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Article

Helium Dielectric Barrier Discharge Plasma Jet (DBD Jet)-Processed Graphite Foil as Current Collector for Paper-Based Fluidic Aluminum-Air Batteries

by
Chung-Yueh Shih
1,2,
I-Chih Ni
3,
Chih-Lin Chan
1,2,
Cheng-Che Hsu
4,
Chih-I Wu
3,5,
I-Chun Cheng
3,5,6 and
Jian-Zhang Chen
1,2,6,7,*
1
Graduate Institute of Applied Mechanics, National Taiwan University, Taipei City 10617, Taiwan
2
Advanced Research Center for Green Materials Science and Technology, National Taiwan University, Taipei City 10617, Taiwan
3
Graduate Institute of Photonics and Optoelectronics, National Taiwan University, Taipei City 10617, Taiwan
4
Department of Chemical Engineering, National Taiwan University, Taipei City 10617, Taiwan
5
Department of Electrical Engineering, National Taiwan University, Taipei City 10617, Taiwan
6
Innovative Photonics Advanced Research Center (i-PARC), National Taiwan University, Taipei City 10617, Taiwan
7
Graduate School of Advanced Technology, National Taiwan University, Taipei City 10617, Taiwan
*
Author to whom correspondence should be addressed.
Energies 2022, 15(16), 5914; https://doi.org/10.3390/en15165914
Submission received: 19 July 2022 / Revised: 5 August 2022 / Accepted: 11 August 2022 / Published: 15 August 2022
(This article belongs to the Section L: Energy Sources)
Browse Figures
Versions Notes

Abstract

:
A helium (He) dielectric barrier discharge plasma jet (DBD jet) was used for the first time for treating graphite foil as the current collector of a paper-based fluidic aluminum-air battery. The main purpose was to improve the distribution of the catalyst layer through modification and functionalization of the graphite foil surface. The plasma functionalized the graphite foil surface to enhance the wettability where the more hydroxyl could be observed from XPS results. The 30 s-He DBD jet treatment on the graphite foil significantly improved the battery performance. The best current density of 85.6 mA/cm2 and power density of 40.98 mW/cm2 were achieved. The energy density was also improved to 720 Wh/kg.

Graphical Abstract

1. Introduction

Metal-air batteries have played a vital role in the field of energy storage devices due to their low cost and high energy density. Refs. [1,2] Paper-based aluminum-air (Al-air) batteries have attracted much attention in recent years [3,4,5,6,7,8,9,10,11,12] because they are inexpensive and ecofriendly, and possess high energy density. Aluminum, which is abundant in Earth’s crust, is used as the anode in Al-air batteries [13]. During battery discharge, anodic passivation and self-corrosion reaction reduce the electrochemical performance of Al-air batteries [14,15]. Thus, studies have adjusted the components or morphology of aluminum, for example, by using a different state of the electrolyte or optimizing the battery structure, to improve the aluminum reaction during battery discharge. Wang et al. used a gel electrolyte to produce a flexible liquid-free paper-based Al-air battery with high specific capacity [16]. In 2019, Shen et al. designed a micro-fluidic paper-based Al-air battery with high energy density, in which the electrolyte flows along the paper channel by capillary force [17].
Atmospheric pressure plasma (APP) has some advantages compared to the low-pressure plasma. It can be operated at regular pressure without using vacuum system; therefore, it is of low cost and easy to set up. There are some common methods to generate low-temperature APP, such as corona discharge, atmospheric pressure plasma jet (APPJ) and dielectric barrier discharge (DBD). DBD is a non-equilibrium plasma which is commonly used for functionalization, etching or deposition in APP application [18,19,20,21,22]. DBD can avoid arc discharge which has high current density [23,24]. With high speed jet flow, the APPJ could produce a uniform reaction species and homogeneous discharge [25,26]. In this study, we used the dielectric barrier discharge jet (DBD jet) which combines DBD and APPJ to ensure a stable and homogeneous plasma treatment process.
Our research group has long investigated different plasma device for fabrication of batteries [27,28,29,30,31,32,33,34]. A He-DBD jet has been applied for the fabrication of perovskite solar cells (PSCs) and supercapacitor because of its low processing temperature [31,32,33,34,35]. Additionally, most of the papers about Al-air batteries use metal/carbon and catalyst to form their cathode without being pre-modified, which can be seen from the Table S2 in our Supplementary Information. In this study, a He DBD jet was used for treating graphite foil as the current collector of a paper-based fluidic Al-air battery to improve the distribution of the catalyst layer by functionalization of graphite foil surface. As a result, the battery performance was greatly improved. The plasma parameters of the DBD jet were based on our previous research [31,32,33,34,35]. The electrochemical performances of the fluidic paper-based Al-air batteries were investigated with different plasma treatment times on the graphite foil.

