Hydrothermally synthesized Nickel cobalt oxide for bifunctional electrochemical supercapacitor and nonenzymatic glucose biosensor

doi:10.21203/rs.3.rs-1098022/v1

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Hydrothermally synthesized Nickel cobalt oxide for bifunctional electrochemical supercapacitor and nonenzymatic glucose biosensor

https://doi.org/10.21203/rs.3.rs-1098022/v1

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Herein, various nickel cobalt oxide nanostructures with different Ni concentrations are prepared via hydrothermal route and then calcination process for electrochemical supercapacitor as well as nonenzymatic glucose biosensor. The electrode synthesized on carbon cloth using Ni_0.9Co_2.1O₄ nanosheet-like morphology showed a maximum 516.51 F g⁻¹ specific capacitance at 10 mV s⁻¹ scan rate and the cyclic stability of 87.7% over 2000 GCD cycles. The electrode prepared with Ni_0.3Co_2.7O₄ on CC offered a linear response from 0 to 0.3 mM glucose concentration and exhibited a maximum of 759.5 µA mM⁻¹ cm⁻² glucose sensitivity.

Biophysics

Hydrothermal

Nickel cobalt oxide

Supercapacitor

Nonenzymatic glucose sensing

Nowadays, human beings have suffered from problems such as deficiency of fossil fuels, global warming, and pollution. Hence, it is essential to produce energy from renewable sources Like solar, tide, and wind. Also, low-cost, environmentally friendly, advanced energy storage and conversion devices must store energy harvested from renewable resources ^1–4. There are different energy storage devices such as conventional capacitors, biofuel, lithium ions batteries (LIBs), and supercapacitors ^5–9. Supercapacitors, also called electrochemical supercapacitors, are the most desirable candidates for energy storage. Their unique electrochemical properties like high power density, excellent coulombic efficiency, and high cyclic stability make them compatible with other energy storage devices. Still, supercapacitors suffered from low energy density as compared to LIBs. So, to improve the energy density of supercapacitors, efforts have been made to develop novel electrodes with suitable synthesis strategies ^10–14.

The different conducting polymers ¹⁵, transition metal oxides, and transition metal hydroxides such as Co₃O₄¹¹_,NiO ¹⁶, Co(OH)₂¹⁷, Ni(OH)₂¹⁸, RuO₂¹⁹, MnO₂²⁰ has been widely studied as an electrode for pseudocapacitors. The transition metal oxides deliver higher specific capacitance as compared to conducting polymers due to multi-electron redox reactions. In addition, ternary metal oxides, because of their better electrical conductivity and rich redox-active sites, shows better supercapacitor performance than single metal oxide ²¹. Spinel nickel cobalt oxide (NiCo2O4) has been widely used as high-performance capacitive electrode material in recent years. It shows better electrical conductivity, relatively lower electron transport activation energy, and better electrochemical activity than cobalt oxide (Co₃O₄)and nickel oxide (NiO) ^22,23. This high electrical conductivity and improved specific capacitance of NiCo₂O₄are because of contributions from both the Co and Ni ions with diverse valence states.

Researchers have made many efforts to enhance electrochemical performance by developing nickel cobalt oxide with different morphologies. Waghmode et al. ²⁴ synthesized NiCo₂O₄ nanoflowers by chemical bath deposition method and observed capacitance was 610 F g^-1at 1 mA cm^-2. Ma et al.²⁵, with the solution precursor thermal spray method, developed NiCo₂O₄hollow microspheres, which showed specific capacitance 902 F g^-1at 1 A g^-1. Qi et al. ²⁶ synthesized NiCo₂O₄hollow microspheres by a hydrothermal method which showed specific capacitance 720 F g^-1at 2 A g^-1. Saravanakumar et al. ²⁷ synthesized NiCo₂O₄ nanoparticles via hydrothermal route and observed specific capacitance was 294 F g^-1at 1 A g^-1. Uke et al. ²⁸ synthesized NiCo₂O₄ nanomorphs by hydrothermal method and observed specific capacitance was 479 F g^-1 with better retention.

