| Citation: |
Erhao GAO, Keying GUO, Qi JIN, Li HAN, Ning LI, Zuliang WU, Shuiliang YAO. NaCl aqueous solution as a novel electrode in a dielectric barrier discharge reactor for highly efficient ozone generation[J]. Plasma Science and Technology, 2023, 25(7): 075502. DOI: 10.1088/2058-6272/acbef6
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Ozone (O3) generated by a dielectric barrier discharge (DBD) is widely used in various industrial processes. In this study, NaCl aqueous solution was used as a novel electric power transmission electrode in a DBD reactor (instead of a traditional metal electrode) for highly efficient ozone generation. The results demonstrated that a high O3 yield of 242 g kWh-1 with a concentration of 14.6 g m-3 O3 was achieved. The power transmission mechanism works because NaCl aqueous solution behaves as a capacitor when an alternating pulse voltage below 8 kHz is used. Compared with the resistance of the discharge barrier and discharge space, the resistance of NaCl aqueous solution can be ignored, which ensures that O3 is generated efficiently. It is expected that O3 generation using NaCl aqueous solution as a novel electrode in a DBD reactor could be an alternative technology with good application prospects.
Ozone (O3) is an oxidant with an extremely strong oxidation capacity (its standard redox potential is -2.07 V) and is widely used in advanced oxidation [1], chemical biological processes [2], agricultural [3], food [4], medicine [5, 6] and water and wastewater treatment [7]. O3 is usually produced by applying a high voltage to a dielectric barrier discharge (DBD) generator in a discharge space in which an O2-containing gas is present. A DBD generator is composed of a pair of metal electrodes and an insulating glass tube [8]. In a DBD generator, oxygen molecules are decomposed into active oxygen atoms, which then combine with O2 to form O3. A large amount of electrical energy is injected into the discharge space, resulting in an increase in the temperature of O2-containing gas, which reduces O3 yield [9]. Thus, the discharge space is cooled using cooling water passing through the inside of the metal electrode, but this increases the complexity and energy consumption of the ozone generator. In this regard, the development of a simple and energy-efficient approach for ozone generation has attracted much attention [10–12].
Traditional O3 generation technology has five technical features, namely O2-containing gas, alternating power supply, dielectric medium, metal electrodes and cooling water, in which the metal electrode is the key component determining how much energy is consumed. The commonly used metal electrodes are aluminum (Al) and copper (Cu), but the Al and Cu industries are highly energy-intensive and pollution-creating [13, 14]. By contrast, a quartz tube containing aqueous solution used as the inner electrode is an excellent choice for O3 generation, because the discharge space can be better cooled by the solution and a quartz electrode has stronger corrosion resistance and better durability than a metal electrode. In addition, the CO2 emission of Al and Cu is 17.7 times and 2.3 times greater than that of quartz, the price is 12 times and 40 times and the cost of the inner electrode is 13 times and 143 times, respectively (table 1). Therefore, using a quartz tube containing aqueous solution, instead of metal, as the electrical power transmission electrode could not only lower the cost but also reduce CO2 emission significantly.
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Herein, NaCl aqueous solution is used to substitute for a metal electrode to transmit electrical power for highly efficient O3 generation. NaCl solution is a typical electrolyte, and its electric transmission derives from its superior capacitance and resistance properties, with the capacitance being realized from the relative change in position of hydrated ions of Na+ and Cl- [such as ionic aqueous clusters Na+(H2O)n (n = 4, 5, 6, 14) and Cl-(H2O)n (n = 4, 5, 6, 7, 8, 14) [23]], and the resistance is due to the movement of hydrated ions towards the electrodes. The ionic conductivity of 0.1 mol l-1 NaCl aqueous solution at 25 ℃ is 1.07 Ω-1 m-1, which is much lower than that of an electronic conductor (such as copper, 6.5 × 107 Ω-1 m-1) [24]. This study aims to explore NaCl aqueous solution as a potential power transmission electrode for O3 generation, and the capacitance and resistance properties of NaCl aqueous solution that reflect the power transmission mechanism are carefully analyzed.
