A nanofluidic chemoelectrical generator with enhanced energy harvesting by ion-electron Coulomb drag

doi:10.21203/rs.3.rs-3828339/v1

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A nanofluidic chemoelectrical generator with enhanced energy harvesting by ion-electron Coulomb drag

https://doi.org/10.21203/rs.3.rs-3828339/v1

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A sufficiently high current output of nano energy harvesting devices is highly desired in practical applications, while still a challenge. Theoretical evidence has demonstrated that Coulomb drag based on the ion-electron coupling interaction, can amplify current in nanofluidic energy generation systems, resulting in enhanced energy harvesting. However, experimental validation of this concept is still lacking. Here we develop a nanofluidic chemoelectrical generator (NCEG) consisting of a carbon nanotube membrane (CNTM) sandwiched between metal electrodes, in which spontaneous redox reactions between the metal and oxygen in electrolyte solution enable movement of ions within the carbon nanotubes. Through Coulomb drag effect between moving ions in these nanotubes and electrons within the CNTM, an amplificated current of 1.2 mA·cm^-2 is generated, which is 15.6 times higher than that collected without a CNTM. Meanwhile, one single NCEG unit can produce a high voltage of ~0.8 V and exhibit a linear scalable performance up to tens of volts. Different from the other Coulomb drag systems that need additional energy input, the NCEG with enhanced energy harvesting realizes the ion-electron coupling by its own redox reactions potential, which provides a possibility to drive multiple electronic devices for practical application.

Physical sciences/Nanoscience and technology/Nanoscale devices/Nanofluidics

Physical sciences/Chemistry/Physical chemistry/Electron transfer

energy harvesting

Coulomb drag

nanofluidic

carbon nanotube

interface energy

The phenomenon of Coulomb drag was initially documented as electron-electron interactions between two closely spaced, yet electrically isolated conductors, referred to as “layers”. Due to long-range interactions between these two distinct layers, an electrical current flowing through one of the layers, known as the “active layer”, can induce an electrical current in the other layer, the “passive layer”. During this process, both the energy and momentum of the carriers in the “active layer” transfer to the carriers in the “passive layer”, resulting in the generation of an open circuit voltage and short circuit current through efficiently “dragging” them along.^1–3

A similar dragging effect has also been observed in nanofluidic-based devices, extending the concept of Coulomb drag to interactions between a moving ionic fluid and electrons in conductors.^4–9 It has been discovered that a nanoampere electrical current in graphene can be induced by ionic flow which is driven by applying voltage to the fluidic chamber,¹⁰ as the flow of fluids induces electrical polarization, driving electrical currents. Conversely, electrical excitations also contribute to ions movement. By applying an externally biased voltage to the single-walled carbon nanotube (SWCNT) shell layer, an electrical current is generated which drags ions through the SWCNT nanochannels, resulting in an ionic drag current with opposite direction.¹¹ Recently, Xiong et al. demonstrated that this generated current originates from the confined ion-electron interactions via a nanofluidic Coulomb drag mechanism through calculations and simulations.¹² The model predicts the amplification of ionic current by the electric energy applied on the semiconductive membrane due to the significant difference between ion mass and hole mass on the semiconductive membrane, deepening the understanding of the ion-electron interactions in nanochannels and demonstrating the potential for enhancing the current output in energy harvesting. With the amplified current resulting from Coulomb drag effect, the bottleneck of low current in the practical application of nano energy generators can be addressed.^13–15 However, further experimental work is still needed to verify the amplification of ionic current. In addition, all previously reported studies on Coulomb drag effect needed an external electrical field to drive the electrons or ionic flow.^10,11 These additional energy input components increase the complexity of the energy-harvesting devices, hindering their practical application. Therefore, it is important to develop nanofluidic-based energy generators that can not only exploit the current amplification effect by Coulomb drag but also power the ionic flow itself.

In this work, we present a high-performance nanofluidic chemoelectrical generator (NCEG) based on a carbon nanotube membrane (CNTM), which is fabricated by sandwiching a CNTM with an area of around 25 mm² between two metal electrodes. To drive the ionic flow by the NCEG itself, we utilize metal-air redox reactions that can convert chemical energy into electrical energy without external stimulation.^16–18 Through the spontaneous redox reactions, a chemical potential is established across the membrane, which provides a driving force for the migration of ions in the nanochannels of CNTM. As a result, the current coupling of ion-electron is amplified to three times larger than that of the literatures where an external voltage was applied to drive the ionic flow.^10,11 Furthermore, this device can generate a stable and sustained direct voltage of 0.8 V and a short-circuit current density of 0.8 mA·cm^− 2, with a power density of 74 µW·cm^− 2, under ambient conditions for up to 80 hours. This work firstly provides experimental evidence that ion-electron Coulomb drag interactions can amplify currents for energy harvesting and offers a scalable strategy for energy harvesting devices based on nanofluidic systems.