In the medical industries, quality control in food and clinical diagnosis of diabetes; rapid, accurate, and sensitive detection of glucose is essential ^29,30. Recently, sensitive and selective enzyme-based sensors have been studied for glucose sensing. But, they cannot be reused for continuous glucose detection. They suffer from low stability, which limits their use in actual application ^31,32. The other method, i.e., nonenzymatic glucose biosensing, exhibited high stability, sensitivity, and reproducibility. Qin et al.³³ developed NiCo₂O₄ nanowires with the help of hydrothermal and calcination treatment. The prepared glucose sensor shows 72.4 mM mM^-1 cm^-2 glucose sensitivity and 0.37 mM detection limit. Hussain et al. ³⁴ prepared NiCo₂O₄ nanoneedles on Nickel Foam exhibited a sensitivity of 91.34 mV/decade with a response time less than 10 s. Yang et al. ³⁵ synthesized hollow nanorods of NiCo₂O₄ with the help of sacrificial template accelerate hydrolysis method achieved 1685.1 mM mM^-1cm^-2 glucose sensitivity. Ma et al. ³⁶ developed NiCo₂O₄ nanowrinkles on graphene oxide sheets with hydrothermal route achieved glucose sensitivity of 548.9 mM mM^-1 cm^-2.

In the present investigation, the different nickel cobalt oxide nanostructures by varying concentrations of Ni in cobalt oxide are prepared by the hydrothermal route and studied for both supercapacitor and glucose biosensing applications. The electrodes are synthesized using a flexible carbon cloth (CC) current collector with a simple doctor blade method. The synthesized Ni_0.9Co_2.1O₄nanosheets exhibited 516.51 F g^-1specific capacitance at 10 mV s^-1 with capacity retention of 87.7% over 2000 cycles. At the same time, Ni_0.3Co_2.7O₄nanosheets showed maximum 759.5 µA mM^-1 cm^-2glucose sensitivity with^alinear response from 0.0 to 0.3 mM glucose concentration.

A. Preparation of different Nickel cobalt oxide powders:

The nickel cobalt oxide powders with different Ni percentages were synthesized by the hydrothermal route and then calcination. In a synthesis of Co₃O_4, 0.1 M Co(NO₃)₂ 6H₂O and 0.2 M of urea were added in Double distilled water (DDW). NH₃ was added to the solution dropwise up to pH = 11 and stirred for 30 min. Afterward, the whole solution was poured into a Teflon liner (100 mL), fitted in stainless-steel autoclave and reaction carried out at 180°C for 18 h. Then, the autoclave was cooled to room temperature, and reaction products were cleaned with DDW and ethanol many times and dried at 60 °C oven for 12h. Lastly, the prepared powder was calcinated at 400°C for 2 h. Similarly, powders with different Ni concentrations were synthesized by adding a different percentage of Ni as 0%, 10%, 20%, 30%, and 40% in Co₃O₄. Based on the various percentages of Ni precursor, the stoichiometries are observed Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O_4, respectively.

B. Preparation of electrode

In an ultrasonication bath, a piece of CC (2 cm ´ 1 cm) was cleaned with ethanol, acetone, and DDW each for 10 min respectively, and dried overnight at 60 °C in the oven. The actual electrode was prepared by mixing prepared powders (active material), PVDF as a binder, and a carbon black ratio of 80:10:10. Then sufficient amount of NMP solvent was mixed to obtain a uniform slurry. Then the prepared slurry was coated on CC (1 cm 1 cm) and subjected to 80 °C in a hot air oven for 12 h. These prepared electrodes were used for electrochemical supercapacitor and nonenzymatic glucose biosensor study. The experimental procedure can be presented in Fig. 1.

XRD pattern of prepared powders recorded using a Bruker D2 phaser tabletop model under Cu Ka radiation. FTIR was taken by Lambada-7600, Australia. The morphology was analyzed using FE-SEM from the Mira-3, Tescan, Brno-Czech Republic. Biologic SP-300 electrochemical workstation used for electrochemical supercapacitor and glucose biosensor study.

3.1 XRD study

Fig. 2 (A) presents the XRD spectra of different Nickel cobalt oxide nanostructures. The observed d-spacing values in XRD spectra are associated with standard JCPDS card 01-080-1543 for Co₃O₄and 01-073-1702 after adding different Ni concentrations. The peaks are observed at an angle, 64.98, 59.19, 44.68, 36.79, 31.16,18.94° which applied to the cubic structure and assigned to the (440), (511), (400), (311), (220), and (111) crystal planes respectively. The crystallite size is calculated by using Scherer's formula ^7,37. The calculated values for average crystallite size are 34.18, 36.61, 43.10, 30.96, and 34.18 nm for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O_4, respectively.