O3 generation was performed using the experimental system shown in figure 1. The DBD reactor mainly consisted of two quartz tubes, one stainless steel rod connected with a pulse power supply (M10K-08, Suzhou Allftek, China), Al foil (as a ground electrode), 0.3% NaCl aqueous solution (as an electrode connected with the high-voltage terminal of a pulse power supply) and two rubber stoppers. The length of the Al foil (l) changed from 4.8 cm to 30.8 cm. A DBD was produced in the discharge gap space by applying voltage pulses to the stainless steel rod and Al foil from the pulse power supply. The waveforms of the discharge voltage and current were observed and recorded using a high-voltage probe (P6015A, Tektronix, USA), current probe (CP8030H, Cybertek, China) and oscilloscope (MDO3034, Tektronix, USA). The discharge energy was calculated using the waveform data for the discharge voltage and current [9]. O2 (purity 99.999%) was supplied to the DBD reactor at a flow rate of 30 l h-1. The O3 concentration was detected using an O3 detector (BMOZ-200t, Weifang Shengxin, China). O3 yield was defined as the amount of O3 per kWh discharge energy injected into the DBD reactor.
The discharge power P (W) from the pulse power supply to the DBD reactor for O3 generation was calculated using equation (1)
| P=fΣ | (1) |
where Vi and Vi+1 are the discharge voltages (V) at discharge times ti and ti+1 (s), respectively. Ii and Ii+1 are the discharge currents (A) at discharge times ti and ti+1, respectively. i and i + 1 are step values of the datum sequences and f is the pulse frequency.
O3 yield was defined as the amount of O3 per kWh discharge energy injected into the DBD reactor. It was calculated using equation (2)
| (2) |
where E is the O3 yield (g kWh–1), C is the O3 concentration (g m–3), and 30 is the flow rate (l h–1).
The experimental device shown in figure 2(a) was used to measure the capacitance and resistance properties of 0.3 wt% NaCl aqueous solution. The NaCl aqueous solution was placed in a plastic box. Two inside walls of the plastic box were partly pasted with Al foil. The area of Al foil in water was 4.7 cm × 4.2 cm. The distance between two Al foils was 5.4 cm. Triangular wave voltages of 7 V (peak-to-peak) and a frequency between 100 Hz and 3 MHz were applied between two Al foils using a signal generator (CA1645, Vantek, China). The voltage and current waveforms were observed and recorded with a current probe (CT-1, Tektronix, USA), voltage probe (TPP0250, Tektronix, USA) and oscilloscope (MDO 3034, Tektronix, USA).
The resistance characteristics of NaCl aqueous solution of different concentrations used as a power transmission electrode were studied by simulating the barrier and discharge parts as a resistor with a resistance (R0) of 10.127 kΩ (figure 2(b)). The voltage and current waveforms from a pulse power supply (pulse frequency of 0‒8 kHz; M10K-08, Suzhou Allftek, China) were measured and recorded using a voltage probe (P6015A, Tektronix, USA), current probe (CP8030H, Cybertek, China) and oscilloscope (MDO3034, Tektronix, USA). All experiments were carried out at room temperature (25 ℃).
O3 generation was investigated using the experimental system in figure 1. Figure 3(a) shows that O3 concentration increased linearly with increasing discharge power, where discharge power was increased by increasing the voltage, pulse frequency or discharge space (Al foil length l). When the discharges were carried out at a fixed pulse frequency (300 Hz) and different voltages (16, 18, 20, 22 or 24 V), the discharge power and O3 concentration were 1.77 W and 14.8 g m-3 and increased to 5.55 W and 32.0 g m-3 when l was 30.8 cm. When l was 4.8 cm, the increase in O3 concentration with discharge power was obviously lower than for other l values (figure 3(a)). Similar results were found when the discharges were carried out at a fixed voltage (20 V) and different pulse frequencies (100, 200, 300, 400 or 500 Hz) (figure 3(b)). High-energy electrons generated during a DBD make O2 dissociate into O via O2 + e = O + O and O3 is generated via O2 + O = O3. More high-energy electrons are formed with increasing discharge power, which can improve O3 generation. In addition, the O3 concentration increased first and then stabilized with increase in l at the same discharge power. This may be because the residence time of O2 in the discharge space increases with the increasing l, which contributes to the O3 generation reaction.
