Te/C nanocomposites for Li-Te Secondary Batteries

Seo, Jeong-Uk; Seong, Gun-Kyu; Park, Cheol-Min

doi:10.1038/srep07969

Te/C nanocomposites for Li-Te Secondary Batteries

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Published: 22 January 2015

Volume 5, article number 7969, (2015)
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Te/C nanocomposites for Li-Te Secondary Batteries

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Jeong-Uk Seo¹^na1,
Gun-Kyu Seong¹^na1 &
Cheol-Min Park^1,2^na1

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Abstract

New battery systems having high energy density are actively being researched in order to satisfy the rapidly develo** market for longer-lasting mobile electronics and hybrid electric vehicles. Here, we report a new Li-Te secondary battery system with a redox potential of ~1.7 V (vs. Li⁺/Li) adapted on a Li metal anode and an advanced Te/C nanocomposite cathode. Using a simple concept of transforming TeO₂ into nanocrystalline Te by mechanical reduction, we designed an advanced, mechanically reduced Te/C nanocomposite electrode material with high energy density (initial discharge/charge: 1088/740 mA h cm⁻³), excellent cyclability (ca. 705 mA h cm⁻³ over 100 cycles) and fast rate capability (ca. 550 mA h cm⁻³ at 5C rate). The mechanically reduced Te/C nanocomposite electrodes were found to be suitable for use as either the cathode in Li-Te secondary batteries or a high-potential anode in rechargeable Li-ion batteries. We firmly believe that the mechanically reduced Te/C nanocomposite constitutes a breakthrough for the realization and mass production of excellent energy storage systems.

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Introduction

Rechargeable Li-ion batteries are representative energy storage systems owing to their high operating voltage and relatively high energy density^1,2,3,4,5,6. However, to satisfy the rapidly develo** market for longer-lasting mobile electronic devices and hybrid electric vehicles (HEVs), much work has been devoted to finding new energy storage systems with higher energy densities than Li-ion batteries^{7,8,9,10,11,12,13}. Among various rechargeable battery systems, rechargeable Li-sulfur (S) batteries have been proposed as an alternative system for Li-ion secondary batteries because of their high theoretical energy density of 1675 mA h g⁻¹ or 3467 mA h cm⁻³ and appropriate redox potential of ~2.15 V (vs. Li⁺/Li) by the reaction of S₈ + 16Li ↔ 8Li₂S^{14,15,16,17,18,19,20,21,22,23,24,25,26,27,28,Full size image}

TeO₂→Te (nanocrystalline) + O₂ ↑; by HEMM

The mechanical reduction of TeO₂ may be related to the high pressure on the order of 6 GPa and temperature above 200°C generated during HEMM. Upon consideration of the simple mechanical reduction of TeO₂, we used this mechanical reduction method to produce a Te/C nanocomposite and we subsequently synthesized MR-Te/C nanocomposites. The XRD pattern of the MR-Te/C nanocomposite is shown in Figure 3b. All of the XRD peaks corresponded to Te peaks (JCPDS #36-1452) and no other phases were detected. The TEM bright-field image, the HRTEM images combined with FT patterns and the STEM image with energy dispersive spectroscopy (EDS) map** of the MR-Te/C nanocomposite show that Te nanocrystallites with sizes of approximately 5–10 nm were well dispersed within the amorphous carbon matrix (Figure 3c). Thus, it can be concluded that the MR-Te/C nanocomposite particles are composed of well-dispersed nanosized (5–10 nm) Te crystallites within the amorphous carbon matrix, as schematically illustrated in Figure 3d.