Schematic and electrical output characteristics of NCEG

In general, an applied voltage is needed to drive ion movement by Coulomb drag phenomenon in the nanofluidic system.^10,11 However, for a nanofluidic-based energy generator through Coulomb drag, it is essential that the device itself can facilitate ion transport within the nanochannels without requiring additional voltage components, thereby simplifying its structure. Here, we reported a compact nanofluidic energy generator device with an active electrode, in which the redox reactions on the electrode were employed to provide chemical potential, driving the transport of ions in nanochannels, and enhancing the collected current by Coulomb drag (Fig. 1a). As shown in Supplementary Fig. 1a, a highly arrayed porous CNTM is sandwiched between a pair of metal electrodes, which are a gold foil and a conductive carbon tape (Nissin SEM double-sided conductive carbon tape) containing an aluminum substrate, respectively. And the preparation procedure of nitrogen-doped CNTM is illustrated. With a template of porous anodic aluminum oxide (AAO), nitrogen-doped CNTM was grown through the conventional chemical vapor deposition (CVD) approach using humidified acetonitrile bubbler as the single source of both carbon and nitrogen. The optical photograph and the cross-section SEM of the CNTM are shown in Fig. 1b. The peaks of nitrogen and carbon in X-ray photoelectron spectroscopy (XPS) of nitrogen-doped CNTM (Supplementary Fig. 2) prove the successful fabrication of nitrogen-doped CNTM on the AAO template. When only the bottom conductive carbon tape electrode and the CNTM encounter 0.1 M NaCl electrolyte, an open circuit voltage (V_OC) of approximately 0.8 V (Fig. 1c) and a persistent current density of around 0.8 mA·cm^− 2 (Fig. 1d) can be achieved.

The origin of the output voltage signal

Figure 2a shows that the output voltage signal is from the redox reactions between the metal electrode and oxygen. In the presence of the electrolyte solution, the oxidation of the bottom metal electrode occurs, generating an electrical potential, thus realizing the conversion of chemical energy into electrical energy.^19–21 The output voltage can drive ions in nanochannels transporting, which then couple electrons from CNTM moving and will be explained later. To confirm the origin of the output voltage signal, position variations of the electrolyte solution were explored. As shown in Fig. 2b, no significant voltage output can be observed when the electrolyte solution only contacts with the bottom of the CNTM. In this case, the necessary conditions for redox reactions are not sufficient. With the contact between the electrolyte solution and the bottom electrode on the CNTM, the redox reactions occurred and a potential difference between the conductive carbon tape electrode and O₂ in the electrolyte was built, resulting in a V_OC of around 0.8 V. However, the V_OC of the generator decreased sharply to 0 V when the electrolyte submerged both the bottom and top electrodes, which can be ascribed to the counteraction of the primary battery potential between the two electrodes. Furthermore, the sign of output voltage can be controlled by changing the reaction electrode. As shown in Fig. 2c, a V_OC of 0.8 V is generated when the electrolyte contacts with the bottom electrode, while a voltage of -0.8 V results from the contact between the electrolyte and the top electrode. To exclude the effect from CNTM, two different connection statuses between the electrode and CNTM were explored (Fig. 2d). In both cases, the output voltages have no obvious difference, which can further confirm that the output voltage in the nanofluidic chemoelectrical generator is only related to the redox potential between the metal electrode and O₂ in the electrolyte. The redox reactions that occurred between the metal electrode and oxygen are summarized as following:

${\text{O}}_{2}+4{e}^{-}+2{H}_{2}O\to 4{OH}^{-}$ (cathode electrode) (1)

$M\to {M}^{n+}+n{e}^{-}$ (anode electrode) (2)

where M represents the metal electrode.