Ozone yield is an important indicator for an O3 generator. The relationship between the O3 yield and discharge power showed that the O3 yield with increasing discharge power was obviously decreasing when l was 4.8 cm and above 22.4 cm, but when l was between 9.2 and 18.1 cm there was no clear relationship between the O3 yield and discharge power (figures 3(c) and (d)). The highest O3 yield was 242 g kWh-1 when l = 26.7 cm and the discharge power was 1.51 W (figure 3(c)). To test the stability of O3 generation, a 1-h O3 generation experiment was carried out under a fixed voltage and a frequency of 50, 200 or 500 Hz. The O3 concentration remained stable within 1 h at a fixed frequency (figure 3(e)). This fact implies that stable O3 generation can be obtained by using a DBD reactor constructed with NaCl aqueous solution as the power transmission electrode.
We compared the yields of O3 prepared using different DBD reactors equipped with metal electrodes and found that the yields of O3 reported by different researchers varied (figure 3(f)). The yield of O3 reached 165 g kWh-1 with a concentration of 16.5 g m-3 in Zhang's work using similar coaxial DBD geometry to the present experiment [10]. The O3 yield was lower than that in our study. The maximum O3 yield of 320 g kWh-1 was obtained under an O3 concentration of 3.5 g m-3 using a multi-hollow surface DBD [36]. From figure 3(f), the O3 yield decreased with increase in O3 concentration. In this study, the O3 yield decreased from 242 g kWh-1 to 173 g kWh-1 as the O3 concentration increased from 13.3 g m-3 to 35.3 g m-3. A top limit line can be clearly drawn to describe the maximum O3 yield at a fixed O3 concentration. Our best O3 yield results are on the top limit line, which shows that the NaCl aqueous solution electrode can achieve the same O3 yield as a metal electrode, and the NaCl aqueous solution electrode could replace the metal electrode for O3 generation.
In order to understand the electric power transmission mechanism of the NaCl aqueous solution, the discharge voltage and current waveforms were analyzed. From the voltage waveform (figure 4(a)), it can be confirmed that the peak value of voltage was 17.8 kV, the rise time was 50 μs (the time between the voltage rise from 10% to 90% of the peak value) and the full width at half maximum was 77 μs. The DBD is a typical combination of a large number of micro discharges [37], and they can be confirmed from sharp pulses (the spike part of the current waveform) of non-continuous and very short duration (figure 4(a)). In the voltage–current diagram (figure 4(b)) it can be seen that when the voltage changed, the positive currents of white lines C1 and C3 remained constant at values of 0.002 and 0.022 A, respectively. Obviously, the NaCl aqueous solution presented capacitive characteristics during the discharge. Corresponding to C1 and C3, the voltage increased from 0 to 17.8 kV within 83.6 μs, thus the voltage rise speed was 2.1 × 108 V s-1. From the current value of C1 (0.002 A), the capacitance during the C1 period can be calculated to be 9.5 pF. From the current value of C3 (0.022 A), the capacitance of the C3 period was 105 pF. The C1 period is the non-discharge period and the C3 period is the discharge period. The difference in capacitance between C1 and C3 is due to the increase in discharge charges deposited on the surface of the discharge tube after discharge, which led to the increase in capacitance. We also calculated the voltage/current values during the duration of a pulse discharge to evaluate the impedance characteristics. The impedance was within the range of 3 kV A-1 to 10 MV A-1 (figure 4(c)). The influence of voltage wave (triangle wave) frequency on the capacitance and resistance properties of 0.3% NaCl aqueous solution was studied using the experimental system in figure 2(a).
