Electrochemical response of n-type bismuth telluride based thermoelectric materials in NaCl solutions: A comparison between a single-phase alloy and a nanocomposite containing MoS2 nano-particles

Mohsen K. Keshavarz; Arash Fattah-alhosseini

doi:10.1016/j.arabjc.2018.01.021

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Original article

13 (

); 1858-1865

doi:

10.1016/j.arabjc.2018.01.021

Electrochemical response of n-type bismuth telluride based thermoelectric materials in NaCl solutions: A comparison between a single-phase alloy and a nanocomposite containing MoS₂ nano-particles

Mohsen K. Keshavarz^{^a}, Arash Fattah-alhosseini^{^b,⁎}

a Department of Mining & Materials Engineering, McGill University, Montreal, Quebec (QC) H3A 0C5, Canada

b Department of Materials Engineering, Bu-Ali Sina University, Hamedan 65178-38695, Iran

⁎Corresponding author. a.fattah@basu.ac.ir (Arash Fattah-alhosseini)

Received: 2017-11-1, Accepted: 2018-1-30, Published: 2018-01-01

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

This work presents a systematic assessment of electrochemical responses of n-type bismuth telluride-based thermoelectric materials in NaCl solutions. A single-phase alloy and a nanocomposite (with embedded MoS₂ nanoparticles) produced by means of mechanical alloying and hot extrusion were investigated. The polarization and electrochemical impedance spectroscopy tests in NaCl solutions revealed that the passivity of the nanocomposite specimen was considerably improved compared with the coarse-grained single-phase alloy. Mott–Schottky analysis revealed that passive layers of both single-phase alloy and nanocomposite specimens had an n-type semiconducting behavior, and the donor density reduced in the passive layer of the nanocomposite specimen.

Keywords

Thermoelectrics

Nanocomposite

Bismuth telluride

Corrosion

Electrochemical impedance spectroscopy (EIS)

Mott–Schottky (M–S) analysis

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1 Introduction

Thermoelectric (TE) materials, are basically semiconductors, that can convert heat to electricity and vice versa. These materials are mostly used in the niche applications either as generator or refrigerator (Goldsmid, 2010; Goldsmid and Delves, 1961; Goldsmid, 1960 ). Bismuth telluride-based alloys are among the well-known thermoelectric (TE) materials due to their high performance around the room temperature. During the last six decades, there have been enormous efforts to improve the efficiency of different families of TE materials to boost their applications. In this regard, within the last decade, researchers have obtained achievements by nanostructuring or developing nanocomposite (NC) TE materials, especially in bismuth telluride based alloys (Poudel et al., 2008; Liu et al., 2012; Keshavarz et al., 2013, 2014 ). While study and improvement of TE properties of these materials have received huge interests, some of their key properties when these materials are in service, such as mechanical and corrosion properties, have not received sufficient consideration. Bismuth telluride based TE materials have been synthesized and fabricated via electrochemical routes (Tittes et al., 2003; Tittes and Plieth, 2007; Yoo et al., 2005 ), however, there is a very limited number of works in the open literature on the electrochemical and corrosion behaviors of bismuth telluride based alloys (Zimmer et al., 2008; Rosalbino et al., 2013). In the present work, we compared the electrochemical behaviors of an n-type single-phase bismuth telluride based quaternary alloy with a NC counterpart consisted of the primary single-phase alloy (SPA) as its matrix, embedded with MoS₂ nano-particles. The comprehensive studies on other properties of these materials, including their TE properties can be found in Keshavarz et al. (2014) and Keshavarz Khorasgani (2014)).

Our systematic study includes evaluation of the electrochemical responses of n-type SPA and NC bismuth telluride based TE materials in 0.58 wt% (0.1 M) and 3.5 wt% NaCl solutions, and Mott–Schottky (M–S) analysis.

2 Experimental procedures

2.1

2.1 Samples processing

Nanostructured powders of n-type (Bi_0.95Sb_0.05)₂(Te_0.95Se_0.05)₃ alloy was prepared from high purity (99.999%) shots of Bi, Sb, Se, and Te (5N Plus) by mechanical alloying using an attritor. The MoS₂ nano-particles (99.99% purity, MKnano) were added (0.3 wt%) to the alloyed powder and mixed for 1 h to obtain the NC powder mixture. The SPA powder, as well as NC powder mixture, was consolidated using the hot extrusion method at around 680 K. The products were in form of circular cross-section rods with 1-inch (2.54 cm) diameter and lengths about 1 foot (30.5 cm). A detailed description of the synthesis procedure can be found in Keshavarz et al. (2014).

