Highly sensitive nonenzymatic H2O2 sensor based on NiFe-layered double hydroxides nanosheets grown on Ni foam

Surfaces and Interfaces 12 (2018) 102–107

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Highly sensitive nonenzymatic H2O2 sensor based on NiFe-layered double hydroxides nanosheets grown on Ni foam ⁎

Tao You, Chang Qing, Liu Quanhui, Yang Guolin, Guan Hongtao, Chen Gang , Dong Chengjun

T ⁎

School of Materials Science and Engineering, Yunnan University, 650091 Kunming, PR China

A R T I C LE I N FO

A B S T R A C T

Keywords: NiFe-LDH Ni foam Nanosheet Nonenzymatic H2O2 Sensor

Here, NiFe-LDH grown on Ni foam was successfully synthesized through a facile one-step hydrothermal approach and then directly applied as the electrode for nonenzymatic H2O2 sensor. The structure and morphology, of the as-synthesized NiFe-LDH were firstly characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and transmission electron microscopy (TEM). It is found that NiFe-LDH nanosheets assemble differently on inner and outer Ni foam with different Fe contents. The subsequent electrochemical measurements showed that the NiFe-LDH/Ni foam electrode exhibited remarkable electrocatalytic activity towards H2O2 oxidation with a high sensitivity of 1704 µA mM−1 cm−2 (0.5 µM to 0.84 mM) and low limit of detection (0.5 µM). These impressive performances indicate that the NiFe-LDH nanosheets is a promising candidate for nonenzymatic H2O2 sensors.

1. Introduction As we all known, Hydrogen peroxide (H2O2) is a vital mediator in various fields, such as electrochemistry [1], chemical [2], biochemical industries [3], environmental protection [4], pharmaceutical [5] and so on. Thus, the rapid and accurate detection of H2O2 appears quite important. So far, many technologies have been developed to determine H2O2, including electrochemistry, spectrophotometry, fluorescence, and chemiluminescence [6]. Especially, electrochemical method is one of the most effective ways for the determination of H2O2 because of its intrinsic merits such as high sensitivity, selectivity, ease of preparation, fast response, low cost [7]. During the electrode preparation, one step and in situ hydrothermal method has been widely used synthesizing electrode due to its facile operating process [8]. Such an approach makes assembly on self-supported conductive substrates for electrical addressing, controlling, and detecting come true. Besides, the atoms on the surface layer of conductive substrates could be the source of production [8], which is beneficial to the strong interaction between production and highly conductive substrates, greatly contributing to catalytic activity as well as high charge transfer efficiency [9]. Further, electroactive materials prepared by in situ oxidation of conductive substrates would reduce the internal resistance and maintain a rapid redox reaction [10]. Layered double hydroxides (LDHs) possess unique structure, in which the positively charged layer spaces have been incorporated by anions and solvation molecules [11]. Particularly, the latest reports

⁎

Corresponding authors. E-mail addresses: [email protected] (G. Chen), [email protected] (C. Dong).

https://doi.org/10.1016/j.surfin.2018.05.006 Received 3 February 2018; Received in revised form 1 May 2018; Accepted 4 May 2018 Available online 07 May 2018 2468-0230/ © 2018 Elsevier B.V. All rights reserved.

demonstrate that man LDH and their hybrids have showed excellent performances for H2O2 detection. Yang and coworkers reported the Ni/ Al and Co/Al LDHs modified electrode for H2O2 detection [12]. Habibi et al. improved the sensing performance of Ni-Al LDH by Ag nanoparticle modification [13]. Asif's group found that the CuO@MnAlLDHs could be a high efficient catalyst towards H2O2 reduction for biosensing application [14]. Apart from its successful application as a predursor for oxygen evolution reaction (OER) activity [15–17], NiFeLDH has been recently employed as an efficiently mimic enzyme for colorimetric determination of glucose and H2O2 [18]. However, the performance of NiFe LDH based electrode for electrochemical determination of H2O2 is still unknown, which motivates this work. Inspired by the above considerations, we developed a facile one-step hydrothermal approach to directly grown NiFe LDH nanosheets on Ni foam. The NiFe LDH/Ni foam was used as the electrode for nonenzymatic H2O2 detection, which exhibits high sensitivity, fast response time and low detection limit. Hence, we believe that the low cost and simple synthesis of the NiFe LDH may probably enhance the application of the sensor in H2O2 detection. 2. Experimental section 2.1. Preparation All the chemical reagents in the experiments were of analytical grade and used without any further purification. At the very beginning