In these reactions, the pH of the electrolyte^22–24 and electrode activity^25–28 have significant effects on output voltage. The output voltage shows a higher value up to 1.2 V but decays gradually when the neutral NaCl electrolyte solution was substituted by a strong acid or alkaline (Fig. 2e), indicating the accelerated redox reactions caused by the more reactive electrolyte solutions.²⁹ The presence of bubbles at the reaction interface (Supplementary Fig. 3) also confirmed the chemical reactions, as evidenced by chemical equations (3) and (4) below:

$$M+HCl\to {MCl}_{n}+{H}_{2}\uparrow$$

$$M+NaOH\to {NaMO}_{2}+{H}_{2}\uparrow$$

The decayed output voltage can be attributed to the corrosive depletion of the bottom electrode.^30–32 The electrode activities of various metals determine the potentials in the redox reactions.³³ As shown in Fig. 2f, the output voltages are highly correlated with the electrode activities, in which more active electrodes result in higher output voltages. After the redox reactions, the metal ions (Zn²⁺ as an example) will be released from Zn electrode and can be driven to move from the bottom reaction site to the top layer (Supplementary Fig. 4), which can further confirm the redox reactions and the generation of transmembrane potential.

Current amplification via ion-electron Coulomb drag

For ions transport in a nanofluidic device, free electrons can be induced to migrate via ionic Coulomb drag when the cations of the electrolytes move along the solid channel surface benefiting from the ionic selectivity in surface charged nanochannel.^8–12 Theoretical study has demonstrated the potential utilization of Coulomb drag between ions within nanochannels and electrons/holes on semiconductors to amplify ionic current, due to a significant disparity between the ion mass and the effective mass of electrons/holes.¹² In the previous part, it has been proved that the redox reactions were employed to power the ionic transport in the nanochannels of CNTM. As a result, an amplified current density of 1.2 mA·cm^− 2 can be observed in the CEG device, which is 15.6 times higher than the current collected by the primary cell without CNTM (Fig. 3a).

To further validate the mechanism of the current amplification induced by the ionic flow in the nanochannels, we conducted a comparison of the current in the NCEG with and without the presence of an electrolyte solution (0.1 M NaCl). In this case, all the electrodes in the NCEG were replaced as gold electrodes to avoid the potential difference. The output voltage of the redox reactions was replaced by an external voltage applied via a waveform generator to power the ionic flow. As shown in Fig. 3b, under different voltage output, including ± 2, ±1, and ± 0.5 V, the current densities detected with NaCl electrolyte are consistently higher than those without NaCl electrolyte. This can be attributed to the reduction of electrical resistance with electrolyte and the Coulomb drag effect within nanochannels. As schemed in Fig. 3d i, without the addition of electrolyte solution, the electrons powered by external voltage can only transfer in the semiconductor, CNTM, whose electrical resistance is much higher than that of electrolyte solution, resulting in a low current. Once the electrolyte solution is added, an ion pathway is established in parallel as depicted in the equivalent circuit on the right of Fig. 3d iii, enabling the charges from the redox reactions to be transported via the cations and anions in the electrolyte solution (Fig. 3d ii). Figure 3e and 3f confirm the ionic flow along the nanochannels of NCEG, where both sodium and chloride were detected on the top surface of the CNTM by EDS in the case that the bottom surface of CNTM was only in contact with the electrolyte solution. With the ionic flow along the nanochannels of NCEG, the Coulomb drag effect between the ionic flow in the nanochannels and electrons in the CNTM occurs, significantly contributing to the amplification of the current density. Figure 3d iii illustrates the interactions between the electrons in the CNTM and the ions flowing in the nanochannels. Based on the principle of momentum conservation and the fact that the typical mass ratio between the ions and the holes is of the order of 10⁵ to 10⁶,¹² the ion transport in the nanochannels promotes the number of electrons in the CNTM and therefore a remarkably amplified current can be achieved.

Figure 3b also shows that the deviation between the current density values with and without electrolyte solution increases with the increase of the loading external voltages. The increase of current density (ΔJ_SC1) exhibited an exponential enhancement with the increase of external voltage (Supplementary Fig. 5), indicating that with the increase of current in the circuit, the number of ions moving in the nanochannels is sharply increased, leading to more electrons transferring in the CNTM (Fig. 3d iii). A similar effect was also observed when different external resistances were loaded in the circuit. As the circuit diagram illustrated in the inset of Fig. 3c, under a fixed voltage of 0.8 V provided by the redox reactions, the increase of loaded resistance leads to a drop in the circuit current density, which was calculated as J_{SC−theoretical} in Fig. 3c. As shown in Supplementary Fig. 6, the current density difference (ΔJ_SC2) decreases with the increase of the loading external resistances. Strikingly, the measured circuit currents are much higher than the theoretical values of the current, showing the current amplification caused by the ionic Coulomb drag.