Electrochemical performances of mechanically reduced Te/C nanocomposite

To evaluate the MR-Te/C nanocomposite as a cathode material for a new Li-Te secondary battery system, the electrochemical properties of the nanocomposite were tested and the results are shown in Figure 4 and S3. The voltage profiles of the Te and MR-Te/C nanocomposite electrodes are shown in Figure 4a (potential vs. volumetric capacity) and S3a (potential vs. gravimetric capacity), respectively. The MR-Te/C nanocomposite electrode showed a discharge potential of 1.7 V (vs. Li⁺/Li) and the first discharge and charge capacities were 1088 and 740 mA h cm⁻³ (459 and 312 mA h g⁻¹), respectively, at a current density of 10 mA g⁻¹. The nanocomposite showed an excellent capacity retention of 97.4% of the initial charge capacity after the 10th cycle. However, the voltage profile of the MR-Te/C nanocomposite electrode showed a slight slope compared with those of Te electrode, which was caused by the results of the cooperated electrochemical reactions between nanocrystalline Te and ball-milled amorphous carbon and subreaction between the electrolyte and electrode surface as mentioned above. In Figure S4, the voltage profile of the ball-milled amorphous carbon electrode showed the first discharge and charge capacities of 162 and 87 mA h cm⁻³ (193 and 103 mA h g⁻¹), respectively, on the condition of the potential range between 1.0 and 3.0 V and current density of 10 mA g⁻¹. The high discharge and charge capacities of the ball-milled carbon were attributed to the degree of disordered structure and morphology and Li diffusion into the inner cores of the fractured carbons^37,38,39. The first charge capacity of the ball-milled carbon (34.9 wt%) contributed in the MR-Te/C nanocomposite electrode was approximately 30 mA h cm⁻³ or 36 mA h g⁻¹. Considering the theoretical capacity of 65.1 wt% Te (273 mA h g⁻¹) and the capacity of 34.9 wt% ball-milled carbon (36 mA h g⁻¹) contributed in the MR-Te/C nanocomposite, Te in the composite electrode was fully reversible with Li, whereas the high initial discharge capacity of MR-Te/C nanocomposite was also correlated with the ball-milled carbon (corresponding to 67 mA h g⁻¹) and the subreaction between the electrolyte and electrode surface.

The MR-Te/C nanocomposite electrode showed much better electrochemical performance than the Te and Te/C nanocomposite electrodes. Comparisons of the cycling performance were made for the Te, Te/C and MR-Te/C nanocomposite electrodes in the potential range between 1.0 and 3.0 V. The gravimetric and volumetric capacities of the Te and Te/C nanocomposite electrodes, as shown in Figure 4b and S3b, decreased gradually after a few cycles. The reversible capacity and capacity retention of the MR-Te/C nanocomposite electrode was significantly enhanced as compared to the Te and Te/C nanocomposite electrodes. The MR-Te/C nanocomposite electrode showed a very stable capacities of more than 704 mA h cm⁻³ or 297 mA h g⁻¹ (current density: 10 mA g⁻¹) and 597 mA h cm⁻³ or 252 mA h g⁻¹ (current density: 100 mA g⁻¹) over 100 cycles, corresponding to ca. 95% and 96% of the initial charge capacities, respectively. Additionally, the average Coulombic efficiency per cycle of the MR-Te/C nanocomposite electrode is above 99.5%. The size of the Te crystallites of the MR-Te/C nanocomposite electrode after various cycling was also analyzed using HRTEM. The HRTEM results of the samples obtained after the 10th and 50th cycles are shown in Figure S5a and b, respectively. The HRTEM images combined with FT patterns reveal the presence of the Te phase, whose crystallite size is approximately 5–10 nm after the 10th cycle and the Te crystallites still remained 5–10 nm in size upon further cycling, even after 50 cycles. These results show that the Te nanocrystallites within the MR-Te/C nanocomposite do not agglomerate during cycling. The excellent cycling behaviour of the MR-Te/C nanocomposite electrode was attributed to the uniform distribution of 5–10-nm-sized Te crystallites within the amorphous carbon buffering matrix, which alleviated the effect of the volume expansion on the active materials, as illustrated in Figure 3d. On the basis of the results, the MR-Te/C nanocomposite can provide a new cathode material for Li-Te secondary batteries owing to its reduction potential of 1.7 V (vs. Li⁺/Li) and excellent cycling behavior.