When the frequency of the triangular voltage wave increased from 8 kHz to 10 kHz, the current waveform changed obviously (figure 5). When the frequency of the triangular voltage wave was below 8 kHz, the current was constant as the voltage changed at a certain speed. The NaCl aqueous solution presented capacitive characteristics, and the capacitance values were in the range of 110‒130 nF at different frequencies (figure 6). When the frequency of the triangular voltage wave increased to 9 kHz, the current did not stay constant when the voltage alternated at a constant speed, and the NaCl aqueous solution presented both capacitance and resistance properties. When the frequency of the triangular voltage wave was above 10 kHz, resistance characteristics appeared and the current and voltage were basically linear.
The capacitance and resistance properties of an electrolyte solution can be described using double layer theory. The capacitance and resistance of an electrolytic cell can be presented using an equivalent circuit, in which the body of the electrolyte solution is a resistor and the double layers over the electrode surfaces are taken as the in-parallel connected capacitor (CD) and resistor (RD). When the frequency (f) of the applied voltage is far higher than 1/2πCDRD, the resistance in the double layers becomes far lower than that in the body of the electrolyte solution, and the whole electrolytic cell shows resistance characteristics. Thus, 8‒10 kHz may be the boundary area for the 0.3% NaCl aqueous solution to change from a capacitor to a resistor.
Due to the impedance being within the range between 3 kV A-1 and 10 MV A-1 (figure 4(c)), we used a resistor (10.127 kΩ) to simulate the entire resistance of the discharge circuit. The waveforms of discharge voltage and current are shown in figure 7. The voltage increases from 0 to 176 V (peak value) in 50 μs, indicating that the frequency of the voltage pulse is equivalent to triangular voltage waves with a frequency of around 5 kHz. Under such a a pulse voltage frequency it is obvious that the NaCl aqueous solution acts as a capacitor when the frequency (here 5 kHz) is lower than 8 kHz.
The relations of voltage and current across 0.3% NaCl aqueous solution, pure water and resistor are illustrated in figure 8. It was found that the electric resistance of the 0.3% NaCl aqueous solution was 10 200 Ω (figure 8(a)) and those of pure water and the resistor were 28 360 Ω (figure 8(b)) and 10 127 Ω (figure 8(c)), respectively. The resistance of the NaCl aqueous solution decreased obviously when a small amount of NaCl was added and became a constant when the NaCl concentration was higher than 0.05% (figure 8(d)). The whole discharge circuit has a resistance property when the NaCl aqueous solution is connected in series with the resistor (R0). Furthermore, the resistance of the NaCl aqueous solution was only 0.72% of that of the resistor (R0); this finding indicated that the resistance of the NaCl aqueous solution can be ignored, i.e. the energy used in the NaCl aqueous solution for electric transmission can be ignored, which ensures that O3 can be generated efficiently. Certainly, the frequency of the voltage pulse should be controlled under 8 kHz during the O3 generation using a DBD.
In this study, O3 was generated stably in a DBD reactor using NaCl aqueous solution as an electric power transmission electrode rather than a conventional metal electrode. The O3 yield was almost equivalent to the best value in related publications. The O3 yield achieved a level of 242 g kWh-1 and 14.6 g m-3 O3 concentration. The power transmission mechanism is due NaCl aqueous solution having a behavior of a capacitor when the alternating pulse voltage is below 8 kHz. The resistance of the NaCl aqueous solution can be ignored in this kind of application, as the resistance of the discharge barrier is far higher than that of the NaCl aqueous solution. NaCl aqueous solution as a novel electrical power transmission electrode is simpler and more energy-efficient than traditional metal electrodes. Its industrial application for O3 generation is quite promising and it will contribute to abatement of CO2 emission and global warming control.
This research was supported by National Natural Science Foundation of China (Nos. 12075037 and 22206013), the Natural Science Foundation of Jiangsu Province (No. BK20210857) and the Leading Innovative Talents Cultivation Project of Changzhou City (No. CQ20210083).
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Figures(8) / Tables(1)
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