2. Materials and Methods

2.1. He DBD Jet

Figure 1 shows the schematic of the He DBD jet in this study. The inner and outer diameters of the quartz tube were 8 mm and 10 mm, respectively. There were two annular copper electrodes fixed outside the quartz tube. The gap between the two electrodes was 10 mm. One was a ground electrode. The other was a power electrode connected to the high AC voltage with a frequency of 20 kHz and a peak voltage of 10 kV. Due to the high frequency and high voltage, the plasma was emerged between the electrodes inside the tube and was carried down with a He jet flow of 3 slm to treat the sample surface.

2.2. Materials

Graphite foil (thickness: 0.5 mm) was purchased from FAR EAST CARBON Co., Ltd., New Taipei City, Taiwan. Palladium 10% on carbon (type 487, Pd/C) was purchased from Alfar Aesar, Ward Hill, MA, USA. Moreover, 5 wt% Nafion solution and potassium hydroxide (KOH, purity: 85%) were purchased from Sigma-Aldrich, St. Louis, MO, USA. Aluminum foil (thickness: 0.05 mm, purity: 99%) was purchased from GoodFellow, Huntingdon, UK. Filter paper (grade 4, thickness: 0.205 mm, pore size: 20–25 μm) was purchased from Whatman, Maidstone, UK.

2.3. Fabrication of the Al-Air Battery

Figure 2 shows a flowchart of the Al-air battery fabrication process. The cathode electrode is made of a catalyst layer and a current collector. The graphite foil (8 mm × 25 mm) was used as a current collector. First, the graphite foil was sequentially cleaned using ethanol (purity: 95%) and deionized (DI) water via ultrasonication for 15 min. Then, it was placed in an oven at 70 °C and dried for 15 min. Second, one end of the graphite foil (8 mm × 5 mm) was treated with the He DBD jet for 30 s, 1 min, and 3 min. The distance between the end of the DBD jet and the graphite foil surface was fixed at 5 mm. Third, 24 μL of the catalyst ink prepared by ultrasonicating Pd/C in DI water (20 mg/mL) was carefully applied on the DBD jet-processed end of the graphite foil (8 mm × 5 mm) by drop casting. The catalyst-coated graphite foil was left to stand at room temperature for at least 45 min until the catalyst layer dried. Next, 4 μL of Nafion solution was dropped on the air-dried catalyst layer to prevent the catalyst from detaching from the graphite foil. Then, the cathode was left to stand at room temperature for another 30 min. The aluminum foil (8 mm × 25 mm) was used as the anode. The Al-air battery is sandwich-structured. A piece of filter paper (80 mm × 10 mm) was set between the anode and cathode as the electrolyte channel. The electrodes were fixed on a polymethylmethacrylate (PMMA) substrate (60 mm × 40 mm) by tape, as shown in Figure S1. The PMMA substrate was cleaned by the same process as that used for the graphite foil. The active areas of the electrodes were controlled at 8 mm × 5 mm. During the discharge of the Al-air battery, rectangular absorbent filter paper pads (40 mm × 30 mm) were placed on one end of the filter paper channel. The other end was immersed in the electrolyte (1.5 M KOH). Thus, the electrolyte flowed along the paper channel by capillary force.