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the typical XRD patter of the NiFe-LDH on Ni foam. Three intense characteristic peaks correspond to (111), (200) and (220) planesof Ni foam (JCPDS No. 04–0850). Other peaks appearing at 2θ of 11.634°, 23.390°, 34.466°, 39.116, 46.610°, 59.981°, 61.344° can be well indexed respectively to the (0 012), (204), (2010), (2016), (220), (2120) facets of NiFe LDH, which is in good agreement with JCPDS No. 26–1286. No other diffraction peaks of impurities were found, demonstrating the high purity of the as-synthesized product in our experiment. The overall morphologies of the NiFe-LDH were observed by SEM and depicted in Fig. 2. In Fig. 2(a), the Ni foam was totally covered by NiFe-LDH. A large number of NiFe-LDH dispersed on the outer part of Ni foam, while the inner Ni foam seems to be smooth. From the magnified SEM images in Fig. 2(b)–(d), the hierarchical NiFe-LDH spheres (several microns in diameter) are conglomerated on the outer Ni foam, which is interconnected with numerous nanosheets. On the contrary, interconnected nanosheets are successively resembled on the surface of the inner Ni foam, as illustrated in Fig. 2(e) and (f). These results prove that the NiFe-LDH appears different growth mechanism, which may be explained in the following. Under hydrothermal conditions, the urea decomposes into ammonia, which created an alkaline environment [19]. When Ni2+ and Fe3+ are mixed with OH−in aqueous solution, the initial burst nucleation occurs, deriving to the aggregation of the supersaturated nuclei and further assembling into nanosheets with the reaction time due to the famous Ostwald ripening. Furthermore, the spheres were formed by crosslinking nanosheets together to decrease the system energy [20]. There is more chance for the outer Ni foam to assemble nanosheets, leading to distinct NiFe-LDH in our product. Besides, the different growth mechanism is attributed to the huge difference between Ni foam and NiFe-LDH in both lattice and thermal coefficient [21]. To further study the difference of NiFe-LDH in different Ni foam, the corresponding chemical compositions were examined by EDS (Fig. 3), which confirms the existence of Ni, Fe and O elements. It is worth to note that the Fe contents (7.23 at%) are less for the NiFe-LDH on the inner Ni foam Fig. 3(a). Even for the outer part, as shown in Fig. 3(b), the EDS spectrum also shows that the final molar ratio of Ni: Fe (11.5:1) is different from the ratio of the starting precursors used, indicating different growth rate of Ni and Fe at the same hydrothermal condition, which is agree well with the results of SEM. TEM measurements were carried out to further investigate the structure of the as-synthesized NiFe-LDH nanosheets which were ultrasonically peeled off from Ni foam. As can be seen from Fig. 4(a)–(c), the NiFe-LDH nanosheets are ultrathin (around 25 nm) and partially transparent. The NiFe-LDH nanosheets are of rippled or wrinkled (Fig. 4(c)). In Fig. 4(d), the obtained d-spacing value of 0.24 nm corresponds to (208) crystal plane of NiFe-LDH. In short, the TEM images indicate that the NiFe-LDH nanosheets are smooth on the surface and high crystallization.

a piece of Ni foam with 2 cm × 4 cm in size was pretreated by immersing into a hydrochloric acid, and then cleaned by ethanol and deionized water. In a typical synthesis, 2 mmol Ni(NO3)2·6H2O and 2 mmol Fe(NO3)3·9H2O were dissolved in 60 mL deionized water to form a homogeneous solution by magnetic stirring. After that, 4 mmol NH4F and 10 mmol urea were further added. The resulting solution was then transferred into a 100 mL Teflon-lined stainless steel autoclave. The autoclave was sealed and kept at 120 °C for 6 h in an oven. When the reaction was completed, the autoclave was naturally cooled to room temperature. The Ni foam was taken out carefully and rinsed several times with deionized water and absolute ethanol, respectively. 2.2. Characterizations The crystal structure of productwas examined by a X-ray diffraction (XRD, Rigaku TTRIII) with an incident X-ray wavelength of 1.540 Å (Cu Kα line).The morphology and microstructureof Ni-Fe LDH/Ni foam were investigated by a scanning electron microscope (SEM, FEI QUANTA 200, operating at an accelerating voltage of 10 KV) and a transmission electron microscope (TEM, JEM-2100 JEOL, Japan, running at 200 kV). The NiFe-layered double hydroxides were ultrasonically peeled off from Ni foam and dispersed in ethanol, then casting them on the copper grids. The chemical compositions were recorded with an energy dispersive spectrometer (EDS) equipped on SEM. 2.3. Electrochemical measurements Electrochemical measurements were performed in a conventional three-electrode cell, in which the NiFe hydroxides nanosheets, a platinum plate, and a saturated calomel electrode (SCE) electrode were used as the working electrode, the counter electrode and the reference electrode, respectively. Cyclic voltammetry (CV), and amperometry measurements were recording using a CHI660D electrochemical workstation (Chenhua, Shanghai) in a solution of 0.2 M NaOH electrolyte. 3. Results and discussion 3.1. Characterization of the Ni-Fe LDH The photographs in inset of Fig. 1 clearly compare the changes in color with/without NiFe-LDH. By eye, it is of evidence that the Ni foam was uniformly covered with a brown NiFe-LDH, indicating the successful growth of NiFe-LDH after hydrothermal reaction. Fig. 1 shows