Enhanced output energy power and application

Figure 4a and 4b display the energy outputs with different resistive load conditions. With a 25 mm² working area of the CNTM, the maximum volumetric power density can reach 74 µW·cm^− 2 when an optimal resistance of 10 KΩ was connected with the NCEG. A long-term stability measurement shows that the NCEG can work steadily for 80 hours with a negligible output V_OC decay (Fig. 4c). Moreover, airflow disturbances and varied light environment have limited influence on the voltage outputs of the NCEG (Supplementary Fig. 7). To measure the scalable performance of the NCEG, one, two, and three NCEG units were connected in series connection and output voltages of ~ 1.0 V, ~ 1.8 V and ~ 2.9 V, can be obtained, respectively (Fig. 4d). Similarly, the short-circuit current increased to ~ 0.4 mA with three cells connected in parallel (Fig. 4e). With further increasing the number of devices in series to fourteen, an output voltage of ~ 10 V can be achieved (Supplementary Fig. 8) and a linear relationship between series number and output voltage were obtained (Fig. 4f). With three NCEG units connected in series, an electronic timer can be powered as shown in inset of the Fig. 4f. Compared with the reported hydroelectric devices, the NCEG presents a huge advantage on the current density resulting from the Coulomb drag effect (Supplementary Table S1).

In this work, a NCEG that can achieve a milliampere-level current output was designed by sandwiching a CNTM between two metal electrodes. It has been demonstrated that the redox reactions between active metal and oxygen provide sufficient power to drive ionic flow within the nanochannels in the CNTM. Meanwhile, the theory that Coulomb drag induced by the movement of ions in the nanochannels can be used to amplify the current output is validated. The developed NCEG device exhibits constant and stable electrical output with high environmental tolerance, achieving an output power density of 74 µW·cm^− 2. We anticipate that this approach of amplifying the current output of NCEG not only enhances our fundamental understanding of energy harvesting principle in nanofluidic systems but also facilitates the development of new-generation energy generators in practical applications.

Materials:

The anodic aluminum oxide AAO membranes with a thickness of 60 µm, a top pore size of 200 nm, and a bottom pore size of 30 nm were purchased from Sterlitech Corporation, Germany. Different metal electrodes (Al, Zn, Cu, Fe, and Au) were purchased from Taizhou Sennuo Material Technology Co. Ltd, China. The aluminum base conductive carbon tape (Nissin SEM double-sided carbon conductive tape) and non-woven substrate conductive carbon tape (conductive carbon fiber cloth) were purchased from Guangzhou Li-ge Technology Co, Ltd, China. Acetonitrile was purchased from J&K Scientific China.

Fabrication of nitrogen-doped CNTM:

An asymmetric porous AAO membrane was used as a template to fabricate the CNTM through the conventional chemical vapor deposition (CVD) process. In the CVD process, acetonitrile was employed as the carbon source precursor. Typically, the AAO substrate was first placed into the horizontal growth chamber of a standard atmospheric pressure CVD system. To conduct a reduction treatment on the AAO substrate, the temperature of the chamber was heated up to 1000°C with a gas mixture (Ar, 100 standard cubic centimeters per minute, sccm and H₂, 50 sccm) for 0.5 h. Afterward, the carbon precursor was introduced to implement the growth step with a humidified acetonitrile bubbler. After 1.0 h of growth, the system was cooled down to room temperature under Ar protection.

Design of NCEG:

The NCEG device was simply built by attaching two electrodes on the upside and downside of the CNTM, respectively. Typically, aluminum-based conductive carbon tape (Nissin SEM double-sided carbon conductive tape) was used as the bottom electrode, and Au works as the top electrode. To investigate the effect of the potential difference in the redox reactions process, various materials, including Al, Zn, Cu, Fe, Au, and conductive carbon fiber cloth were used as the bottom electrode.

Characterizations:

Scanning electron microscope (SEM) (Hitachi-SU8220) was used to characterize the morphologies of AAO substrate and CNTM grown of AAO template. X-ray photoelectron spectroscopy (XPS) (PHI 5000 VersaProbe, ULVAC-PHI, Inc) was used to analyze the surface element composition of CNTM and AAO. X-ray energy dispersion spectroscopy (EDS) (OXFORD X-Max 80) was used to characterize the elemental composition of the CNTM before and after electrical output measurement.