2.4. Characterization

The surface images of the graphite foil were inspected using scanning electron microscope (SEM, JSM-7800F Prime, JEOL, Tokyo, Japan). X-ray photoelectron spectroscopy (XPS) analysis was performed using an X-ray photoemission spectrometer (5000 Versa Probe, ULVAC PHI, Kanagawa, Japan). The water contact angle was measured using a goniometer (100SB, Sindatek, Taipei City, Taiwan). The electrochemical performance was evaluated by linear sweep voltammetry (LSV), battery discharge test and electrochemical impedance spectroscopy (EIS) using an electrochemical workstation (Autolab PGSTAT204, Metrohm, Utrecht, the Netherlands). In LSV measurement, the current was measured from the open circuit voltage (OCV) to 0 V with a scan rate of 5 mV/s. Then, the current density and power density were calculated. In battery discharge test, the voltage was measured every 0.1 s with certain current of 0.008 A (20 mA/cm2). The total mass of Al (0.015 g) was used to calculate the capacity of the batteries. The energy density also was calculated by the capacity and the voltage.

3. Results

3.1. SEM Analysis

Figure 3 shows SEM images of the graphite foil without and with the He DBD jet plasma treatment. We took pictures at a microscopic level to observe the severity of the surface crack on the graphite foil. After cleaning and drying of the graphite foil, a few surface cracks and uneven surface on the graphite foil could be observed, as shown in Figure 3a,b. As shown in Figure 3c,d, the surface cracks decreased, and some graphite pieces remained on the graphite foil surface after plasma treatment for 30 s. With plasma treatment for a longer time, i.e., 3 min, more severely surface cracks occurred, which were associated with the surface damage, as shown in Figure 3g,h. These results suggest reactive plasma species likely made some impacts on the graphite foil surface during plasma treatment by ion bombardment, thereby damaging the surface [36,37].

3.2. XPS Analysis

To investigate the change in the elemental composition of the graphite foil after He-DBD jet treatment, XPS was performed to analyze C1s and O1s spectra of the graphite foil, as shown in Table 1 and Table 2 and Figure 4, Figure 5 and Figure S2. In Figure 4 and Table 1, it is evident that the elemental composition of C decreased and O increased for a longer plasma process. In Figure 5, the C1s spectra of the graphite foil can be deconvoluted into four groups: sp2 carbon (C=C) at 284.5 eV, sp3 carbon (C–C) at 285.3 eV, hydroxyl (C–OH) at 286.2 eV and epoxy (C–O–C) at 286.8 eV [38,39]. After He DBD jet treatment, the amounts of oxygenated components (hydroxyl (C–OH) and epoxy (C–O–C)) increased, which can be seen from Table S2. It suggests that the oxygen ions from plasma species may bond into the graphite foil surface during the He-DBD jet plasma treatment, leading a higher wettability of graphite foil. This is evidenced in our previous studies regarding the processing of DBD jet materials. Furthermore, the He DBD jet caused ion bombardment on the graphite foil surface, resulting in more surface cracks and a lower C content [36]. These results correspond to the SEM results.

3.3. External Quantum Efficiency Analysis

Figure 6 shows the static water contact angle of the graphite foil without He DBD jet plasma treatment. Without He DBD jet plasma treatment, the water contact angle of the graphite foil was 65.16°. After plasma treatment, the water contact angle became almost zero. This indicates that He DBD jet plasma treatment makes the graphite foil surface more hydrophilic, corresponding to the increase in the oxygen-containing function groups on the graphite foil as indicated by the XPS results. The comparison of the hydrophilicity between the graphite foils with and without plasma treatment are shown in the Supplementary Information (Video S1).

3.4. Electrochemical Performance of Paper-Based Al-Air Batteries

Figure 7 presents the polarization (V-I) and power density curves recorded at different scan numbers as measured by LSV. The arrows indicate whether a given curve corresponds to the voltage or power density. The LSV measurement was performed when the active area of the filter paper was filled with electrolyte (1.5 M KOH). The LSV measurement from OCV to 0 V was recorded nine times. Figure 8 shows the discharge curves at a current density of 20 mA/cm2. Compared with the graphite foil without He DBD jet plasma treatment, the graphite foil with 30-s He-DBD jet treatment has maximum current density (85.6 mA/cm2), power density (40.98 mW/cm2) and energy density (720 Wh/kg), as shown in Figure 7 and Figure 8. It suggests that the highly hydrophilic graphite foil produced after 30-s He DBD jet treatment is good for liquid-electrode contact [5]. This result also shows that the Al-air batteries with 30-s DBD jet treatment has a good capacity and a better polarization with maximum current density and power density compared with other research of Al-air batteries, as listed in Table S2. However, a graphite foil with longer He-DBD jet plasma treatment times decreased the performance of the batteries. Furthermore, the battery performance became unstable at the ninth LSV measurement. It indicates that more damage (severe surface cracks) and oxygenated components on the graphite foil surface resulted in increased sheet resistance of the graphite foil that, in turn, caused degradation of the cathode catalyst [36].

