A novel Cu-Cu2O hetero-structure for ultrasensitive detection of dopamine

doi:10.21203/rs.3.rs-3901267/v1

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A novel Cu-Cu2O hetero-structure for ultrasensitive detection of dopamine

https://doi.org/10.21203/rs.3.rs-3901267/v1

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published 20 Aug, 2024

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Herein, Cu-Cu₂O heterostructure were grown in situ on the surface of Cu nanoplates by chemical etching at room temperature. A novel dopamine (DA) electrochemical sensor based on Cu-Cu₂O/glass carbon electrode (Cu-Cu₂O/GCE) was constructed. The Cu-Cu₂O/GCE sensor showed a wide linear range of 0.001 mM to 2 mM and a low limit of detection (LOD) of 7.1 nM (S/N = 3) for DA. The improved performance of the Cu-Cu₂O/GCE is attributed to the special void structure which increases the catalytic active sites and electrochemical active surface areas (ECSA). Besides, the optimization of Cu₂O and Cu ratio effectively regulates the electron configuration of the Cu-Cu₂O heterojunction. The Cu-Cu₂O/GCE sensor also showed good reproducibility, stability, and excellent anti-interference ability.

Cu-Cu2O heterostructure

void structure

Chemical etching

Sensor

Dopamine

Dopamine (DA) is an important catecholamine neurotransmitter that exists in the brain and peripheral nervous system(Amani et al. 2022; Lakshmanakumar et al. 2021; Liu et al. 2020; Tavakkoli et al. 2019; Wang et al. 2023b; Zhou et al. 2023). Abnormal levels of DA can lead to various neurodegenerative diseases, such as Parkinson's disease, Huntington's disease, schizophrenia, and epilepsy have been reported to mediate HIV replication in human macrophages(He et al. 2022; Lakard et al. 2021). To diagnose, prevent, and treat DA-related neurological diseases, the sensitive detection of DA is of great significance. Among various measurements, such as liquid chromatography-tandem mass spectrometry, capillary electrophoresis, high-performance liquid chromatography, and electrochemical analysis, the electrochemical sensor has the potential to become an ideal and reliable technique for rapid recognition and real-time detection of DA due to easy operation, fast response, high sensitivity, and even in-real detection(Al-Graiti et al. 2017; Cogal 2020; Cogal et al. 2021; Mani et al. 2016; Tang et al. 2022b).

Nanomaterials, such as carbon materials, noble metal materials, metal oxide, metal sulfide, metal hydroxide, hydrogel, et al. as catalytic active substances were widely used to fabricate electrochemical sensors(Du et al. 2023; Hatala et al. 2021; Li et al. 2022a; Suhito et al. 2019; Tang et al. 2022a; Xu et al. 2023a; Xu et al. 2023b). Among them, Cu-based nanomaterials have been attracting more interest due to their rich content, low cost, high conductivity, and excellent catalytic activity(Xu et al. 2022). Besides, Cu as a sacrificial template to fabricate a metal-semiconductor interface hybrid structure is an effective route to develop a novel precious metal-free sensor(Yuan et al. 2021). Cu_xS and Cu₂O are usually used as Cu-based semiconductor materials with excellent performance. G. Xu et al. fabricated a dendritic Cu-Cu₂S nanostructure successfully, which exhibited good performance in the determination of glucose(Xu et al. 2019). Unfortunately, Cu_xS has different compositions (CuS, Cu₃₁S₁₆, Cu₉S₈, Cu₇S₄, Cu₂S, etc.), which is hard to control composition and purity(Soosaimanickam et al. 2020), while Cu₂O is a kind of p-type semiconductor with narrow band gap ( 2.0 ~ 2.2 eV) and has attracted much attention in sensors(Gupta et al. 2018; Liu et al. 2022a; Xu et al. 2019; Zhang et al. 2011). Wu et al. fabricated Cu₂O HMS/CB/GCE sensor in Deep Eutectic Solvents, which exhibited excellent electrocatalytic activity for DA oxidation(Wu et al. 2015). M. Devaraj et al. constructed Cu/Cu₂O nanoparticle sensor that exhibited excellent electrochemical enhancement due to the coexistence of Cu₂O with more reactive sites, which promotes the oxidation of DA(Devaraj et al. 2016). However, Cu₂O is generally produced by oxidizing Cu at higher synthesis temperatures, making the shape and degree of oxidation difficult to control.

