

conversion efficiency at room temperature [18]. Me et al. reported the interfacial barrier

height to filter out the low energy carrier by introducing conducting filler (P3HT) into Bi2Te3

nanocomposites matrix [5]. Enhanced figure of merit in Bi2Te3-P3HT, MoS2-Bi2Te3, Bi2Te3-

graphene and Sb2Te3-Pt nanocomposites are also reported [5, 19-21]. Lai et al. [22]

introduced MWNCT into rutile TiO2 to significantly enhance thermoelectric power factor of

the nanocomposite. Among the various conducting filler, CNTs as the conducting filler is

attracting because it has extraordinary electrical, mechanical and thermal properties even at

room temperature [23]. However, it is very difficult to get good dispersion of conducting

filler into the inorganic matrix by sol-gel or ball milling techniques [24]. Notably,
hydrothermal technique is an easy technique to get homogeneous dispersion of CNT filler

into the inorganic matrix [25].

In this report, a thermoelectric study for enhancing figure of merit of Bi2Te3 by

incorporation of MWCNT using hydrothermal technique has been carried out. In Bi2Te3-

MWCNT nanocomposite, Bi2Te3 nanostructures are decorated over the surface of MWCNT.

Bi2Te3-MWCNT nanocomposite showed an enhanced figure of merit as compared to Bi2Te3.

In addition, the surface potential study of nanocomposite has also been carried out to study

the nature of different phases present in the nanocomposite, affecting the thermoelectric

properties.

2. Experimental details

2.1 Synthesis of Bi2Te3 nanostructures

Bi2Te3 nanostructures were synthesized by hydrothermal technique. Initially, an

appropriate amount of tellurium was added to the aqueous solution of sodium borohydride

and sodium hydroxide and the solution was heated with continuous stirring at 65C for 15–20

min till the formation of hydrogen stop (solution A). An aqueous solution containing bismuth

chloride was also prepared by dissolving bismuth chloride in deionized water (solution B).

Afterwards, solution A and B were mixed together and stirred for 1h at 65C. Excess sodium

hydroxide was added to maintain the pH of the solution at 12 during the synthesis. The final

solution was filled in a stainless steel autoclave with Teflon liner and the autoclave assembly

was kept in an electric oven at 180C for 12h. The resulting black precipitate was centrifuged

and washed with distilled water, ethanol and acetone respectively. Finally, the dark product

(Bi2Te3) was dried in an oven at 70C for 5h.

2.2 Synthesis of Bi2Te3-MWCNT nanocomposite

Figure 1 shows the schematic of the synthesis process of Bi2Te3–MWCNT

nanocomposite. MWCNT surface was used as substrate for the growth of Bi2Te3–MWCNT
nanocomposite. Initially, MWCNT were added to an aqueous solution of bismuth chloride

and sonicated for 1h which is named as solution C. Afterward, appropriate amount of

tellurium was added to the aqueous solution of sodium borohydride and sodium hydroxide

and then resulting solution was heated to 65C for 15–20 min, till the formation of hydrogen

stops (Solution D). Afterwards, Solution C and solution D were mixed together and stirred

for 1 h at 65C. The resulting solution was transferred to a stainless steel vessel (autoclave)

with Teflon liner. The autoclave was kept in an oven at 180C for 12 h. The final product was

filtered, washed and dried at 70C for 5 h, and denoted as Bi2Te3–MWCNT nanocomposite.

2.3 Characterization techniques

The structural properties of Bi2Te3-MWCNT nanocomposite were studied using X-ray

diffractometer (Rigaku Ultima-IV with Cu-Kα radiation source). The morphology of the

samples was studied by scanning electron microscopy (SEM) [Model No. -Quanta 3D FEG,

FEI] and transmission electron microscope (TEM) [JEOL JEM-2200 FS]. For electrical

measurements, pellets of the Bi2Te3 and Bi2Te3-MWCNT nanocomposite powder were

prepared using the hydrothermal press at 5 ton/inch2 pressure. Renishaw plc Micro Raman

Spectrometer was used for the measuring the Raman spectra using 514 nm laser. Surface

potential measurements were carried out using the Atomic Force Microscope (AFM) [Bruker

Dimension Icon]. A Pt-Ir coated antimony doped Si cantilever (Model: SCM-PIT from

Bruker) of curvature 30 nm at 75 kHz frequency was used for Kelvin Probe Force

Microscopy (KPFM) measurements. A scan rate of 0.75 Hz and lift height of 60 nm was used

for both the samples to obtain the surface potential image. Electrical contact pads of area ~2

mm2 were deposited by e-beam evaporation technique. The temperature dependent electrical

conductivity () was measured in the four probe configuration set up under vacuum (10-3