3.5. Electrochemical Impedance Spectroscopy Analysis

The above results can be further validated through EIS measurements. The EIS measurement was implemented on OCV of the Al-air batteries with an amplitude of 10 mV and a frequency range of 100 kHz to 0.01 Hz. Figure 9 shows the Nyquist plot of EIS. The inset shows the equivalent circuit. Furthermore, Table S1 lists the EIS fitting parameters. Rs, Rpa and Rpc, corresponding to the solution resistance, polarization anode resistance and polarization cathode resistance, respectively. Rpc includes the cathodic charge transfer resistance, cathodic diffusion layer resistance and accumulated resistance caused by corrosion, existing molecules or ions. Similarly, Rpa includes the anodic charge transfer resistance, anodic diffusion layer resistance and accumulated resistance [40,41]. Table S1 indicates that Rs and Rpa did not obviously change when the graphite foil was treated with He DBD jet plasma. However, Rpc of the graphite foil with 30-s He DBD jet plasma treatment was 21.57 Ω; this value was much lower than those of the others, and it corresponds to the above results.

4. Conclusions

This study successfully functionalized the graphite foil surface with He DBD jet plasma treatment. By plasma, the graphite foil surface could be so hydrophilic that the DI water droplet penetrate into the surface directly. An appropriate He DBD jet plasma treatment time of the graphite foil could enhance the wettability of the graphite foil and decrease the amount of the surface cracks. These surface modification and functionalization effectively improve the distribution of the catalyst layer, resulting in lower polarization cathodic resistance and higher power density and energy density. Furthermore, the resulting battery could light up an LED, as shown in Video S2 (Supplementary Information). This indicates that the resulting battery could be used for the micro-electrical device.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/en15165914/s1, Figure S1: Setting of the paper-based Al-air battery; Figure S2: XPS survey scan spectra of graphite foil without and with He DBD jet treatment; Figure S3: XPS of O1s spectra of graphite foil without and with He DBD jet treatment; Table S1: EIS fitting parameters, Table S2: Comparisons of Al-air batteries [42,43,44,45,46].

Author Contributions

Conceptualization, J.-Z.C.; methodology, C.-Y.S., C.-L.C. and J.-Z.C.; formal analysis, I.-C.N., C.-Y.S. and C.-L.C.; investigation, C.-Y.S., C.-L.C. and J.-Z.C.; resources, C.-C.H., C.-I.W., I.-C.C. and J.-Z.C.; data curation, C.-Y.S. and C.-L.C.; writing—original draft preparation, C.-Y.S., C.-L.C. and J.-Z.C.; writing—review and editing, J.-Z.C.; supervision, J.-Z.C.; project administration, J.-Z.C. All authors have read and agreed to the published version of the manuscript.

Funding

We sincerely convey our gratitude for acquiring funding support from the Advanced Research Center for Green Materials Science and Technology from The Featured Area Research Center Program of the Higher Education Sprout Project by the Ministry of Education (111L9006) and the National Science and Technology Council in Taiwan (NSTC 111-2221-E-002-088-MY3, NSTC 111-2634-F-002-016). This study is also partly supported by the National Science and Technology Council of Taiwan under grant no. MOST 111-3116-F-002-005.

Institutional Review Board Statement

Not applicable. The authors declare that no animal or human participants were involved in this study.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

Our gratitude to C.-S. Lin and Y.-T. Lee of the Instrumentation Center, National Taiwan University for assisting us with FEG-SEM experiments.

Conflicts of Interest

The authors declare no conflict of interest in this study.

