A Quasi-Solid-State Solar Rechargeable Battery with Polyethylene

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A Quasi-Solid-State Solar Rechargeable Battery with Polyethylene Oxide Gel Electrolyte Bao Lei, Guoran Li, Peng Chen, and Xue-Ping Gao ACS Appl. Energy Mater., Just Accepted Manuscript • DOI: 10.1021/acsaem.8b02193 • Publication Date (Web): 25 Jan 2019 Downloaded from http://pubs.acs.org on January 27, 2019

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ACS Applied Energy Materials

A Quasi-Solid-State Solar Rechargeable Battery with Polyethylene Oxide Gel Electrolyte Bao Lei, Guo-Ran Li, Peng Chen, Xue-Ping Gao* Institute of New Energy Material Chemistry, School of Materials Science and Engineering, Nankai University, Tianjin 300350, China. * E-mail: [email protected]. Tel/Fax: +86-22-23500876. Abstract

A quasi-solid-state solar rechargeable battery with polyethylene oxide gel electrolyte as cathode and anode electrolyte is proposed in this work.In the fabricated battery, solar energy can be converted and stored as chemical energyunder light irradiation,which is further to electrical energyin the dark as well. In the meantime, the working stability of the battery is improvedby introducing the gel electrolyte into the battery system.

Key words: solar rechargeable battery; solar energy conversion; energy storage; quasi-solid-state; gel electrolyte

1. Introduction In the past decades, energy crisis and environment pollution become a global problems, accompanied with the excessive usage of fossil sources.1-3 Thus, seeking for

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renewable and green source is absolutely necessary for the future sustainable energy requirement. Solar energy, naturally clean, green and abundant, is the potential alternative for the energy pursuit.4 As important energy conversion devices, solar cells can realize solar to electrical energy conversion directly.5-7 From conventional Si-based solar cells to new generation perovskite solar cells, the great progress in solar cells make it possible for commercial usage of solar source.8-10Whereas, an intrinsic drawback of the unstable output of solar irradiation brings a discontinuous solar to electrical energy conversion. Moreover, solar cells only achieve the solar energy conversion for direct use, without storage capability of electrical energy. For highly efficient utilization of solar energy, an extra backup energy storage system is necessary to integrate into solar cells for storing the electrical energy, such as secondary batteries. Therefore, developing a solar rechargeable battery achieving solar energy conversion-storage, and further comprehensive utilization attracts extensive interest. Generally, a typical solar rechargeable battery is fabricated by combining photo-anode with secondary batteries together. In the battery, solar energy is converted and stored as chemical energy during the photo-charging process, and further to electric energy in the subsequent discharging profiles.11-16.For dye-sensitized TiO2 photo-anode based solar rechargeable battery system, cathode active material is soluble I3-/I-couple in organic solvent. Energy storage anode on the secondary battery side is mainly focused on oxidation-reduction

reactions

in

battery,17-19ion

flow

insertion/extraction

or

doping/de-doping reactions,20-27 and hydrogen adsorption/oxidation reactions in liquid electrolyte.28. It means that liquid-phase electrolyte is essential to soluble energy storage electrode materials and diffusion of ions in the as reported solar storable battery

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mentioned above. However, the stability of such battery system based on liquid electrolyte is unsatisfactory, due to the loss of active materials originated from the leakage in long-term photo-charging and discharging processes. Recently, the gel electrolyte based on polyethylene oxide (PEO) can be successfully used in quasi-solid-state dye-sensitized solar cells (DSSCs) and lithium-ion batteries,29-34 respectively. Therefore, gel electrolyte based on PEO would be a potential choice for assembling a quasi-solid-state solar rechargeable battery and improving the working stability of the battery system. Herein, a quasi-solid-state solar rechargeable battery is prepared by introducing a polyethylene oxide (PEO) gel electrolyte into the battery system with soluble LiI as cathode material, 9,10-anthraquinone (AQ) as anode, and Nafion 117 membrane as the separator. The proposed battery system could be a potential solution to realize in situ solar energy conversion and storage as chemical energy, and further conversion of chemical energy to electrical energy.

