Supplemental Information. A Low-Cost and High-Energy Hybrid. Iron-Aluminum Liquid Battery Achieved. by Deep Eutectic Solvents

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1 JOUL, Volume 1 Supplemental Information A Low-Cost and High-Energy Hybrid Iron-Aluminum Liquid Battery Achieved by Deep Eutectic Solvents Leyuan Zhang, Changkun Zhang, Yu Ding, Katrina Ramirez-Meyers, and Guihua Yu

2 Supplemental Information 1

3 Experimental Procedures Materials Iron (III) chloride hexahydrate (FeCl3 6H2O, 99%), aluminum chloride (AlCl3, anhydrous, 99%), urea, lithium chloride (LiCl, 99%), potassium hexacyanoferrate (III) (K3Fe(CN)6), potassium hexacyanoferrate (II) trihydrate (K4Fe(CN)6 3H2O), 1,2-dichloroethane (DCE), Li metal, titanium foil (99.7%), copper mesh and copper foil were purchased from Sigma Aldrich. Polyvinylidene fluoride (PVDF) binder and ethylene glycol (EG) was bought from Fisher Scientific. Super P carbon black was received from Timcal Graphite & Carbon. Aprotic electrolyte for anode (1 M LiPF6 in ethylene carbonate (EC)/diethyl carbonate (DEC) with volume ratio of 1:1), EC and dimethyl carbonate (DMC) were purchased from BASF. Preparation of the Fe & Al based deep eutectic solvents The Fe DESs were synthesized by mixing iron (III) chloride hexahydrate, urea and EG with various specific molar ratios in a small vial. In order to speed up the process of getting a homogeneous liquid, the mixture was stirred on a hot plate with the temperature of about 40 C in an ambient environment. After several minutes, the dark-brown eutectic liquid was formed, and was stable during long-term storage at ambient conditions. To name a series of Fe DESs, a combination of three numbers was used to represent the molar ratios of FeCl3 6H2O/urea/EG. For example, Fe(210) DES represented that the molar ratio of FeCl3 6H2O : urea : EG was 2 : 1 : 0, indicating that EG was not in the DES. Based on the literature of DESs, various Fe eutectics were obtained: 120, 121, 126, 110, 221, 210, 421, 211 and 212 Fe DESs. With different molar ratios of FeCl3 6H2O/urea/EG, the concentration of Fe DESs can be adjusted to meet different requirements. With the decrease of concentration, the color of Fe DES would change from darkbrown to light-brown and it would become transparent. For LiCl solubility in Fe DESs, Fe(126) DES can easily dissolve 4~5 M LiCl. But for Fe(210) DES, it is difficult to dissolve LiCl. Furthermore, to obtain the Fe catholyte, 0.05~0.1 ml EC/DMC was added into 1ml Fe DESs to further decrease the viscosity, which was named as Fe-DES/EC-DMC. The working of this battery doesn t require LiCl in the catholyte, although 0.3~0.5 M LiCl is still added into Fe DESs to ensure the high coulombic efficiency. The Al DES was prepared by gradually mixing urea and anhydrous AlCl3 powder together in a vial with strong agitation in the glove box. The molar ratio of AlCl3/urea was 1.3. In Al DES, the concentration of AlCl3 can reach ~ 8.4 M but the concentration of active species is 4.8 M. In order to decrease the 2

4 viscosity and improve the conductivity of the as-prepared Al DES as an anolyte, DCE was added into the Al DES with the volume ratio of 2:1 (Al-DES/DCE). After the dilution, the concentration of active ions is still as high as 3.2 M. After forming a homogeneous liquid at room temperature, 1 M LiCl was dissolved into this Al-DES/DCE to function as supporting salts. In fact, the solubility of LiCl in Al DES can reach almost 2.3 M. To avoid the influence of moisture, all the chemicals, spoons and vials involved in preparing the Al DES were dried at high temperature for a long time before use. Determination of the viscosity & conductivity of the Fe based eutectics Viscosity was tested using a rheometer (AR-2000EX, TA instrument) attached to a 25 mm parallel upper plate and a peltier bottom plate. The test required about 0.5 ml of liquid. To determine the applicable frequency, we first tested the viscosity of EG under a wide range of frequencies at 25 C since the standard values of EG s viscosity were known. As the frequency increased, the viscosity gradually decreased. Thus, the specific frequency used in here was determined by getting close to the standard value of EG at 25 C. All the tests were conducted using 10 rad s -1 frequency with the temperature range from 10 C to 40 C. The ionic conductivities of Fe DESs were measured by the electrochemical impedance spectra (EIS) using two glassy carbon electrodes. The diameter of the glassy carbon was 3 mm and the distance between the two electrodes was 6mm. Based on these two parameters and the resistance values from EIS tests, we could approximate the conductivities of Fe DESs. Cell assembly and electrochemical measurement The assembly method is similar to our previous reports. The first step is to make the cylinder cell, sealing two cylindrical quartz shells (inner/outer diameters are 8/14 mm) by sandwiching the LATP (Li1+x+3zAlx(Ti,Ge)2 xsi3zp3 zo12) separator with Surlyn resin sealant and heating at 120 C for 2 hours. Then, current collectors were prepared for the cathode and anode respectively. For the cathode current collector, a thin layer of Super P/PVDF was coated onto the surface of Ti foil, and a tiny hole was drilled for injecting the catholyte. 90 wt% Super P carbon and 10 wt% PVDF were mixed in NMP solvent, and to remove the solvent, the current collector was dried in a vacuum at 100 C for 12 hours. For the Li anode s current collector, copper mesh was welded to copper foil, and Li metal was pressed onto the copper mesh in a glove box. In the Fe-Al hybrid battery, an Al strip was directly attached to copper foil as anode. 3