Herein, the Cu nanoplates with two-dimensional structures were used as templates and corroded in NaOH solution to obtain Cu-Cu₂O heterostructure nanoplates at room temperature. The effect of NaOH concentration on the morphology of Cu-Cu₂O heterostructure on the surface of Cu nanoplates was studied. Thanks to the porous structure of Cu-Cu₂O, the prepared Cu-Cu₂O/GCE sensor was able to effectively quantitatively detect the DA.

2.1 Chemical reagents

Sodium hydroxide (NaOH, 99%), dopamine hydrochloride (C₈H₁₁NO₂·HCl, 98%), uric acid (C₅H₄N₄O₃, 99%), disodium hydrogen phosphate (Na₂HPO₄, 99%), sodium dihydrogen phosphate (NaH₂PO₄, 99%), hydrogen peroxide solution (H₂O₂, 30%), ascorbic acid (C₆H₈O₆, 99%), glucose (C₆H₁₂O₆, 99%), sodium chloride (NaCl, 99.99%), and Nafion solution were purchased from Innochem. The 0.2 M PBS with a pH of 7.4 was prepared with NaH₂PO₄ and Na₂HPO₄. Cu nanoplates were lab-made.

2.2 Synthesis of Cu-Cu₂O nanoplates

Cu nanoplates were produced using the seed-assisted hydrothermal process(Xu et al. 2022) and then completely submerged in 5 mL of NaOH solution at different concentrations (including 0.1 M, 0.3 M, 0.6 M, and 1 M) with stirring for 10 min for the etching reaction at room temperature. After a slight darkening of the color was observed, the products were separated by centrifugation with water until the pH was neutral. Finally, the cleaned products Cu-Cu₂O nanoplates were redispersed into 200 µL of water.

2.3 Electrochemical detection of DA

7 µL of Cu-Cu₂O nanosuspension was dropped on the pretreated GCE, dried at room temperature, and then covered with 5 µL of Nafion solution on the surface of the electrode and evaporated for 20 min to obtain Cu-Cu₂O/GCE.

2.4 Material characterization

The morphology of Cu-Cu₂O nanoplates was observed by scanning electron microscopy (SEM, Zeiss Gemini 300, Oberkochen, Germany). The crystal structure of Cu-Cu₂O nanoplates was analyzed by X-ray diffraction (XRD, Bruker D8, Karlsruhe, Germany). The electrochemical performance of working electrodes was carried out on a CHI 660e electrochemical workstation (Shanghai Chenhua Inc., China). The electrochemical performance of Cu-Cu₂O/GCE on the detection of DA was evaluated by conventional electrochemical techniques including cyclic voltammetry (CV), differential pulse voltammetry (DPV), and chronoamperometry i-t Curve (i-t).

Scheme 1 illustrates the typical synthetic process of Cu-Cu₂O nanoplates and the electrochemical detection of DA. The Cu nanoplates were synthesized by Ag seed-assisted hydrothermal method in a water bath at 90 ℃ (Xu et al. 2022). Then the washed Cu nanoplates were injected into a NaOH aqueous solution and stirred at room temperature. The surface of Cu nanoplates started to be corroded under alkaline conditions and the Cu₂O nanoplates were also produced simultaneously. Eventually, Cu-Cu₂O nanoplates were synthesized successfully. Finally, the electrochemical detection of DA was performed at electrochemical workstation.