The rate capability test of the MR-Te/C nanocomposite electrode was also conducted in the potential range between 1.0 and 3.0 V. The results are shown in Figure 4c (potential vs. volumetric capacity) and 4d (volumetric capacity vs. cycle number) and in Figure S3c (potential vs. gravimetric capacity) and S3d (gravimetric capacity vs. cycle number). The figures show the cyclability of the MR-Te/C nanocomposite electrode as a function of the C rate, where C is defined as the full use of the restricted charge capacity of 700 mA h cm⁻³ in 1 h. At rates of 2C and 5C, the MR-Te/C nanocomposite electrode showed very high charge capacities of 590 and 550 mA h cm⁻³, respectively, corresponding to ca. 79% and 75% of the charge capacity for the rate at 0.1C with stable cycling behavior. The rate capability of the MR-Te/C nanocomposite electrode was excellent, with a higher capacity than that of commercially available Li₄Ti₅O₁₂ anodes for Li-ion batteries. The fast rate capability of the MR-Te/C nanocomposite electrode is ascribed to the presence of the ca. 5–10-nm-sized mechanically reduced nanocrystalline Te within the amorphous carbon matrix, which contributed to short Li diffusion paths. Additionally, the better electrical conductivity of Te than S and Se contributed to the fast rate capability. Considering the excellent rate capability and high volumetric capacity with a reduction potential of ca. 1.7 V (vs. Li⁺/Li) of the MR-Te/C nanocomposite electrode, it can be utilized as either the cathode in Li-Te secondary batteries or a high-potential anode in rechargeable Li-ion batteries.

Discussion

By introducing a new materials pair into a secondary battery system, we have successfully developed a stable Li-Te secondary battery system with excellent electrochemical performances. Specifically, we adopted a Li metal anode and a MR-Te/C nanocomposite cathode, which are stable materials, achieving a redox potential of ~1.7 V (vs. Li⁺/Li). Using a simple and interesting concept of transforming TeO₂ into nanocrystalline Te by mechanical reduction, the MR-Te/C nanocomposite was synthesized and applied as a high-performance cathode in Li-Te secondary batteries. Additionally, the MR-Te/C nanocomposite can be utilized as a high-potential anode in rechargeable Li-ion batteries. The advantageous features of the MR-Te/C nanocomposite are as follows. First, when the MR-Te/C nanocomposite was applied as a cathode material in a new Li-Te secondary battery, it showed a relatively high redox potential of ~1.7 V (vs. Li⁺/Li), high energy density (initial discharge/charge: 1088/740 mA h cm⁻³), excellent cyclability (ca. 705 mA h cm⁻³ over 100 cycles) and fast rate capability (ca. 550 mA h cm⁻³ at 5C rate). Second, because the MR-Te/C nanocomposite electrode showed a better rate capability and higher energy density than commercially available Li₄Ti₅O₁₂ anodes, the MR-Te/C nanocomposite can be used as a high-potential anode for rechargeable Li-ion batteries. Third, as demonstrated on the basis of the DCP and ex situ XRD results, the one-step electrochemical reaction mechanism of the Te electrode with Li provides a stable battery system unlike rechargeable Li-S battery forming various soluble Li-polysulfides generated during the discharge/charge process in various electrolytes.

In summary, we have developed a simple mechanical reduction method of transforming TeO₂ into nanocrystalline Te using a high-energy mechanical milling technique at ambient temperature and pressure. Further modification with carbon produced a MR-Te/C nanocomposite that, when applied as a cathode material for a new Li-Te rechargeable batteries, showed excellent cycling performance with high volumetric capacities. Additionally, the MR-Te/C nanocomposite electrode showed excellent rate capabilities with high volumetric capacities, which proves that it is very applicable to high potential anodes with Li₄Ti₅O₁₂. We anticipate that the MR-Te/C nanocomposite will pave the way for the realization and mass production of excellent energy storage systems.

Methods

Sample Preparation

Te/C nanocomposite was prepared using Te (Aldrich, 99.98%, average size ca. 50 μm) and carbon (Super P, Timcal) powders. The powders were prepared by HEMM (Spex-8000) at ambient temperature and pressure as follows: the powders were placed into an 80 cm³ hardened steel vial with stainless steel balls (diameter: 3/8 in. and 3/16 in.) at a ball-to-powder ratio of 20:1. The HEMM process was carried out under an Ar atmosphere for 6 h. Preliminary studies showed that the optimum composition was 70 wt% Te to 30 wt% carbon. Mechanically reduced Te was synthesized by the same HEMM technique using a TeO₂ powder (Aldrich, >99%, average size ca. 20 μm). To synthesize the mechanically reduced Te/C nanocomposite, the same HEMM technique was employed to mill mixtures of the TeO₂ and carbon powders. Preliminary electrochemical tests revealed that, in terms of the electrochemical performance such as initial capacity, initial coulombic efficiency and cycle performance, the optimum amounts were 70 wt% TeO₂ and 30 wt% C, which correspond to the exact composition of 65.1 wt% Te and 34.9 wt% C within the mechanically reduced Te/C nanocomposite.