3.2. Nonenzymatic amperometric sensing of H2O2 The as-synthesized NiFe-LDH/Ni foam was directly employed as H2O2 sensing anode. Fig. 5(a) presents the cyclic voltammograms (CVs) of the NiFe-LDH/Ni foam in 0.2 M NaOH at different scan rates (5–50 mV/s). A pair of well-defined redox peaks can be clearly seen. As the scan rate is increased, both anodic and cathodic peak current increase. Besides, the anodic peak appears positive shift, while the cathodic peak moves negatively, which is widely accepted a quasi-reversible electron transfer reaction for the electrochemical reactions. Furthermore, the linear relationship of oxidative or reductive peaks current versus the square route of scan rate with good correlation coefficients of R2 = 0.9927 (oxidative peaks) and R2 = 0.9854 (reductive peaks), as plotted in Fig. 5(b), suggesting that the reaction was a diffusion-controlledprocess. The electrooxidation of H2O2 by NiFe-LDH can be explained in the

Fig. 1. XRD pattern of NiFe-LDH nanosheets on Ni foam. (The photographs in inset comparably show the Ni foam with/without NiFe-LDH). 103

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Fig. 2. SEM images of overall NiFe LDH/Ni foam(a), outerparts(b–d) and innerparts (e and f) of Ni-Fe LDH.

Fe(OH)3 + H2O2 → Fe(OH)2 + 2H+ + O2 ↑

following based on the previous discussions [2,21–24]. −

Ni(OH)2 + OH → NiOOH + H2O + e

(1)

NiOOH + H2O2 + e→ Ni(OH)2 + O ↑

(2)

2

−

H + OH →H2O +

(3) (4)

From these equations, the electrons are easily transferred from NF-

Fig. 3. EDS pattern of NiFe LDH/Ni foam for inner parts (a) and outer parts (b). 104

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Fig. 4. TEM images of NiFe-LDH nanosheets(a–c) and HRTEM images of NiFe-LDH nanosheets (d).

subsequent measurements. The amperometric response of NiFe-LDH/Ni foam electrode towards successive addition of certain H2O2 was recorded (Fig. 6(c)), which shows a fast response (less than 16 s). The limit of detection (LOD) was determined to be 0.5 µM, as illustrated in inset of Fig. 6(c). Fig. 6(d) shows the corresponding calibration curve, which displays excellent linearity between the steady current and the H2O2 concentrations in the range from 0.5 µM to 84 mM. The linear regression equation was Ip (µA) = 1.36352C (mM) + 0.1995 with a correlation coefficient of 0.9955. Based on the slope of the fitted curve, the sensitivity of NiFeLDH/Ni foam electrode was determined to be 1704 µA mM−1 cm−2. The performance of our H2O2 sensor has been compared with some reported hydroxides based nonenzymatic H2O2 sensors, as summarized in Table 1. Apparently, our sensor exhibits an excellent integrative performance with higher sensitivity, fast response time and lower detection limit. The excellent integrative performance of NiFe-LDH/Ni foam electrode can be mainly attributed to the following aspects. Especially, the hierarchical structure with cross-linked outer Ni foam and interconnected inter Ni foam can expose more active sites to