Electrical output measurement:

The open-circuit voltage (V_OC) and the short-circuit current (I_SC) of the device were recorded using the digit multimeter (Keithley DMM7510). To confirm the source of the voltage output signal, the positions where the electrolyte solution contacted the CNTM were manipulated and the corresponding voltage output was recorded. To explore the important role of the ionic flow within nanochannels in the current amplification, the currents with and without ionic flow were compared. Since the chemical voltage on the NCEG only generates when the electrolyte solution contacts with the CNTM, a waveform generator (SDG1000X, Shenzhen Dingyang Technology, China) was applied to provide external bias voltage, including ± 0.1 V, ± 0.3 V, ± 0.5 V, ± 0.7 V, ± 1 V, ± 1.5 V, and ± 2 V. The top and bottom electrodes in the NCEG device were both replaced as gold electrodes to get rid of the voltage generated by the chemical difference. The currents of the NCEG with and without the contact of electrolyte solution (0.1 M NaCl) were compared following the equation:

$$\varDelta {J}_{SC1} \left(mA·{cm}^{-2}\right)={J}_{SC-electrolyte}-{J}_{SC-without electrolyte}$$

$$={(I}_{electrolyte}-{I}_{without electrolyte})/S$$

where the I_electrolyte is the real-time current when the electrolyte contacted the device, I_{without electrolyte} is the real-time current when the device connected to the circuit at the corresponding external voltage without electrolyte, and S = 0.25 cm^− 2 is the working area of the device. To further explore the effect of the circuit current on the current amplification, the circuit current on the NCEG device was adjusted via loading different electrical resistances, including 100, 500, 1000, 3000, 5000, and 10000 Ω. The theoretical current of the circuit with different loads of resistances can be calculated based on the equation below:

$${J}_{SC-theoretical} (mA·{cm}^{-2})=\frac{U}{{R}_{S}+{R}_{L}}/S$$

Where U = 0.8 V is the average voltage output of the NCEG device, R_S = 10000 Ω is the internal resistance of the device, determined by the maximum power output when the external resistance is equal to the internal resistance (Fig. 4a), and the R_L is the load resistance. To exhibit the significance of Coulomb drag in the nanochannels, the differences between the measured current and the theoretical current were calculated following the equation:

$$\varDelta {J}_{SC2} (mA·{cm}^{-2})={{J}_{SC-measured}-{J}_{SC-theoretical}=(I}_{measured}-\frac{U}{{R}_{S}+{R}_{L}})/S$$

Where I_measured is the current measured.

Data availability

All data generated or analyzed during this study are included in the paper and its Supplementary Information, and from the corresponding author on request.

Acknowledgments

We acknowledge the help from Xiaoliu Wen in drawing the schemes including Figures 1a, 2a, and 3d. This work was financially supported by the National Key Technologies R&D Program of China （Grant No. 2023YFC2415900）, the National Natural Science Foundation of China(No.22275079), Shenzhen Science and Innovation Committee (20220815164834003), Shenzhen Science and Technology Program (KQTD20221101093559017), Guangdong Provincial Key Laboratory of Advanced Biomaterials (2022B1212010003) and Starting Grant from Southern University of Science and Technology (SUSTech). We also acknowledge the assistance of technical support from SUSTech Core Research Facilities.

Author contributions

K.X. conceived and supervised the project. Y. S. J. and T. W. designed the experiments, discussed the results, and wrote the paper. Y. S. J. fabricated devices, carried out experiments, and performed data analysis. W. C. L. explored and directed the synthesis of CNTM material samples. All authors analyzed the data and discussed the results.

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published 03 Oct, 2024

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A nanofluidic chemoelectrical generator with enhanced energy harvesting by ion-electron Coulomb drag

Status:

Journal Publication

Version 1

Abstract

Figures

Introduction

Results and Discussions

Schematic and electrical output characteristics of NCEG

The origin of the output voltage signal

Current amplification via ion-electron Coulomb drag

Enhanced output energy power and application

Conclusions

Materials and Methods

Materials:

Fabrication of nitrogen-doped CNTM:

Design of NCEG:

Characterizations:

Electrical output measurement:

Declarations

References

Additional Declarations

Supplementary Files

Status:

Journal Publication

Version 1