2. Results and discussion The configuration and working principle of the designed quasi-solid-stated solar rechargeable battery with PEO gel electrolyte are shown inFig.1. The detailed forming scheme of the PEO gel electrolyte is shown in Fig. 1b. PEO is a thermoplastic polymer with good solubility in water and organic solvent. When the dried PEO polymer is added into organic electrolyte with lithium salt, polymer network is swelled accordingly to form gel

electrolyte.35During

this

process,

Li-ions

3

are


dispersed

uniformly

in

the


quasi-solid-state electrolyte, leading to a cross-link in the network as a transparent gel (Fig. S1). The swollen gel electrolyte holds liquid solvent in the network and prevents leakage of the fabricated cell. In general, the working principle in a typical solar rechargeable battery can be expressed as following two processes: photo-charging process under light irradiation and constant-current discharging process in the dark. In the initial photo-charging process, the dye-sensitized TiO2photo-anode and AQ anode are closed in the circuit by connecting B and C through a single-pole double throw switch. Under the condition of light irradiation, a pair of electron-hole is produced immediately on N719 dye molecules. The photo-generated electrons are jumped to excited state, and injected on the conduction band of TiO2 rapidly, then passed onto AQ through external circuit finally. With strong reducibility, AQ can be reduced to AQ- by the receiving the photo-generated electrons. Meanwhile, Li-ions are diffused from cathode side to anode side through the Nafion separator to counterbalance the negative charge of AQ-. At the same time, iodide ions (I-) can be oxidized to triiodide ions (I3-) by holes on dye in the gel electrolyte, accompanied with releasing Li-ions. Therefore, solar energy is transformed to chemical energy, which is stored as a fully-charged state of I3- and AQ- in cathode and anode, respectively. Usually, in a typical dye-sensitized solar cell, counter electrode receives the photo-generated electrons for reducing the I3- to I- in the electrolyte. In a secondary battery, anode receives/stores electrons from external circuit originated with cathode in the charge process. As to the solar recharge battery, in the photo-charge process, AQ electrode receives the photo-generated electrons as counter electrode on the DSSC side. On the other hand, AQ is also reduced by the photo-generated electrons for storing the chemical energy, which is regarded as anode on the side of secondary battery. Here, as

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bi-functional electrode, AQ is considered not only as a counter electrode on the DSSC side for receiving the photo-generated electrons, but also as anode on the side of secondary battery for storing the chemical energy converted from solar energy.

Fig.1. (a) Configuration and electron transfer scheme of the designed quasi-solid-state solar rechargeable battery with PEO gel electrolyte. (b) From dried PEO polymer network in organic solvent, the schematic of the quasi-solid-state cathode and anode gel electrolyte, respectively. The reactions in the photo-charge process are expressed as follows: ℎ𝑣

𝐷𝑦𝑒 + 𝑇𝑖𝑂2 𝐷𝑦𝑒 + + 𝑇𝑖𝑂2(𝑒 ― )(1) 2𝐷𝑦𝑒 + +3𝐼 ― →2𝐷𝑦𝑒 + 𝐼3―

(2)

𝐴𝑄 + 𝑥𝐿𝑖 + + 𝑥𝑒 - →𝐿𝑖𝑥(𝐴𝑄)(3) After the photo-charge process, the electrochemical constant current discharge process can be conducted in the dark. Here, I3-/I- cathode and AQ/AQ- anode are closed

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by connecting A and C, while the TiO2 photo-anode (B) is turned off in the circuit. Specifically, AQ- anode is electrochemically oxidized to AQ with discharging electrons, which flow to the cathode side via external circuit and to support the reduction reactionofI3- to I-. Meanwhile, for counterbalancing the negative charge, lithium ions are forced to diffuse from anode side to cathode side. With converting back to the initial state of I- and AQ, the discharging process is completely finished. It means that the chemical energy, generated initially by solar energy in photo-charge process, is subsequently transferred into electrical energy through constant current discharging process. The related reactions in the discharge process could be described as following: 𝐼3- + 2𝑒 -

𝑑𝑖𝑠𝑐h𝑎𝑟𝑔𝑒

3𝐼 - (4)

𝑑𝑖𝑠h𝑎𝑟𝑔𝑒

𝐿𝑖𝑥(𝐴𝑄)

𝐴𝑄 + 𝑥𝐿𝑖 + + 𝑥𝑒 - (5)

In the photo-charge process, AQ is reduced to AQ-, accompanied with the transfer of C=O and C=C double bonds in structure. In the presence of lithium, the transfer kinetics become slow with the formation of an insoluble lithium salt. The reaction mechanism of the AQ unit in the photo-charge process and discharge process can be expressed as following:36, 37

Cyclic voltammogram (CV) measurements are operated to identify the working mechanism of the as-prepared quasi-solid-state battery, and the corresponding CV results of N719 dye, LiI and AQ are shown in Fig. 2.For the LiI cathode, two pairs of redox