5 Next, the cathode current collector and previous cylinder cell were bonded together using sealant. Lastly, we added electrolytes to both the anode and cathode sides before testing. Either commercial A6 electrolyte or Al-DES/DCE were injected into the quartz shell of the anode part and then covered by the copper foil in the glovebox and sealed hermetically using epoxy. In the cathode, Fe-DES/EC-DMC was injected into the cylindrical quartz shell through the hole drilled in the Ti foil in advance and the hole was then immediately covered by Kapton tape. In order to balance the concentration difference between charge carriers (Li + ) of Al anolyte and redox species (Fe 3+ ) of Fe catholyte, the volume of Al-DES/DCE is determined by the volume & concentration of Fe-DES/EC-DMC. To mitigate the influence of high viscosity and reduce the testing time, 50 μl Fe(126)- DES/EC-DMC & 30 μl Fe(210)-DES/EC-DMC are usually used as catholytes. Therefore, the volume of Al anolyte is decided to be 170~190 μl Al-DES/DCE for Fe(210) catholyte. And for Fe(126) catholyte, the volume of Al-DES/DCE is usually 100~120 μl. All electrochemical measurements were conducted on a BioLogic VMP3 potentiostat system or Autolab (PGSTAT302N) electrochemical workstation at room temperature. For the Li anode, the cut-off potential was set between 2.9 V and 4 V. The cut-off potential for Fe-Al hybrid battery was set between 0.8 V and 2.2 V. The capacity and energy density were calculated based on the volume of Fe catholyte. A three electrode system was used to determine the CV curves of Fe DESs and Al-DES/DCE. For Fe DESs, the three electrodes were glassy carbon electrode (WE), Ag/AgCl electrode (RE) and Pt wire (CE), respectively. For the Al-DES/DCE, the glassy carbon electrode was the working electrode while both the reference and counter electrodes were Al metal. For CV tests of Fe DESs, 2M LiCl was added into the liquid as supporting salts. To improve the power density, the semi-flow device was used to test the polarization curve of Fe(126)-Al & Fe(210)-Al battery, in which the carbon felt was used as current collector and a pump was used to supply the Fe catholytes through the cathode compartment at a flow rate of ~41.5 ml min -1. Characterizations The surface morphology of Al anode before and after test were observed by Scanning Electron Microscopy (SEM) (S5500, Hitachi) operating at SEM mode. The XRD patterns of Al anode before and after test were characterized by X-ray diffractometer (XRD) (Rigaku MiniFlex 600) using Cu Kα radiation 4

6 (λ = Å). To understand the coordination environment of Fe 3+ in the FeCl3 6H2O-urea-EG eutectic system, the Raman spectra of Fe DESs, urea/eg, FeCl3 6H2O and FeCl2 4H2O were recorded by a Micro-Raman Spectrometer (Witec, Alpha 300) under 488nm. Furthermore, the Raman spectra of discharged and charged Fe(126) & Fe(210) catholytes were characterized to understand the redox reactions of Fe DESs. 5

7 Figure S1. Photo of Fe(210) DES and Fe(126) DES after staying at ambient environment for eight months. Synthesized at ambient environment, Fe DESs also exhibit good stability during long-term storage in air. We find that the liquid of Fe DES can keep clear and transparent for a long time, indicating its stability at ambient environment. For example, after storing in air for eight months, the physical sate of Fe(126) DES still remains stable. 6

8 Figure S2. CV curves of (a) 121, (b) 126, (c) 221, (d) 210, (e) 421, (f) 211, and (g) 212 Fe DESs at different sweeping rates with 2 M LiCl as supporting salts; (h) CV curves of various 210 based Fe DESs with 2 M LiCl at the scan rate of 1 mv s -1. 7

9 Table S1. Data analysis of CV curves of various Fe DESs at 1 mv s -1. Fe DESs Concentration Cathodic peak / V Anodic peak / V (Ea + Ec) / 2 Ipa / Ipc M M M M M 5.5M 5.1M 4.9M 4.2M

10 Figure S3. Viscosity of (a) various 120 & 110 based Fe DESs and (b) different 210 based Fe DESs as a function of temperature and composition. 9

11 Figure S4. CV curves of EG & EC/DMC at the sweeping rate of 10 mv s

12 Figure S5. The charging and discharging curves of Fe(126)-Li battery during cycling. 11

13 Figure S6. (a) CV curves of Al-DES/DCE liquid at various sweeping rate; (b) XRD patterns of Al-metal anode before (black) and after (red) electrochemical test; SEM images of Al-metal anode (c) before and (d) after electrochemical test. 12