Torr) condition. The charge carrier concentration and mobility was measured by Hall

measurement. The Seebeck coefficient was measured by a differential method using home
designed Seebeck coefficient measurement setup [26]. The temperature difference between

the hot side and cold side was maintained at 5K during the entire measurement. Seebeck

voltage was measured using Keithley 2182A nanovoltmeter. The hot disc thermal constants

analyzer (Hot Disc Inc., Sweden) is used for the measurement of thermal conductivity by

TPS (transient plane source) method in which wide range (0.02-200 W/mK) of the thermal

conductivities can be measured.

3. Results and discussion

XRD pattern of Bi2Te3, and Bi2Te3-MWCNT nanocomposite is shown in Figure 2. The

XRD pattern of Bi2Te3 nanostructure has diffraction peaks corresponding to (101), (015),

(1010), (110), (116), (205), (0210), (1115) and (125) planes of single phase Bi2Te3 [JCPDS

card no. 15-0863]. No visible peak corresponding to MWCNT in Bi2Te3-MWCNT

nanocomposite was observed due to the low amount of MWCNT in the nanocomposite. The

particle size of the sample is estimated using Debye–Scherer equation,

k 
d (2)
 cos 

where kβ is 0.9, λ is Cu-Kɑ wavelength (1.54 Å), β is the full width half maximum of the

intense XRD peak and θ is the Bragg angle [27]. The average crystallite size of Bi2Te3

nanostructures is estimated as ~15±1 nm.

Figure 3 shows the Raman spectra of Bi2Te3 nanostructures and Bi2Te3-MWCNT

nanocomposite. The peak at 95 cm-1, 111 cm-1 and 135 cm-1 corresponds to single phase

Bi2Te3 due to E22g, A1u and A21g mode respectively. Bi2Te3 is centro-symmetric and therefore

A1u (classical Raman-active mode) is forbidden in the Raman spectra of Bi2Te3 bulk, however

the appearance of A1u peak at 111 cm-1 in the Raman spectra of present Bi2Te3 sample

confirms the breakdown of the centro-symmetric nature in Bi2Te3 nanostructures. Raman

spectra of the MWCNT-Bi2Te3 nanocomposite shows two peaks at 1354 cm−1 and 1582 cm−1,
which corresponds to the D and G band of MWCNT, confirming the presence of MWCNT in

the nanocomposite.

Figure 4 shows the SEM image of Bi2Te3 and Bi2Te3-MWCNT nanocomposite. The SEM

image of Bi2Te3 shows flower like morphology. The SEM image of the Bi2Te3-MWCNT

nanocomposite shows that Bi2Te3 nanoflowers morphology are decorated over the surface of

MWCNT. Figure 5 shows the TEM and high-resolution TEM images of synthesized Bi2Te3-

MWCNT nanocomposite. It can be clearly seen from TEM image that the Bi2Te3

nanostructures grow over the surface of MWCNT. The high-resolution TEM image

demonstrates a good interface between MWCNT and Bi2Te3, indicating good contacts with

Bi2Te3 and MWCNT.

The measured surface potential of Bi2Te3 and Bi2Te3-MWCNT nanocomposites using

Kelvin Probe Force Microscopy (KPFM) technique is shown in Figure 6(a) and (b). The

variation in surface potential is denoted in the surface potential map by different colours. In

addition, the presence of different charge carrier density in nanocomposite samples

corresponds to the presence of secondary phase, which are MWCNT in the present case [28,

29]. The surface potential statistical distribution of the surface potential image of the Bi2Te3

and Bi2Te3-MWCNT nanocomposites is shown in figure 6(c) and 6(d) respectively. Gaussian

fitting of the surface potential distribution showed a peak at 325 mV for Bi2Te3, whereas

Gaussian fitting for Bi2Te3-MWCNT nanocomposite showed two peaks at 390 mV and 550

mV. Peak obtained at 325 mV in Bi2Te3 nanostructure clearly indicates that there is no

secondary phase in the sample. It can be seen clearly from Figure 6(d) that Bi2Te3-MWCNT

nanocomposite shows a drastic change in surface potential due to incorporation of MWCNT

in Bi2Te3. Peaks obtained at 390 mV and 550 mV in Bi2Te3-MWCNT nanocomposite sample

are attributed to Bi2Te3 and MWCNT, respectively. A large difference between peaks (390
mV and 550 mV) in the surface potential histogram of Bi2Te3-MWCNT nanocomposite

indicates the formation of interfacial barrier height.