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potential peaks, located at -0.05/-0.33 V and 0.29/0.16 V (vs. Ag/Ag+),are related to the two-step electrochemical redox processes.38-40 The oxidation potential of N719is 0.7 V (vs. Ag/Ag+),much higher than two pairs of redox peaks of I-/I3-, indicating a complete oxidization reaction of I- to I3- by holes on dye molecules in the photo-charging process under light irradiation, as presented in Eq. 2.In the case of AQ electrode, a pair of redox potential is observed at -0.07/0.22 V (vs. Ag/Ag+). While, the conductive band edge of TiO2is -0.68 V (vs. Ag/Ag+) in aprotic solvent, which is negative than the reduction peak of AQ (-0.07 V, vs. Ag/Ag+). It implies that the photo-generated electrons can be fluently passed to AQ from the sensitized TiO2throughthe external circuit during the photo-charging process. As a result, AQ anode is reduced to AQ- by the photo-generated electrons, as shown in Eq. 3. According to the analysis above, AQ/AQ- couple is considered as anode, when matched with I-/I3- cathode in the battery. Therefore, according to the analysis of potentials and energy level of cathode, anode, N719 dye and TiO2 conductive band, the working mechanism of the as-fabricated quasi-solid-state solar rechargeable battery is feasible.

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Fig.2. CVs of LiI cathode and AQanode in 7.5 wt. % PEO gel electrolyte(50 mV s-1) Ion conductivity ( S cm-1) is an important factor of the PEO-based gel electrolyte for evaluating the quasi-solid-state battery system, which can be calculated through electrochemical impedance spectra (EIS). Usually, the  value is obtained from the following equation:41

 = L/RS(6) Herein, R(Ω) is regarded as the bulk resistance of intercept of the Nyquist plots with real axis. L (cm) is considered as the thickness of the gel electrolyte, and related to the distance between two FTO conductive glass electrodes. S (cm2) is the area of the gel electrolyte.42, 43As shown in Fig. 3a, Nyquist plots of the gel electrolytes are consisted of single sloped lines with the frequency range used in the measurement. The calculated  values of the gel electrolyte with different PEO amounts are shown in Fig. 3b. Clearly, the value is enhanced slowly with increasing amount of PEO first, and then reduced sharply when the PEO amount is increased further for the gel electrolytes. When the PEO

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content is 7.5 %, the gel electrolyte with an optimized  value of 3.88 ×10-4 S cm-1 is obtained. Correspondingly, as displayed in Fig. 3c, the discharge capacities are highly related to the ion conductivity for the quasi-solid-state battery with different PEO gel electrolytes. In particular, the battery with 7.5 wt. % PEO gel electrolyte shows a large discharge capacity after initial activation, in which the ion conductivity is higher. Therefore, the gel electrolyte with 7.5 wt. % PEO is chosen as the optimized condition for the further investigation of the quasi-solid-state solar rechargeable battery.

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Fig. 3. (a) Nyquist plots of the symmetric cells using different amount of PEO gel electrolyte with two identical FTO conductive glasses as electrodes. (b) The calculated ion conductivity from impedance data with different PEO amounts in gel electrolyte. (c) Cycling stability of the battery with different PEO amounts. In theory, the photo-charged voltage of a typical battery in the photo-charging process depends on the open-circuit voltage (Voc)provided by DSSC, which is corresponding to the potential difference between conductive band edge ofTiO2and potential of I-/I3-redox couple. However, the polarization caused by the ion diffusion from the Nafion membrane to cathode and anode active-materials is not to be ignored in the quasi-solid-state battery system. Therefore, the working voltage of the quasi-solid-state battery is lower than the value of Voc due to the electrochemical and concentration polarizations from both cathode and anode sides. For this circumstance, the voltage of the quasi-solid-state battery in photo-charging process is slightly less than 0.76 V.

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Fig. 4. (a) Voltage profiles of the batteries with liquid electrolyte and PEO-based gel electrolyte (photo-charging for 10 min under light irradiation and discharging at 4 mA g-1).(b) Cycle stability of the batteries with liquid electrolyte and PEO-based gel electrolyte. The battery performance is further investigated by photo-charging for 10 min under light irradiation first, and then discharging at 4 mA g-1.As illustrated in Fig. 4a,the battery voltage with PEO gel electrolyte jumps rapidly to 0.65 V under irradiation, and then gradually climbs to 0.74 V, demonstrating a feasible energy conversion and storage as the existence of fully charged state(I3- and AQ-) from the initial state (I- and AQ), respectively. On the contrary, the battery voltage with liquid electrolyte approaches quickly to 0.75 V, indicating a faster diffusion of lithium ions and active materials in liquid electrolyte than the gel electrolyte. Compared to the charging process in the conventional lithium-ion batteries with galvanostatic technique, the current of the solar rechargeable battery drops dramatically from the maximum value under light irratiation.28Actually, the battery presents a constant-voltage characteristic in the photo-charging process.