3.1 Characterization of Cu-Cu₂O nanoplates

The morphologies and composition of Cu-Cu₂O nanoplates were detected by SEM and XRD as shown in Fig. 1. Figure 1a shows the SEM image of Cu nanoplates, which has a smooth surface with a size between 1 and 15 µm. In comparison, Cu nanoplate is covered with a crossed array nanosheets (Fig. 1b). Furthermore, these nanosheets construct porous surface structures, which can effectively increase the ECSA. Figure 1(c, d, e) shows the HAADF-STEM elements mapping, Cu and O elements. It can be seen that O not only exists on the surface of Cu but whole region, and the EDS information in Figure S1 (Supporting Information) shows that a large amount of O exists in the Cu-Cu₂O nanoplates, which indicates that a large amount of Cu₂O obtained, rather than the oxidation of surface copper by oxygen in the air. Figure 1f shows the XRD patterns of Cu nanoplates before and after corrosion. The red XRD pattern shows only a stronger peak at 2θ of 43.40^օ, which is contributed to facet (111) of Cu (Cubic, JCPDS No. 04-0836)(Devaraj et al. 2016; Xu et al. 2022; Yin et al. 2022), and the black XRD pattern shows a new peak at 2θ of 36.43^օ, which is attributed to the facet (111) of Cu₂O (Cubic, JCPDS No.05-0667)(Chen et al. 2015; Zhang et al. 2021). The characteristic Cu₂O peak was found in the etched sample, which indicates that Cu-Cu₂O nanoplates were synthesized successfully. Furthermore, Fig. 1g shows the XPS spectra of Cu 2p exhibits peaks at 932.9, 934.2, 952.5, and 954.1 eV, which are attributed to Cu 2p_3/2 and Cu 2p_1/2 peaks including metallic Cu and Cu(I) from Cu₂O. The peaks at 932.9 and 952.5 eV are attributed to metallic Cu(0), while 934.2 and 954.1 eV are associated with the Cu(I) chemical state in Cu₂O(Bai et al. 2018; Liu et al. 2022b; Wang et al. 2023a; Zhang et al. 2021; Zhong et al. 2019). The two satellite peaks are situated at 943.3 eV and 962.3 eV(Lyu et al. 2021; Yang et al. 2021a). The XPS results further indicate that Cu₂O exists in the etched sample.

The effects of NaOH solution on the morphology and composition of Cu-Cu₂O nanoplates were discussed in Fig. 2. Significant change was observed at the periphery of Cu nanoplates, with 0.1 M NaOH solution, where the small nanoplates were grown in situ (Fig. 2a), and the correlative XRD pattern in Fig. 2b shows a weak characteristic Cu₂O peak. When the concentration increases to 0.3 M, the surface of Cu nanoplates is almost covered with more small nanosheets (Fig. 2c), which cross each to form a crossed array of nanosheet structures. The stronger intensity of Cu₂O peak investigating that more Cu₂O generated (Fig. 2d). When the 1.0 M concentration, the pore size becomes larger and the structure of nanoplates is damaged (Fig. 2e), which is attributed to terrible corrosion. Meanwhile, more Cu₂O forming can be confirmed by the XRD pattern in Fig. 2f.

3.2 Electrochemical characterization of Cu-Cu₂O nanoplates

The electrochemical oxidation reaction of DA on bare naked GC and Cu-Cu₂O/GCE electrodes was measured by CV scanned in a saturated PBS solution (pH = 7.4) (Fig. 3a). The black and blue curves represent the GCE and Cu/GCE, respectively, which show a pair of redox peaks only in the Cu/GCE due to the chemical reaction of Cu (Gu et al. 2020; Li et al. 2018). By contrast, the green CV curves show a new oxidation peak at 0.245 V due to the electrocatalytic oxidation of DA(Devaraj et al. 2016). Compared with Cu/GCE, the response current of Cu-Cu₂O/GCE to DA (red curve) increases by 6 times, which indicates that the addition of Cu₂O can effectually enhance the electrocatalytic activity. Figures 3b and 3c show DPV curves and response currents of various Cu-Cu₂O/GCE to investigate the influences of NaOH concentration. As a result, the Cu-Cu₂O nanoplates obtained in 0.6 M solution show the best catalytic activity. Therefore, an appropriate amount of Cu₂O can effectively enhance the electrocatalytic activity of Cu-Cu₂O nanoplates. Furthermore, the kinetic characteristics of DA oxidation on Cu-Cu₂O nanoplates were investigated. Figure 3d shows that the peak current values at a potential of 0.23V gradually increased with the scanning rate from 20 to 70 mV/s. A good linear relationship between the peak current value and scanning rate was obtained by using linear fitting (Fig. 3e) and expressed by I_pa = 477.15v^1/2 + 41.37 (R² = 0.9990), indicating that the electrocatalytic oxidation of DA on the surface of Cu-Cu₂O/GC is a diffusion-control process(Devnani et al. 2019). In addition, the oxidation peak potential also gradually shifts to a positive direction and also has a linear relationship with the logarithm of the scanning rate (Fig. 3f), which can be described by the equation of P_ox = 0.029lnv + 0.386 (R² = 0.9881). According to the equation:

E = E^o + (RT/αnF)ln(RTk^o/αnF) + (RT/αnF)lnv (1)

T, R, k^o, E^o, F represent the Kelvin temperature (K), ideal gas constant (8.314 J/(mol·K)), the inhomogeneous electron transfer rate, the formal potential (V), the Faraday constant (96480 C/mol), respectively, and α is usually 0.5 in a quasi-reversible process. Then, n is calculated to be 1.77, which is approximately 2, showing that the electrochemical oxidation reaction of DA is a quasi-reversible process of double electron transfer(Li et al. 2022b).

For quantitative analysis of DA, the DPV curves of Cu-Cu₂O/GCE with various concentrations were detected. As shown in Fig. 4a, the peak current value (P_ox) increases with the increase of DA concentration, indicating a preferable sensibility of Cu-Cu₂O/GCE to DA. Besides, Fig. 4b demonstrates that the P_ox has a good linear relationship with the concentration, which can be expressed as I (µA) = 58.03C_DA + 7.389 with R² value of 0.9936. The corresponding LOD is calculated to be 7.1 nM (S/N = 3). Compared with the recent research works of Cu-based/GCE on DA (Table S1: Supporting Information), the developed Cu-Cu₂O/GCE shows a better performance with a lower detection limit (7.1 nM) in the concentration range of 0.001-2 mM. The anti-interference performance is another important property for electrochemical sensor, which was evaluated by I-t curve method. DA and other interfering substances were injected into the PBS solution in turn at 0.25 V and the I-t curve was recorded (Fig. 4c and 4d). The current value increases immediately with the addition of DA and reaches stability during 3 seconds, investigating that Cu-Cu₂O/GCE has an excellent sensitivity and stable signal to DA. The interfering substances, such as NaCl, H₂O₂, uric acid (UA), and glucose (Glu) are added, which concentration is 10 times than DA, while the current value has no significant changes. A minor increase in current value was found in the case of (limiting amino acids) L-AA, which can be ignored due to the high concentration of L-AA compared with DA. Interference results show that Cu-Cu₂O/GCE has high anti-interference performance for the determination of DA.

Repeatability and long-term stability are two important properties of electrochemical sensors. To evaluate the repeatability of Cu-Cu₂O/GCE, four parallel experiments have been used, which show no significant change and these current values obtained around 140 µA, with a 3.6% relative standard deviation (Fig. 5ab), which shows good repeatability. Besides, the cycle tests were applied to evaluate the stability. Figures 5c and 5d showed that the current value only decreases by 4.7% after 50 cycles, which indicates good stability.

3.3 Discussion of the mechanism

In the above results, for the reversible reaction, the number of electrons was calculated as approximately 2 according to the equation proposed in the literature(Li et al. 2022b), and the possible reaction mechanism is shown in Figure S2 (Supporting Information).

As we all know, the ESCA and active sites are the key factors for the sensor to detect the target detection object. A larger ESCA can generate more active sites to catalyze the oxidation-reduction reaction of the target detection object better and faster(Li et al. 2023; Yang et al. 2021b). It is observed from Fig. 1 that the nanosheets in Cu-Cu₂O obtained after etching are much smaller than those in Cu, which greatly increases the ESCA and active sites. Moreover, the surface of Cu-Cu₂O becomes extremely rough, which leads to the appearance of many micropores, which is more conducive to the mass transfer rate of DA, and further accelerates the oxidation reaction of DA, which is the first reason for the excellent detection performance of Cu-Cu₂O nanosheets.