In order to see the effect of temperature on a figure of merit of Bi2Te3 and Bi2 Te3-

MWCNT nanocomposites, electrical, thermal conductivity and Seebeck coefficient were

measured in the temperature range of 295-340K. Figure 7 shows the temperature dependent

electrical conductivity of Bi2Te3 and Bi2Te3-MWCNT nanocomposite. The electrical

conductivity of both samples decreases monotonically with the increase of temperature,

confirming the degenerate semiconductor behaviour. In Bi2Te3-MWCNT nanocomposite,

nanostructure Bi2Te3 are decorated over the surface of MWCNT and MWCNT act as a

conducting filler between Bi2Te3 matrix, which allows for electrical network to remain intact.

At 300K, the electrical conductivity of Bi2Te3 nanoflowers material increases from ~495

S/cm to ~650 S/cm after the formation of its nanocomposite with 1wt % MWCNT. Using

Hall measurements, the carrier concentration of Bi2Te3 and Bi2Te3-MWCNT nanocomposite

at 300K is obtained as 2.431019 cm-3 and 2.781019 cm-3, respectively. The dependence of

electrical conductivity () on carrier concentration (n) and mobility (µ) is given as

  ne (3)

The value of mobility of Bi2Te3 and Bi2Te3-MWCNT nanocomposite at 300K is found as

127 cm2V-1s-1 and 149 cm2V-1s-1, respectively. The enhanced value of mobility (~17%) in

Bi2Te3-MWCNT nanocomposite is attributed to the formation of conducting channel between

Bi2Te3 nanostructures via MWCNT. Figure 8 shows temperature dependent charge carrier

mobility of Bi2Te3 and Bi2Te3-MWCNT nanocomposite which decreases with increase in the

temperature. The decrease in mobility with increase in temperature in both samples is due to

more scattering of charge carriers. The higher value of electrical conductivity of Bi2Te3

nanoflowers in the presence of MWCNT is due to the increase in the carrier concentration as

well as in carrier mobility.

 Seebeck coefficient of Bi2Te3 and Bi2Te3-MWCNT nanocomposite is shown in Figure

9. The negative value of Seebeck coefficient shows that electrons are in the majority, which

confirms n-type semiconducting nature of the samples. In addition, the increase in Seebeck

coefficient was observed in both the samples with the increase in temperature. The relation

between Seebeck coefficient and the carrier concentration is expressed by Mott formula, [30]

8 2 k 2
 
2/3

S m T  *
(4)
 3n 
2
3eh

where S is the Seebeck coefficient, n is the carrier concentration, kβ is the Boltzmann

constant, e is the charge of carrier, h is Plank’s constant and m* is the effective mass of the

charge carrier. It is expected that Seebeck coefficient will decrease with increase in carrier

concentration. We found that the carrier concentration of Bi2Te3 increases from 2.431019

cm-3 to 2.781019 cm-3 in the case of nanocomposite. Therefore, Seebeck coefficient is

expected to decrease for Bi2Te3-MWCNT nanocomposite sample. Using the carrier

concentration values and equation 4, the Seebeck coefficient of Bi2Te3 (-130 µVK-1) was

found to decrease -119 µVK-1, which is very close to the observed value of -121 µVK-1, in

the case of the nanocomposite.

Temperature dependent thermal conductivity of Bi2Te3 nanostructures and Bi2Te3-

MWCNT nanocomposite is shown in Figure 10. Similar behaviour in thermal conductivity

with the increase in the temperature is observed for both the samples. However, the thermal

conductivity is smaller in the Bi2Te3-MWCNT nanocomposite sample. The thermal

conductivity has the contribution of charge carriers (electronic thermal conductivity, electronic)

and lattice vibration (lattice thermal conductivity, lattice), which can be written as

   electronic   lattice (5)

The electronic thermal conductivity (electronic) is defined by Weidman Franz law,

 electronic  L (6)

where  is the electrical conductivity, T is the absolute temperature and L is the Lorentz

number. The value of electronic thermal conductivity is obtained using a Lorentz

number (2.4410-8 V2K‐2) in the degenerate limit [20]. The Figure 11(a) shows the variation

of electronic thermal conductivity of Bi2Te3 and Bi2Te3-MWCNT nanocomposite. The higher

value of electronic thermal conductivity in Bi2Te3-MWCNT nanocomposite is due to higher

electrical conductivity. The lattice part of thermal conductivity can be obtained using

equation (5) and from the measured value of total thermal conductivity. Figure 11(b) shows

the variation of lattice part of thermal conductivity. The lower value of lattice thermal

conductivity for Bi2Te3-MWCNT nanocomposite confirms more phonon scattering at

interfaces, which result in the reduction of total thermal conductivity of the nanocomposite.