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When AQ-/AQ and I-/I3- couples are connected in the discharging process, the battery shows a gradient discharge curve, corresponding to the potential difference between AQ-/AQ and I-/I3- couples. It means that the chemical energy stored in the photo-charging process is transferred into electrical energy via electrochemical redox reactions on cathode and anode active materials from photo-charged state (I3- and AQ-)back to the original state (I- and AQ). In comparison with liquid electrolyte, the slow activation process is needed for the battery with PEO gel electrolyte. The typical discharge curves in initial 3 cycles are provided as Fig. S2 in supporting information. As presented in Fig. 4b, the discharge capacity is 0.9 mAh g-1 of the battery with PEO gel electrolyte in the first cycle. After 3 cycles, the discharge capacity increases dramatically up to 6.6mAh g-1, and then increases gradually to 8 mAh g-1 after 9 cycles. Correspondingly, the sloped discharge voltage plateau is widened gradually with increasing the cycle number. Meanwhile, accompanied with fast activation process, the discharge capacity of the battery with liquid electrolyte is much higher. However, the working stability of the battery with liquid electrolyte is relatively poor, with low capacity retention of 52.0 % after 19 cycles. While, the high capacity retention of 86.3 %is obtained for the battery with PEO gel electrolyte after 30 cycles on the same condition. It implies that the cycle stability of the as-prepared quasi-solid-state battery is successfully improved by introducing PEO gel electrolyte into the system. As a solar driven system, the battery performance is also controlled by the photo-charge time. To further show the impact of the irradiation time, the battery is carried out with different photo-charge time under constant irradiation (100 mWcm-2). As presented in Fig. S3,after photo-charged for 20 min, the initial discharge capacity of the

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battery is slightly larger than that photo-charged for 10 min. After 5 cycles, the battery also retains a larger discharge capacity with photo-charged for 20 min, indicating a direct correlation between the solar irradiation and the photo-generated I-/I3- and AQ-/AQ active species couples. In the photo-charge and discharge process, the oxidation-reduction reactions occur initially on the surface between solid AQ anode and gel electrode, and then to the interior of AQ anode. In Nyquist plots with the whole frequency range of dummy cells (Fig. S4), there are one arc and a straight line for the battery system. With increasing the cycle number, the arc is decreased gradually, indicating the improved charge-transfer process and slow activation. In general, the overall energy conversion efficiency (OECE) of the battery is related to the photo conversion efficiency (PCE), electrical-to-chemical conversion efficiency (EC) of the DSSC under irradiation, and chemical-to-electrical conversion efficiency (CE) by the electrochemical way in the dark.28 As indicated in Fig. S5, the DSSC with AQ counter electrode presents the photo conversion efficiency (PCE) of 4.28%, slightly lower than that (6.78%) of the DSSC with Pt electrode. For the quasi-solid state battery, the overall energy conversion efficiency (OECE) is increased gradually due to the slow activation process. In particular, the OECE value of the battery is still less than 0.3 % at the present level. Another intrinsic problem is that the open circuit voltage of the battery is lower, which is limited by DSSC. The main purpose in this work is to explore the working feasibility of the quasi-solid state solar rechargeable battery, more efforts should be taken in our next research, including the improvement of the overall energy conversion efficiency and discharge capacity.

Conclusion 13



In summary, a quasi-solid state solar rechargeable battery with PEO gel electrolyte is successfully fabricated. Specifically, photo-generated electrons are passed to anode via external circuit for reducing AQ to AQ-. Meanwhile, I- is oxidized to I3- by holes on N719 dye molecules. Under light irradiation, the battery achieves an energy conversion and storage of solar energy as chemical (I3- and AQ-)in cathode and anode, respectively. Under dark condition, the battery completes a further energy transformation from the stored chemical energy to electric energy in the subsequent constant-current discharge process. Moreover, the as-proposed solar rechargeable battery presents good working stability by introducing PEO gel electrolyte into the battery system. This work offers not only a perspective of the feasible energy conversion, storage, and utilization based on new battery system from solar energy, but also an efficient potential solution to enhancing the cycling stability of the solar rechargeable battery.

Supporting Information Experimental details, photo of the gel electrolyte, the performance of the solar rechargeable battery with different photo-charging times.

Acknowledgments Financial Supports fromthe 973 Program (2015CB251100) and National Natural Science Foundation (21875123) of China are gratefully acknowledged.

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A Quasi-Solid-State Solar Rechargeable Battery with Polyethylene

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