Materials Characterization

To observe the structural changes in the active material of the Te electrode during cycling, ex situ XRD (DMAX2500-PC, Rigaku) analyses were used. The Te/C and mechanically reduced Te/C nanocomposites were characterized using XRD, HRTEM (FEI F20, operating at 200 kV) and EDS (attached to the HRTEM).

Electrochemical Measurements

For the electrochemical evaluation of Te, Te/C and mechanically reduced Te/C nanocomposites, test electrodes consisting of the active powder (70 wt%), carbon black (Denka, 15 wt%) as a conducting agent and polyvinylidene fluoride (PVDF, 15 wt%) dissolved in N-methyl-2-pyrrolidone (NMP) as a binder were fabricated. Samples of each mixture were vacuum-dried at 120°C for 3 h and pressed (electrode thickness: ca. 0.045 mm, electrode area: 0.79 cm², weight of active material: ca. 2.5 mg). Coin-type electrochemical cells were assembled in an Ar-filled glove box using a Celgard 2400 separator, Li foil as the counter and reference electrodes and 1 M LiPF₆ in ethylene carbonate/diethyl carbonate (EC/DEC, 1:1 by volume, Panax STARLYTE) as the electrolyte. All the cells were tested galvanostatically between 1.0 and 3.0 V (vs. Li⁺/Li) at current densities of 10 and 100 mA g⁻¹ using a Maccor automated tester except the rate capability tests. The gravimetric capacity was calculated on the basis of the weight of the active materials and the volumetric capacity was calculated by multiplying the gravimetric capacity by the tap density (Te: 3.93 g cm⁻³, Te/C: 2.45 g cm⁻³, mechanically reduced Te/C: 2.37 g cm⁻³, Li₄Ti₅O₁₂: 1.11 g cm⁻³, ball-milled amorphous carbon: 0.84 g cm⁻³), which was measured using a powder tap density tester (BT-301, Bettersize). Li was inserted into the electrode during the discharge reaction and was extracted from the working electrode during the charge reaction.

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Acknowledgements

This research was supported by the MSIP (Ministry of Science, ICT and Future Planning), Korea, under the “Creative ICT Convergence Human Resource Development” support program (NIPA-2014-H7501-14-1002) supervised by NIPA (National IT Industry Promotion Agency).

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Seo Jeong-Uk and Seong Gun-Kyu contributed equally to this work.

Authors and Affiliations

School of Materials Science and Engineering, Kumoh National Institute of Technology, Gumi, Gyeongbuk, 730-701, Republic of Korea
Jeong-Uk Seo, Gun-Kyu Seong & Cheol-Min Park
Outstanding Research Group Program, Convergence Technology Research Institute, Kumoh National Institute of Technology, Gumi, Gyeongbuk, 730-701, Republic of Korea
Cheol-Min Park

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Jeong-Uk Seo
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C.-M.P. initiated the idea and outlined the experiments. J.-U.S. and G.-K.S. synthesized samples and performed various analyses. C.-M.P. supervised the research work and wrote the manuscript. All authors contributed to discussion on the results for the manuscript.

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Seo, JU., Seong, GK. & Park, CM. Te/C nanocomposites for Li-Te Secondary Batteries. Sci Rep 5, 7969 (2015). https://doi.org/10.1038/srep07969

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Received: 15 September 2014
Accepted: 02 December 2014
Published: 22 January 2015
DOI: https://doi.org/10.1038/srep07969
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Introduction

Electrochemical performances of mechanically reduced Te/C nanocomposite

Discussion

Methods

Sample Preparation

Materials Characterization

Electrochemical Measurements

References

Acknowledgements

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Contributions

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Te/C nanocomposites for Li-Te Secondary Batteries

Abstract

Similar content being viewed by others

Introduction

Electrochemical performances of mechanically reduced Te/C nanocomposite

Discussion

Methods

Sample Preparation

Materials Characterization

Electrochemical Measurements

References

Acknowledgements

Author information

Authors and Affiliations

Contributions

Ethics declarations

Competing interests

Electronic supplementary material

Rights and permissions

About this article

Cite this article

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