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Energies 15 05914 g001 550
Figure 1. Schematic of the He-DBD jet.
Figure 1. Schematic of the He-DBD jet.
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Figure 2. Flowchart of the Al-air battery fabrication process.
Figure 2. Flowchart of the Al-air battery fabrication process.
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Figure 3. Top-view SEM images of graphite foil (GF) (a,b) without and (c–h) with He DBD jet treatment for (c,d) 30 s, (e,f) 1 min and (g,h) 3 min.
Figure 3. Top-view SEM images of graphite foil (GF) (a,b) without and (c–h) with He DBD jet treatment for (c,d) 30 s, (e,f) 1 min and (g,h) 3 min.
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Figure 4. XPS survey scan spectra of graphite foil (a) without and (b–d) with He DBD jet treatment for (b) 30 s, (c) 1 min and (d) 3 min.
Figure 4. XPS survey scan spectra of graphite foil (a) without and (b–d) with He DBD jet treatment for (b) 30 s, (c) 1 min and (d) 3 min.
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Figure 5. XPS of C1s spectra of graphite foil (a) without and (b–d) with He DBD jet treatment for (b) 30 s, (c) 1 min and (d) 3 min.
Figure 5. XPS of C1s spectra of graphite foil (a) without and (b–d) with He DBD jet treatment for (b) 30 s, (c) 1 min and (d) 3 min.
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Figure 6. Static water contact angle of graphite foil without He-DBD jet treatment.
Figure 6. Static water contact angle of graphite foil without He-DBD jet treatment.
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Figure 7. Polarization (V-I) and power density curves recorded at different scan numbers measured by continuous LSV. The current collector was a graphite foil (a) without and (b–d) with He DBD jet plasma treatment for (b) 30 s, (c) 1 min and (d) 3 min.
Figure 7. Polarization (V-I) and power density curves recorded at different scan numbers measured by continuous LSV. The current collector was a graphite foil (a) without and (b–d) with He DBD jet plasma treatment for (b) 30 s, (c) 1 min and (d) 3 min.
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Figure 8. Discharge curves at a current density of 20 mA/cm2.
Figure 8. Discharge curves at a current density of 20 mA/cm2.
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Figure 9. The Nyquist plot of EIS.
Figure 9. The Nyquist plot of EIS.
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Table
Table 1. Elemental composition of C and O in graphite foil, as determined from XPS spectra.
Table 1. Elemental composition of C and O in graphite foil, as determined from XPS spectra.
%CO
No plasma treatment97.622.38
He DBD jet 30 s96.643.36
He DBD jet 1 min94.085.92
He DBD jet 3 min88.0411.96
Table
Table 2. XPS deconvolution results for C1s spectra of graphite foil.
Table 2. XPS deconvolution results for C1s spectra of graphite foil.
%C=CC–CC–OHC–O–C
No plasma treatment87.738.622.860.79
He DBD jet 30 s87.668.512.930.90
He DBD jet 1 min87.337.963.191.52
He DBD jet 3 min77.8713.584.434.12
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Shih, C.-Y.; Ni, I.-C.; Chan, C.-L.; Hsu, C.-C.; Wu, C.-I.; Cheng, I.-C.; Chen, J.-Z. Helium Dielectric Barrier Discharge Plasma Jet (DBD Jet)-Processed Graphite Foil as Current Collector for Paper-Based Fluidic Aluminum-Air Batteries. Energies 2022, 15, 5914. https://doi.org/10.3390/en15165914

AMA Style

Shih C-Y, Ni I-C, Chan C-L, Hsu C-C, Wu C-I, Cheng I-C, Chen J-Z. Helium Dielectric Barrier Discharge Plasma Jet (DBD Jet)-Processed Graphite Foil as Current Collector for Paper-Based Fluidic Aluminum-Air Batteries. Energies. 2022; 15(16):5914. https://doi.org/10.3390/en15165914

Chicago/Turabian Style

Shih, Chung-Yueh, I-Chih Ni, Chih-Lin Chan, Cheng-Che Hsu, Chih-I Wu, I-Chun Cheng, and Jian-Zhang Chen. 2022. "Helium Dielectric Barrier Discharge Plasma Jet (DBD Jet)-Processed Graphite Foil as Current Collector for Paper-Based Fluidic Aluminum-Air Batteries" Energies 15, no. 16: 5914. https://doi.org/10.3390/en15165914

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