2.2

2.2 Microstructural characterization

Chemical composition of the SPA and NC specimens were assessed by X-ray diffraction (XRD) using a Philips X’Pert apparatus equipped with a copper anode. High resolution scanning electron microscopy (SEM) was implemented with a JEOL JSM-7600 TFE instrument to evaluate the microstructure of the specimens. The nano-scale structural and elemental composition analyses were carried out using a JEOL JEM-2100F high-resolution transmission electron microscope (HRTEM) including an energy dispersive X-ray spectrometry (EDS).

2.3

2.3 Electrochemical tests

The surfaces of both SPA and NC specimens were polished and cleaned prior to the electrochemical tests. The tests were run in naturally aerated 0.1 M and 3.5 wt% NaCl solutions at 25 ± 1 °C in a three-electrode flat cell (with SPA and NC specimens as working electrodes, a Pt plate as counter electrode, and Ag/AgCl saturated in KCl reference electrode) by using a µAutolab Type III/FRA2 system. The electrochemical measurements, in both NaCl solutions, were performed after 1 h immersion of the working electrodes at open circuit potential (OCP). To obtain potentiodynamic polarization (PDP) curves scans with a rate of 1 mV s⁻¹ were made starting from −0.25 V (vs. E_corr) to 0.9 V_Ag/AgCl. To carry out the electrochemical impedance spectroscopy (EIS) tests, excitation potential (peak to peak) of 10 mV and scanning frequencies between 0.01 Hz and 100 kHz were selected. It is important to note that the EIS tests were done at OCP condition. To fit the curves and model the data, NOVA 2.1.0 software was used. Lastly, M–S analysis was performed using a 10 mV AC signal in the cathodic direction with 1 kHz frequency and potential step of 25 mV.

3 Results and discussions

3.1

3.1 Microstructural analysis

The phase composition of bulk SPA and NC specimens were characterized by XRD Fig. 1). The patterns of both SPA and NC specimens were well fitted with the reference pattern of (Bi_0.95Sb_0.05)₂(Te_0.95Se_0.05)₃ phase. This certifies that there was no chemical reaction between matrix phase and MoS₂ nanoparticles during mixing and/or hot extrusion processes. In addition, variation in the peaks intensities can be observed in the NC pattern compared to that of the SPA. This can be attributed to alteration of crystallographic texture in the specimens. Bismuth telluride has an anisotropic crystal structure (Goldsmid, 2010). Consequently, a crystallographic texture will be established in the bulk bismuth telluride due to the extrusion process (Vasilevskiy et al., 2002). However, addition of MoS₂ nanoparticles led to modification in the texture of NC specimens to some extent. Similar observation has been reported for extruded p-type bismuth telluride based NCs with embedded MoS₂ nanoparticles (Keshavarz et al., 2016).

XRD patterns of extruded n-type SPA and NC specimens compared with the reference pattern of (Bi0.95Sb0.05)2(Te0.95Se0.05)3 phase.

Fig. 2 shows fracture surfaces of n-type SPA and NC specimens. A clear grain size reduction due to MoS₂ nanoparticles addition in the NC specimen is illustrated. This result confirms that introducing MoS₂ nanoparticles to the n-type SPA inhibits the matrix grain growth during hot extrusion. Nanoparticles of MoS₂ pin the grain boundaries and impede further grain boundaries migration when the material is exposed to high temperature. This phenomenon is known as Zener pinning (Nes et al., 1985).

Fracture surfaces of (a) SPA, and (b) NC specimens.

HRTEM observations indicated that MoS₂ nanoparticles with few nanometers length and thickness of few atomic layers are dispersed at the grain boundaries within the matrix Fig. 3). EDS patterns of areas containing nanoparticles (e.g. indicated in Fig. 3 (a)) exhibited the presence of Mo and S in the nanoparticles Fig. 3 (b)). The intense Cu peaks in the EDS pattern is originated from the Cu grid in the HRTEM specimen holder.

(a) HRTEM image of a MoS2 nanoparticle at the matrix grains’ boundaries in an extruded nanocomposite, (b) EDS pattern of marked area in panel (a).

3.2

3.2 PDP measurements

Fig. 4 depicts the Pourbaix diagram for Bi-Te system at 25 °C (Martin-Gonzalez et al., 2002). Based on this diagram, Bi₂Te₃ demonstrates a passive behavior in a limited potential range for pHs from 3 to 7.5. Hence, to investigate the electrochemical properties of the passive layer, the two 0.58 wt% (0.1 M) and 3.5 wt% NaCl solutions with a pH of 7.2 were selected.

Pourbaix diagram for Bi-Te at 25 °C (Martin-Gonzalez et al., 2002).