3.2 FTIR study

The different Nickel cobalt oxide powders were further characterized by the FT-IR study. Fig. 2 (B) presents the FTIR spectra of all synthesized nickel cobalt oxidepowders. The FTIR spectra display two sharp peaks at about 661 cm^-1 and 565 cm^-1 which are originated from Co-O bonds (stretching vibrations), confirms the formation of Co₃O₄^38,39. As the percentage of Ni increases, these two peaks shift towards a higher wavenumber. The corresponding change in the peak is mentioned in supplementary information Table S1. The relatively weak peaks at about 1632 and 3432 cm^-1 are associated with O-H bending and stretching mode of vibration of water ^40–42.

3.3 FE-SEM study

Fig. 3 shows FE-SEM pictures and EDS analysis of different nickel cobalt oxide powders. The Co₃O₄ in Fig. 3 (A) shows nanosheets like nature. As the different percentages of Ni are added into Co₃O₄,surface modifications are observed. In Fig. 3 (B), the nanosheet-like morphologies are observed, which are merged. As the percentage of Ni increases, the nanosheets are incorporated a lot in Fig. 3 (C). The flakes are started covered with nanoparticles in Fig. 3 (D), and finally, the number of nanoparticles increased as shown in Fig. 3 € corresponding to the Ni_1.2Co_1.8O₄. Fig. 3 (F) shows the EDS spectra of Ni_1.2Co_1.8O_4, which confirms the presence of Ni, Co, and O. Fig. 3 (G-I) presets the elemental distribution of Ni, Co, and O, respectively.

3.4 EIS study

The electrochemical behavior at the electrode-electrolyte interface was studied by using the EIS study. Fig. 4 presents the EIS study of synthesized Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes. EIS spectra were recorded within 1 MHz to 0.1 Hz frequency range in 1 M KOH electrolyte at applied potential 20 mV. Fig. 4 (A) presents the Nyquist plots of Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄electrodes. The Inset of Fig. 4 (A) shows the corresponding fitted circuit diagram. The solution resistance (R_s) values estimated from Nyquist plot for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄electrodes are 0.08, 0.37, 0.36, 0.02, and 0.15 W cm^-2.The charge transfer resistance values for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄electrodes are 88.81, 91.51, 109.10, 79.51, and 90.47 W cm^-2 respectively. The lower R_ct and R_svalues reveal the better electrical conductivity and good adhesion of coated material with current collector ⁴³. The different EIS parameters are mentioned in supplementary information Table S2. Fig. 4 (B) presents the Bode plot of Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄electrodes, respectively.

3.5 Electrochemical supercapacitor study

The three-electrode system with SCE as a reference electrode, platinum wire counter electrode, and preparedCC electrodes as a working electrode is used to study electrochemical supercapacitor performance. The electrochemical performance is studied in 1 M KOH electrolyte.

Fig. 5 A presents the cyclic voltammetry (CV) curves of all nickel cobalt oxide electrodes studied at a 10 mV s^-1 scan rate_. The maximum capacitance values estimated from CV curves are 189.31, 204.22, 220.63, 516.51, and 312.32 F g^-1 for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes, respectively. All CVs, along with different scan rates, are mentioned in Fig. S1 (A-E). From the graphs in Fig. S1, it is clear that with an increase in scan rate, the area under the curve increases as the current drawn increases with the voltage in the CV graph. But the increase in scan rate limits the interaction time between electrolyte and electrode. This limited-time interaction between electrode and electrolyte also limits the utilization of the active surface area of the electrode. Hence specific capacitance decreases with the increase of scan rate ⁴⁴.

The galvanostatic charge-discharge curves are displayed in fig. 5 B of different nickel cobalt oxideelectrodes studied at current density 3 mA cm^-2. The maximum specific capacitance values estimated from GCD curves are 89.10, 101.27, 165.38, 455.27, and 337.01 F g^-1 for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes, respectively. All GCD study with various current densities is mentioned in Fig. S2 (A-E). The cyclic stability is measured for the Ni_0.9Co_2.1O₄electrode as it exhibited a higher capacitance value than other nickel cobalt oxide nanostructured electrodes. The observed stability for the Ni_0.9Co_2.1O₄electrode is 87.7% over the 2000 charging-discharging cycles as depicted in Fig. 5 C. Inset image of Fig. 5C shows the first and last charging and discharging cycles. The higher specific capacitance and stability of Ni_0.9Co_2.1O₄electrode may be due to micro sheets covered nanospheres like morphology. The micro sheets and nanosphere morphology provide maximum surface area so that the interaction between electrode and electrolyte becomes easier, enhancing the specific capacitance value. The calculated specific capacitance from CV vs. scan rate is mentioned in fig. 5 D. In contrast, the variation of specific capacitance vs. current density is mentioned in fig. 5 E. Fig. 5 F presents the Regone plot. The maximum energy density for the Ni_0.9Co_2.1O₄electrode is 15.81 Wh kg^-1(at 0.75 kW kg^-1power density). The comparison of supercapacitor performance of present work and previously reported work is mentioned in Table. 1.