A proposed model to explain the enhancement in electrical conductivity and decrease

in thermal conductivity in Bi2Te3-MWCNT nanocomposite is shown in Figure 12, which

describes the lattice phonon scattering at the interfaces and conduction of electrons through

the MWCNT channels. Interfaces present in the Bi2Te3-MWCNT nanocomposite between

MWCNT and Bi2Te3 nanostructures, act as a barrier for phonons resulting in enhanced

scattering at the interfaces, preventing phonons to travel longer distance and thus the resulting

reduction of lattice part of thermal conductivity. Temperature dependent figure of merit is

shown in Figure 13, which shows that in the case of Bi2Te3-MWCNT nanocomposite, the

figure of merit is increased by ~45%. This confirms that the incorporation of MWCNT in

Bi2Te3 matrix decouple the Seebeck coefficient, electrical conductivity and thermal

conductivity with the help of interfaces and improves the ZT parameter. The addition of

MWCNT in Bi2Te3 matrix gives rise to the formation of compact conductive networks, which

generates higher surface area for contact among the grains of Bi2Te3 nanoflowers and

resulted in improvement of the pathway of electrons. Therefore, the improvement in electrical

conductivity and decrease in thermal conductivity for the Bi2Te3-MWCNT nanocomposite

resulted in the enhancement of the figure of merit of Bi2Te3.

Conclusion

Bi2Te3-MWCNT nanocomposite is synthesized by hydrothermal technique. Bi2Te3-

MWCNT nanocomposite is found to exhibit higher electrical conductivity, lower value of

thermal conductivity and higher figure of merit as compared to Bi2Te3 nanostructures. The

enhanced electrical conductivity of the nanocomposite has been attributed to increase in the

carrier concentration and charge carrier mobility. The reduction in thermal conductivity of

the nanocomposite is due to the reduction in lattice part of thermal conductivity which has

been attributed to more phonon scattering at interfaces, present in the case of nanocomposite.

This work demonstrates the use of MWCNT as conducting filler, as a powerful tool to

optimize the electrical conductivity, Seebeck coefficient and thermal conductivity by

introducing interfaces in Bi2Te3-MWCNT nanocomposite.

Acknowledgments

We gratefully acknowledge the MeitY (Govt. of India) for financial support. One of us (SK)

is thankful to the University Grant Commission (UGC) for providing the senior research

fellowship.
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Figure 1 Schematic illustration of the synthesis process of Bi2Te3-MWCNT nanocomposite.

Figure 2 XRD pattern of Bi2Te3 nanostructures and Bi2Te3-MWCNT nanocomposite.

Figure 3 Raman spectra of Bi2Te3 and Bi2Te3-MWCNT nanocomposite.

Figure 4 SEM image of (a) Bi2Te3 and (b) Bi2Te3-MWCNT nanocomposite.

Figure 5 (a) TEM and (b) HRTEM images of Bi2Te3-MWCNT nanocomposite.

Figure 6 KPFM images of (a) Bi2Te3 and (b) Bi2Te3-MWCNT nanocomposite. Gaussian fit

peaks of surface potential distribution of (c) Bi2Te3 and (d) Bi2Te3-MWCNT nanocomposite.
Figure 7 Variation of electrical conductivity with temperature of Bi2Te3 and Bi2Te3-

MWCNT nanocomposite.
Figure 8 Temperature dependent charge carrier mobility of Bi2Te3 and Bi2Te3-MWCNT

nanocomposite in the temperature regime (300-340K).

Figure 9 Variation of Seebeck coefficient with temperature for Bi2Te3 and Bi2Te3-MWCNT

nanocomposite.
Figure 10 Temperature dependent thermal conductivity of Bi2Te3 and Bi2Te3-MWCNT

nanocomposite.
Figure 11 Temperature dependent (a) lattice and (b) electronic thermal conductivity of

Bi2Te3 and Bi2Te3-MWCNT nanocomposite.

Figure 12 Schematic of charge carrier conduction and phonon scattering mechanism in the

Bi2Te3-MWCNT nanocomposite.
Figure 13 Temperature dependent figure of merit for Bi2Te3 and Bi2Te3-MWCNT

nanocomposite.