According to the Porbaix diagram, for the potentials higher than -1 (V), the behavior of Bi₂Te₃ compound in these two solutions can be described in four regions:

In the potentials from −1 to +0.2 (V); the compound is in immunity region and no corrosion products will be formed on the surface.
In potentials from +0.2 to +0.6 (V); bismuth and tellurium oxides (Bi₂O₃ and TeO₂) will form on the surface that will play a protective role.
In potentials from +0.6 to +1 (V); TeO₂ will turn to hydrogentellurate (HO₄Te⁻), but Bi₂O₃ will continue its protective performance.
Eventually, in the fourth region (potentials higher than +1 (V)), Bi₂O₃ will be electrolyzed and Bi₂O₅ forms.

The stability of the formed passive layer on bismuth telluride depends on the microstructure of the material and the chemical composition of corrosive solution. To study these parameters, PDP tests were carried out and their results are presented in this section

PDP curves of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions are illustrated in Fig. 5. It showed that both SPA and NC specimens are spontaneously passivated in both NaCl solutions. Also, the PDP plots showed that the passivity of the NC specimen was considerably enhanced in both NaCl solutions compared to that of coarse-grained SPA. Considering the passivation process, it can be noted from Fig. 5 that the value of passive current density for NC specimen is lower than that of SPA specimen, which means that the passive film covered on the surface of NC specimen showed higher protective characteristics.

PDP curves of extruded n-type SPA and NC specimens in (a) 0.1 M and (b) 3.5 wt% NaCl solutions.

Fig. 6 depicts the changes in the corrosion potential and corrosion current density of both extruded n-type SPA and NC specimens in NaCl solutions. The Tafel extrapolation was used to obtain the corrosion current density. In this regard, the linear part for the cathodic branch back to the corrosion potential was studied (Burstein, 2005). Fig. 6(a) reveales that the corrosion current density of the NC specimen was significantly decreased compared with the coarse-grained SPA in NaCl solutions. Moreover, Fig. 6(b) shows that the corrosion potential of the NC specimen was increased compared to that of SPA in both NaCl solutions. In other words, the NC specimen showed a more noble value of the corrosion potential compared to the SPA specimen. This suggests that the NC specimen possesses lower active dissolution ability. Fig. 6 clearly shows that corrosion resistance of the NC specimen in the 0.1 M NaCl solution was significantly higher than that of the SPA specimen. However, in the solution with higher corrosivity (i.e. 3.5 wt% NaCl) while the corrosion resistance was improved in the NC specimen, but, the enhancement is much less pronounced compared to the observed improvement in the 0.1 M NaCl solution. Indeed, these results revealed that n-type bismuth telluride NC specimen showed more suitable performance, in terms of corrosion resistance in NaCl solutions in comparison to the conventional SPA.

(a) Corrosion current density, and (b) corrosion potential of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions.

3.3

3.3 EIS measurements

The Nyquist and Bode plots of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions are illustrated in Fig. 7. All the Nyquist and Bode plots have similar profiles. The Nyquist plots show imperfect semicircles. Moreover, the Bode plots depict that at high frequencies specimens had resistive response, but a noticeable capacitive behavior in the middle to low frequency range was observed. Also, in the intermediate frequencies, the Bode-phase plots showed a constant phase performance.

EIS plots for extruded n-type SPA and NC specimens in (a, b) 0.1 M and (c, d) 3.5 wt% NaCl solutions.

As the concentration of NaCl decreased, the low frequency impedance in both SPA and NC specimens increased, and the phase angle improved in the intermediate frequencies. This variation is an indication of a protective passive film formation and growth. Also, for both NaCl solutions, the low frequency impedance significantly increased in NC specimen. In conclusion, the n-type NC bismuth telluride-based specimen offers better passive film formation conditions with improved protective behavior. This can be attributed to the finer microstructure of NC specimens, since smaller grains lead to higher number of potential nucleation sites for passive film.

Based on the impedance plots shown in Fig. 7, one time constant can be employed to obtain EIS spectra or the SPA and NC specimens. Therefore, the equivalent electrical circuit (EEC) shown in Fig. 8 is proposed to model the impedance spectra. The circuit elements in this EEC are: R_s, R_p and Q_p, which represent solution resistance, resistance of the passive film, constant phase element (CPE) corresponding to the capacitance of the passive film, respectively (Grubac and Metikos-Hukovic, 2004). The CPE, Q_p, depends on Y₀ and n (in Eq. (1)), which can be obtained during the fitting process (Hirschorn et al., 2010):

(1)

Q_{P} = Y_{0} {(j ω)}^{n}

Proposed EEC to simulate the experimental EIS data (Grubac and Metikos-Hukovic, 2004).