LDH to Ni foam due to the compact connection between them, which may be the main explanation for the excellent sensing performance towards H2O2. Fig. 6(a) indicates the CV curves of the NiFe-LDH/Ni foam electrode in 0.2 M NaOH with H2O2 concentrations from 0 to 1 M at a fixed scan rate of 10 mV/s. The remarkable enhancements and shifts of both anodic and cathodic peak current are observed, indicating the excellent electrocatalytic properties of NiFe-LDH. It was reported that electrooxidation of H2O2 produces oxygen gas bubbles on the electrode surface, which endows great enhancement of the H2O2 diffusion towards the electrode surface, leading a significantly higher oxidative current [25–26]. A constant potential chronoamperometry was performed at different potential around the anodic peak potential to obtain a better current response. Fig. 6(b) shows the amperometric response of the NiFe-LDH/Ni foam electrode towards six successive addition of 10 µM H2O2 at potentials of 0.38, 0.40 and 0.42 V. A relatively larger response current is observed at 0.40 V. Hence, 0.40 V was selected as the optimum working potential for amperometric detection of H2O2 in the

Fig. 5. (a) Cyclic voltammograms of NiFeLDH/Ni foam electrode in 0.2 M NaOH solution with different scan rate (5–50 mV/s), (b) linear relationship between the cathodic current and the square root of scan rate with scan rate at 10 mV/s. 105

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Fig. 6. (a) Cyclic voltammograms of NiFe LDH/Ni foam electrode in 0.2 M NaOH solution with different H2O2concentration (0–1 mM), (b) Amperometrici–t curveof the NiFe LDH/Ni foam electrode settingat different potencial in 0.2 M NaOH with successive addition of 10 µM H2O2 and (c)Amperometric response with stepwise addition of H2O2 (inset shows the infinitesimal circumstances) under the same conditions, (d) the calibration curve of current response versus H2O2 concentration (inset shows the fitting curve). Table 1 Summary of the sensing performance of various reported hydroxides toward non-enzymatic H2O2. Material

Sensitivity (μA mM−1cm−2)

Detection limit (μM)

Linear range (mM)

Ref.

MnOOH Ni/Al-LDHs Co/Al-LDHs Ag/FeOOH Ni(OH)2 Au NPs-Ni (OH)2eCu CoOOH MnOOH/CC Ni(OH)2/RGOMWNT Ni-Al/LDH/Ag Ni(OH)2/Si NWs FeOOH@PDAAg NiFe-LDH

– 74.82 97.61 8.07 408.1 –

0.115 9 50 22.8 1.5 0.3

1.5 × 10−4–1.6 36–1.75 × 105 200–6.74 × 105 0.03–15 5 × 10−3–0.145 2.5 × 10−3–1.2295

[27] [12] [12] [28] [29] [30]

99 692.42 2042

40 3.2 2.7

40 × 10−3–1.6 20 × 10−3–9.67 0.01–1.5

[31] [32] [33]

1.863 3310

6 3.2

10 × 10−3–10 0–5.5

[13] [22]

11.8

2.5

7.5 × 10−3–18.8

[34]

1704

0.5

−4

5 × 10

–0.84

Fig. 7. Amperometric response of the NiFe LDH/Ni foam electrodeto the sequential addition of 100 µM H2O2 and 10 µM interfering specials of NaCl, DA, KCl, UA, and glucose at 0.4 V.

This work

was studied and shown in Fig. 7. It is clearly seen that there are no responses with the addition of KCl and NaCl. A negligible response towards dopamine (DA), Uric acid (UA), and glucose is observed. These results clearly demonstrate that the NiFe-LDH/Ni foam electrode exhibits high sensing selectivity electrochemical detection of H2O2.

provide accessible pathways for mass transfer and charge transfer. Further, the unique structure may also facilitate facile release of the evolved O2 during electrooxidation [18]. Moreover, the hierarchical porous texture offers more active sites and convenient pathways to facilitate both OH− and electron transfer at the electrode/electrolyte interface. Finally, the in situ direct growth of FeNi LDH on the Ni foam could further improve the conductivity and charge transfer capability [20]. As a H2O2 sensor, the selectivity is also vital characteristic, which

4. Conclusions In 106

summary,

NiFe-LDH

nanosheets

have

been

successfully

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fabricated on Ni foam through a one-step hydrothermal approach. Based on XRD, SEM and TEM measurements, NiFe-LDH are well grown on the surface of Ni foam, which evolves into two growth processes. That is hierarchical NiFe-LDH spheres on outer Ni foam and interconnected nanosheets on inner Ni foam. The nanosheet is estimated to be about 25 nm in thickness. When using as electrochemical electrode for the detection of H2O2, highly sensitive (1704 µA mM−1 cm−2) and selective detection of H2O2 was achieved with a relative low detection limit of 0.5 µM, wide linear detection range of 0.5 µM to 0.84 mM and a fast response (within 16 s). Our study indicates that NiFe-DLH represents a promising sensing material for nonenzymatic amperometric detection of H2O2.

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