14 Figure S7. (a) The first charge and discharge curves of Fe(210)-Li battery at 0.1 ma cm -2 ; (b) the polarization profile of Fe(210)-Li battery at room temperature. 13

15 Figure S8. (a) The initial charge and discharge profile of Fe(210) catholyte paired with Al-DES/DCE at the current density of 0.2 ma cm -2 ; (b) Electrochemical impedance spectroscopy of the Fe(210)-Al battery at room temperature; (c) The full charging and discharging of Fe(210)-Al battery over time; (d) Polarization graph presenting the discharging potential and power density at room temperature. 14

16 Figure S9. The calculation of energy density for hybrid Fe(210)-Al batteries. Using the discharging curve presented in Fig. 5a, the integrated area under this curve is calculated to be Wh L -1, which is the energy density of the Fe(210)-Al battery based on the volume of Fe(210) catholyte. 15

17 Figure S10. (a) Photograph of the semi-flow battery device using Al-DES/DCE as anolyte and Fe(126)- DES/EC-DMC as catholyte; I-V polarization curve of the semi-flow Fe-Al battery using Al-DES/DCE as anolyte and (b) Fe(126)-DES/EC-DMC or (c) Fe(210)-DES/EC-DMC as catholyte. Using flowable electrode we tested the polarization curve of Fe(126)-Al & Fe(210)-Al battery using Al- DES/DCE as anolyte and Fe-DES/EC-DMC as catholyte. The carbon felt was used as current collector to improve the current collection efficiency and thus the power density was much higher than the static device but it was still not comparable to the aqueous flow battery technologies. In addition to the intrinsic high viscosity of Fe DES, the flow device also increased the thickness of glass shell in the cathode side which would weaken the effect of carbon felt. 16

18 Figure S11. (a) The Raman spectra of urea, EG and their mixtures; (b) The Raman spectra of FeCl3 6H2O & FeCl2 4H2O solids. We also observed the Raman spectra of the solid salts of FeCl3 6H2O and FeCl2 4H2O (Fig. S11). Their peak positions were quite different: FeCl2 4H2O had two major peaks at around 187 and 3415 cm -1 ; And FeCl3 6H2O solid had several peaks in the range of 100 to 700 cm -1 and didn t show the feature peak of [FeCl4] -. 17

19 Figure S12. Chemical titration of (a) original, (b) discharged and (c) charged Fe(210) & Fe(126) catholytes using K3Fe(CN)6 or K4Fe(CN)6 aqueous solutions (from left to right, they are K3Fe(CN)6, K4Fe(CN)6, K3Fe(CN)6, K3Fe(CN)6, K4Fe(CN)6 and K4Fe(CN)6); (d) Photos of discharged and charged Fe(210) & Fe(126) catholytes. Utilizing the [Fe(CN)6] 3+ or [Fe(CN)6] 4+, we found only Fe 3+ existed in the beginning (Fig. S12a). During discharging, Fe 3+ was reduced to be Fe 2+ but a little Fe 3+ was still detected in the Fe catholytes after discharging, as shown in Fig. S12b. However, after full charging, only Fe 3+ was detected (Fig. S12c), indicating a reversible reaction in Fe DESs. Fig. S12d showed photos of Fe(126) and Fe(210) catholytes after discharging and charging. The black thing on the quartz shell was Super P carbon which was used as current collector during battery assembly. During charging/discharging, Fe(126) catholyte remained in liquid form, while the Fe(210) catholyte was solidified during discharging and the precipitate would melt during charging, which might have a negative influence on the electrochemical performance. The deep eutectic point will change with the variation of composition ratios. During the charging and discharging process, the reduction and oxidation of Fe 3+ might change the molar ratio of FeCl3/urea but we found the liquid form of Fe(126) DES was maintained during the charging and discharging. Besides, Al DES also kept the liquid state during electrochemical test. It was our opinion that additives (EG or DCE) could decrease the deep eutectic point, making it much lower than room temperature. Thus, even if the change of deep eutectic points occurred in the charging and discharging process, the liquid form of 18

20 Fe(126) or Al DESs could be maintained. Therefore, we believe that it does not influence the electrochemical performance of Fe(126)-Al battery. For Fe(210) DES, we observed the solid formation during discharging. Except for the precipitation of [FeCl2(OD)4], another possible reason was the change of deep eutectic points. 19

21 Figure S13. The potential profile of Fe(213) catholyte paired with Li at the current density of 0.1 ma cm -2. Dissociating the complex cations and anions in Fe(210) DES by EG, Fe(213) DES was obtained, which had a high concentration of 3.8 M. To further decrease the viscosity of Fe(213) DES, 0.05 ml EC/DMC was added into 1 ml Fe(213) DES to make the final Fe(213) catholyte (Fe(213)-DES/EC-DMC). Roughly, Fe(213) catholyte had a concentration of 3.6 M. Paired with Li anode, Fe(213) catholyte showed a high capacity of ~90 Ah L -1 with a low polarization in voltage. Initially, it had the potential to achieve a stable cycling under full charge/discharge. 20

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