Also, Eqs. (2) and (3) were used to calculate impedance of the constant phase element and the capacitance, C, respectively (Vafaeian et al., 2016; Fattah-alhosseini and Imantalab, 2016):

(2)

Z_{CPE} = {[Q {(j ω)}^{n}]}^{- 1}

(3)

C = Y_{0} {(ω_{max})}^{n - 1}

where ω stands for the angular frequency (rad s⁻¹), j is the imaginary number, Y₀ shows the admittance (Ω⁻¹ cm⁻² s⁻¹), and ω_max represents the angular frequency at which the peak occurs in the imaginary element of the impedance, and n is the Q exponent that varies between 0.5 and 1 as following:

Q provides an ideal capacitor, if n = 1;
Q gives a wide range of dielectric relaxation times, if 0.5 < n < 1;
Q presents a Warburg impedance with diffusion character, if n = 0.5.

The alteration in the capacitance and resistance of the passive films formed on the both extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions are illustrated in Fig. 9. The passive film resistance of the NC specimen was significantly increased compared with coarse-grained SPA in both NaCl solutions Fig. 9(a)). Also, Fig. 9(b) illustrates that the passive film capacitance of the NC specimen was decreased compared to that of SPA. This reduction in the capacitance of the passive film suggests lower dissolution and enhanced passivity of the NC specimen (Fattah-alhosseini and Imantalab, 2015).

(a) Polarization resistance and (b) double layer capacitance of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions.

3.4

3.4 M–S analysis

A comparison between the passive films formed on the extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions were evaluated by determining the capacitance (C) at semiconductor/solution interface, then, M–S curves (1/C² vs. E) were plotted to assess the passive layer donor density (N_D) and flat band potential (E_FB) by using Eq. (4) (Tittes and Plieth, 2007; Zimmer et al., 2008):

(4)

\frac{1}{C^{2}} = \frac{2}{ε ε_{o} {eN}_{D}} (E - E_{fb} - \frac{k_{B} T}{e})

where

ε

denotes the passive film dielectric constant (218 for Bi₂Te₃ (Zimmer et al., 2008),

ε_{0}

shows the vacuum permittivity (8.854 × 10⁻¹⁴ F/cm), k, e, and T stand for the Boltzmann constant, the electron charge, and absolute temperature, respectively. The M–S plots of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions are shown in Fig. 10. The capacitance of the NC specimen was decreased compared to that of SPA in both NaCl solutions. In Fig. 10, all plots have a region in which E and C⁻² are linearly related. In this region, the positive slope is an indication of the negative conduction type (n-type) in the passive layer. Similar M–S plots are observed for a different composition of bismuth telluride (Zimmer et al., 2008). The donor density was calculated using Eq. (5):

(5)

N_{D} = \frac{2}{ε ε_{o} e} {[\frac{d (1 / C^{2})}{dE}]}^{- 1}

M–S plots of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions.

In the passive layer, donation of electrons by the cation interstitials and/or oxygen vacancies results in domination of negatively charged particles contribution in the conduction (i.e. n-type conduction) (Macdonald, 2011; Fattah-alhosseini, 2016). Fig. 11 shows the calculated donor density (N_D) and flat band potential (E_FB) of both SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions. The calculated value of N_D of the NC specimen was significantly decreased compared with the conventional SPA in both NaCl solutions Fig. 11(a)). The calculated donor densities (∼10²⁰ cm⁻³) are comparable to those of previously reported values for bismuth telluride-based materials (Yoo et al., 2005; Zimmer et al., 2008). To obtain the flat band potential, the linear part of the M–S plots (1/C² vs. E) was extrapolated to the abscissa. As shown in Fig. 11(b), the flat band potential value of the NC specimen was significantly increased compared with the coarse-grained SPA. The high donor density of the passive layers is an indication of a considerable number of point defects such as cation interstitials and/or oxygen vacancies in the films. Reviewing all the results of the electrochemical analyses revealed that NC specimen showed more suitable corrosion resistance performance compared to that of the conventional SPA.

(a) Calculated donor density and (b) flat band potential of extruded n-type SPA and NC specimens in 0.1 M and 3.5 wt% NaCl solutions.