Moreover, it is found that in the combination of Cu/Cu₂O, electrons in Cu₂O are usually transferred to Cu, which makes the Cu₂O component in the combination of Cu/Cu₂O often in an “electron-deficient” state(Ma et al. 2024; Zhu et al. 2020). Therefore, the production of Cu₂O is conducive to the transfer of electrons on dopamine to the vicinity of electron-deficient Cu₂O, which is conducive to the oxidation reaction of dopamine. However, the production of too much Cu₂O will inevitably lead to the transfer of too many electrons to the vicinity of Cu, which weakens the oxidation of dopamine near Cu. Therefore, controlling the ratio of Cu₂O in Cu/Cu₂O is the key. We just optimized the concentration of NaOH in the process of etching Cu which makes the ratio of Cu₂O in Cu/Cu₂O obtained by us conducive to the improvement of detection performance. Certainly, in the Cu/Cu₂O combination, the electron transfer problem and the ratio problem between Cu₂O and Cu need more detailed mechanism research, which is the direction of our follow-up efforts.

In this study, Cu-Cu₂O nanoplates were developed utilizing a chemical etching technique with the sacrificial templates Cu nanoplates. The constructed Cu-Cu₂O/GCE showed excellent detection and anti-interference performance in the electrochemical detection of DA with a linear current response in a wide range of 0.0001-2 mM with an LOD of 7.1 nM. The improved performance of the Cu-Cu₂O/GCE sensor is attributed to the special structure which increases the catalytic active sites and ECSA. Besides, the optimization of Cu₂O and Cu ratio effectively regulates the electron configuration of the heterojunction. This sensor enables the quick, easy, and selective detection of DA while also providing a novel platform for biosensor applications.

Supplementary Information

The online version contains supplementary material available, including EDS date (Fig.S1), the proposed mechanism of electrochemical oxidation of DA(Fig.S2), and table for comparison of different modified electrodes(Tab. S1)

Declaration of Conflict of interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments:

This research was funded by the National Natural Science Foundation of China (grant numbers：U23A20138 and 52374387) and the Science and Technology Project of Changsha City (kh2201380)

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Scheme 1 is available in Supplementary Files section.

floatimage1.png
Scheme 1. Schematic diagram of preparation of Cu-Cu₂O nanoplates.
Chemcialpapersupportinginformation.doc
The online version contains supplementary material available, including EDS date (Fig.S1), the proposed mechanism of electrochemical oxidation of DA(Fig.S2), and table for comparison of different modified electrodes(Tab. S1)

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A novel Cu-Cu2O hetero-structure for ultrasensitive detection of dopamine

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental Method

2.1 Chemical reagents

2.2 Synthesis of Cu-Cu₂O nanoplates

2.3 Electrochemical detection of DA

2.4 Material characterization

3. Results and Discussion

3.1 Characterization of Cu-Cu₂O nanoplates

3.2 Electrochemical characterization of Cu-Cu₂O nanoplates

3.3 Discussion of the mechanism

4. Conclusion

Declarations

References

Scheme

Supplementary Files

Status:

Journal Publication

Version 1

A novel Cu-Cu2O hetero-structure for ultrasensitive detection of dopamine

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental Method

2.1 Chemical reagents

2.2 Synthesis of Cu-Cu2O nanoplates

2.3 Electrochemical detection of DA

2.4 Material characterization

3. Results and Discussion

3.1 Characterization of Cu-Cu2O nanoplates

3.2 Electrochemical characterization of Cu-Cu2O nanoplates

3.3 Discussion of the mechanism

4. Conclusion

Declarations

References

Scheme

Supplementary Files

Status:

Journal Publication

Version 1

2.2 Synthesis of Cu-Cu₂O nanoplates

3.1 Characterization of Cu-Cu₂O nanoplates

3.2 Electrochemical characterization of Cu-Cu₂O nanoplates