3.6 Nonenzymatic glucose biosensing study

Here the same three-electrode system is used for the glucose sensing study except for 0.1 M NaOH electrolyte. Fig. 6 (A-E) presents the CVs of Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes in the absence of glucose (red) and in the presence of 1.0 M glucose (blue). Fig. 7 (A-E) presents the CV curves of Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes at different concentration of glucose (0.0, 0.2, 0.4, 0.6, 0.8, 1.0 M). Here we can observe that for all samples, peak currents are increased after the addition of glucose. The increase in the peak currents is explained as follows ⁴⁵,

During the oxidation, Ni²⁺ and Co²⁺ ions present in the NiOOH and CoOOH compounds oxidize to Ni³⁺ and Co³⁺ with the release of two electrons (eq. 1-3). After adding glucose, the glucose molecules dissociate and are converted into gluconolactone with the release of two electrons (eq. 4). During reduction, the oxidized species Ni³⁺ and Co³⁺ reduce back to the Ni²⁺ and Co²⁺ by accepting electrons and returning to their original states. Fig. 8 (A-E) presents the CV of different nickel cobalt oxide electrodes in the presence of 1.0 M glucose at various scan rates (10-100 mV s^-1). It can be seen that with scan rate, the anodic and cathodic peaks also increase. Fig. 9 (A-E) presents the chronoamperometry study (I vs. t) of each nickel cobalt oxide electrode at 0.4 V applied potential with the subsequent addition of 0.05 mM glucose into 0.1 M NaOH electrolyte. The inset of Fig. 9 (A-E) shows their calibration curves of Amperometric responses. The observed sensitivities for Co₃O₄, Ni_0.3Co_2.7O₄, Ni_0.6Co_2.4O₄, Ni_0.9Co_2.1O_4, and Ni_1.2Co_1.8O₄ electrodes are 370.7, 759.5, 747.4, 557.7, 688.1 µA mM^-1cm^-2, respectively. The Nyquist plots in the absence of glucose and in the presence of 1.0 mM glucose are shown in supplementary information Fig. S3. The estimated glucose-sensing parameters are given in Table 2. As shown in Fig. 10 (A-E), the selectivity of samples was examined by addition 0.2 mM glucose and other interfering species [0.0125 mM of uric acid (UA), Ascorbic acid (AA), Fructose (FR), Sucrose (SA), and Lactic acid (LA)]. All the electrodes showed a negligible effect of interfering species as compared to glucose. The response times for all prepared electrodes are mentioned in Fig. S4 (Supplementary data). The comparative glucose-sensing study of current work and previously reported work is mentioned in Table. 3.

In summary, the nickel cobalt oxide by varying Ni concentrations has been prepared by the hydrothermal method. The nanosheet like Ni_0.9Co_2.1O₄ electrode exhibited 516.51 F g⁻¹ specific capacitance at 10 mV s⁻¹ and cyclic stability of 87.7% over 2000 galvanostatic charge-discharge cycles. Also, it showed an energy density of 15.81 Wh kg⁻¹ at 0.75 kW kg⁻¹ power density. The Ni_0.3Co_2.7O₄ nanosheets on CC showed linear response from 0 to 0.3 mM glucose concentration and exhibited the highest glucose sensitivity of 759.5 µA mM⁻¹ cm⁻². The overall study is a platform for the development of a flexible, high stability supercapacitor and reliable nonenzymatic glucose sensor.

5. Acknowledgment

Authors thankful to DST-SERB government of India for providing financial support under, Early career research award Scheme File no. ECR/2017/002099.

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Tables 1-3 are in the supplementary files section.

No competing interests reported.

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Hydrothermally synthesized Nickel cobalt oxide for bifunctional electrochemical supercapacitor and nonenzymatic glucose biosensor

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