Bismuth telluride based TE materials can be used as both generators around room temperature or thermoelectric cooling devices (known as Peltier coolers). TE devices are made of TE modules, which in turn contain legs made of n- and p-type materials. When TE devices, as solid-state devices, are expected to possess long service life, the failure of any leg in a module will lead to failure of the whole module. Consequently, besides high efficiency of the TE device, high quality when in service and high reliability of the TE device depends also on the endurance of the materials used in the modules, both mechanically and chemically. NCs of bismuth telluride with embedded MoS₂ nanoparticles have shown superior mechanical performance compared to the SPA (Keshavarz et al., 2016). The results of this study showed that n-type NC of bismuth telluride has greater corrosion resistance, especially in an atmospheric environment, than that of SPA material. Using the proposed NC material can lead to high performance TE modules with higher reliability and longer service life.

4 Conclusions

In this work, the electrochemical responses of extruded n-type single-phase alloy (SPA) and nanocomposite (NC) (containing MoS₂ nanoparticles) specimens in 0.1 M and 3.5 wt% NaCl solutions was evaluated. The following particular conclusions can be drawn from the obtained results:

The microstructure is significantly refined in the nanocomposite specimen.
Potentiodynamic polarization and EIS analyses exhibited that the passive behavior of the NC specimen was considerably enhanced compared with the coarse-grained SPA in both NaCl solutions.
Mott–Schottky analysis indicated that both SPA and NC specimens behaved as n-type semiconductors in NaCl solutions. Additionally, the donor density decreased in the NC specimen.
Overall, n-type bismuth telluride NC thermoelectric specimen demonstrated more suitable performance, in terms of corrosion behavior, compared to that of the conventional SPA.

Acknowledgment

The synthesis of the specimens presented in this work, were carried out at the thermoelectric research lab. of Polytechnique Montreal, managed by Prof. S. Turenne. All the electrochemical tests and analysis were performed at Dr. A. Fattah-alhosseini’s research lab, at Bu-Ali Sina University. The financial support of the Iran National Science Foundation (INSF) (No. 96002434) is gratefully acknowledged.

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Introduction

Experimental procedures

Samples processing
Microstructural characterization
Electrochemical tests

Results and discussions

Microstructural analysis
PDP measurements
EIS measurements
M–S analysis

Conclusions

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[1] Burstein G.T., . A hundred years of Tafel's equation: 1905–2005 - Preface. Corros. Sci.. 2005;47:2858-2870.
[Google Scholar]

[2] Fattah-alhosseini A., . Passivity of AISI 321 stainless steel in 0.5 M H₂SO₄ solution studied by Mott-Schottky analysis in conjunction with the Point Defect Model. Arab. J. Chem.. 2016;9:S1342-S1348.
[Google Scholar]

[3] Fattah-alhosseini A., Imantalab O., . Effect of accumulative roll bonding process on the electrochemical behavior of pure copper. J. Alloy Compd.. 2015;632:48-52.
[Google Scholar]

[4] Fattah-alhosseini A., Imantalab O., . Passivation behavior of ultra-fine grained pure copper fabricated by accumulative roll bonding (ARB) process. Metall. Mater. Trans. A. 2016;47:572-580.
[Google Scholar]

[5] Goldsmid H.J., . Applications of Thermoelectricity. Methuen, London, New York: Wiley; 1960.

[6] Goldsmid H.J., . Introduction to Thermoelectricity. New York: Springer, Heidelberg; 2010.

[7] Goldsmid H.J., Delves R.T., . Materials for thermoelectric refrigeration. GEC J.. 1961;28:102-105.
[Google Scholar]

[8] Grubac Z., Metikos-Hukovic M., . EIS study of solid-state transformations in the passivation process of bismuth in sulfide solution. J. Electroanal. Chem.. 2004;565:85-94.
[Google Scholar]

[9] Hirschorn B., Orazem M.E., Tribollet B., Vivier V., Frateur I., Musiani M., . Determination of effective capacitance and film thickness from constant-phase-element parameters. Electrochim. Acta. 2010;55:6218-6227.
[Google Scholar]

[10] Keshavarz Khorasgani M., . Synthesis and Characterization of Bismuth Telluride-Based Nanostructured Thermoelectric Composite Materials, Ecole polytechnique de Montréal. Université de Montréal; 2014. p. :126.

[11] Keshavarz M.K., Vasilevskiy D., Masut R.A., Turenne S., . p-Type bismuth telluride-based composite thermoelectric materials produced by mechanical alloying and hot extrusion. J. Electron Mater.. 2013;42:1429-1435.
[Google Scholar]

[12] Keshavarz M.K., Vasilevskiy D., Masut R.A., Turenne S., . Synthesis and characterization of bismuth telluride-based thermoelectric nanocomposites containing MoS₂ nano-inclusions. Mater. Characteriz.. 2014;95:44-49.
[Google Scholar]

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