DOI: 10.1002/slct.

201802526 Full Papers

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2 z Materials Science inc. Nanomaterials & Polymers
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Facile Synthesis of Electrospun Nickel (II) Oxide Nanofibers
6 and Its Application for Hydrogen Peroxide Sensing
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8 Sudharshan Vadnala,*[a] Suryasnata Tripathy,[b] Nirupam Paul,[b] Amit Agrawal,[a] and
9 S. G. Singh*[b]
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The aim of the present study is to report an alternative exhibiting a single phase crystalline structure. The NiO nano-
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technique of creating nickel oxide (NiO) nanofibers, manufac- fibers modified glassy carbon electrode (GCE) showed an
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tured by facile and economical electrospinning process. The excellent performance towards the electrocatalytic oxidation of
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crystallinity nature of NiO nanofibers is investigated by X-ray hydrogen peroxide (H2O2). This sensor showed a wide range of
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diffraction (XRD). Nanofibers morphology is examined by detection from 10 μM to 50 mM, low limit of detection 0.33 μM
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Scanning Electron Microscopy (SEM) and Transmission Electron and high sensitivity 42.09 μA μM 1cm 2 for H2O2 detection. The
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Microscopy (TEM). The diameter of the nanofibers is varying entire analysis reaffirms the suitability of NiO nanofibers as one
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from of 100–150 nm. Furthermore, Selected Area Electron of the futuristic sensing material for H2O2 detection.
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Diffraction (SAED) pattern revealed that NiO nanofibers are
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supercapacitors, electrodes, environmental and energy re-
23 Introduction
search. Further, it has high specific surface area, biocompati-
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Since the last decade, an investigation of 1-D metal oxides bility, good oxygen ion conductivity, outstanding structural
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nanofibers have gained significant attention of the scientists stability, non-toxicity, natural abundance, and active electro-
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and technocrats because of their interesting applications in catalytic properties.[8,9] Hence, fabrication of NiO nanofibers
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various fields such as energy storage and conversion, catalysis, using electrospinning and obtaining of single phase crystalline
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sensors, electronics, and biomedicine.[1–3] It is very well structure will have a wide range of potential applications.
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addressed that metal oxides nanostructured materials are Analytical determination of hydrogen peroxide (H2O2) has
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exhibiting large number of novel phenomena at the nanoscale gained significant attention in various fields such as clinic,
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and their functional properties are dependent on the size and pharmaceuticals, food, and environmental analyses, because
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dimension of the structure.[4] Nanofibers have large surface H2O2 is chemical hazard to the environmental and the
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area, high aspect ratio, excellent pore interconnectivity, which production of enzymatic reactions.[10,11] Hence, detection of
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are favorable for electrochemical sensing, energy storage and H2O2 is very important for industrial applications and it is
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conversion. Lithographic[5] and wet chemical[6,7] routes are generally detected by two different processes such as enzy-
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suitable for fabrication of nanostructure materials, but these matic and non-enzymatic reactions. Enzymatic technique for
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techniques are restricted to lengths of nanostructures of only a detection of H2O2 is complicated as these sensors are
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few microns. Therefore, fabrication of nanofibers with industrial insufficient stability initiating from the nature of the enzymes
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scalable is possible by electrospinning technique which can and those are easy to deform thermally and chemically during
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produce the nanofibers with several microns. Moreover, the fabrication, storage and usage.[12] Hence, researchers are
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electrospun nano fibers have great porosity and high surface to highly focusing on the cost effective non-enzymatic sensors for
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volume ratio which enhances its electrochemical sensing detection of H2O2. Recent studies show that some noble metals,
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properties. Thus, it has an advantage of comparative low cost including Ag,[13] Au,[14] Pt,[15] and metal alloy have been used as
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and relatively high production rate. In case of metal oxides, NiO H2O2 sensors because of their high electrocatalytic
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is one of the stable p-type wide band gap semiconducting activities.[16–18] Pure metals and metal alloys are preferred for
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metal oxide and it has potential applications in biological, high sensitivity but their limit of detection (LoD) and range of
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detection is very low as compare with metal oxides and also
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these materials are expensive. In case of metal oxides,
49 [a] Dr. S. Vadnala, Prof. A. Agrawal
transition metals basically have multiple valence states and can
50 Mechanical Engineering Department
Indian Institute of Technology Bombay easily form a redox cycle between the high and low oxidation
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E-mail: sudharshan.vadnala@gmail.com states. As a result the change in metal valence, lattice oxygen
52 [b] S. Tripathy, N. Paul, Prof. S. G. Singh will be free to create an oxygen vacancy or reinstated to form
53 Electrical Engineering Department
an adsorbed oxygen species.[19] Furthermore, fabrication of
54 Indian Institute of Technology Hyderabad
E-mail: sgsingh@iith.ac.in nanostructured metal oxides are cost effective and highly
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Supporting information for this article is available on the WWW under sensitive due to their large surface to volume ratio of the
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https://doi.org/10.1002/slct.201802526 nanostructures. So far, several metal oxide nano particles/nano
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24 Figure 1. (a) Indicate the XRD pattern of NiO nanofibers, (b & c) represents the nanofibers as synthesized nanofibers at room temperature and after calcined
25 nanofibers, TEM images of (d) NiO nanofibers (e) high resolution images of NiO nanofibers with d spacing 0.21 nm along the direction (200), (f) selected area
electron diffraction (SAED) pattern of NiO nanofibers.
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29 Results and Discussion
fibers such as NiO,[20,21] MnO2,[22] Fe2O3,[23] Cu2O,[24] CeO2,[25] and
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SnO2[26] are studied as electrochemical sensors for detection of Figure 1(a) shows the single phase crystalline structure of the
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biosensors and H2O2. Among the metal oxides, NiO is one of NiO nanofibers after calcination at 450 °C. The XRD peaks at 2θ
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the stable nanomaterial which can be useful for detection of positions, 37.2°, 43.3°, 62.9°, 75.5° and 79.5°, respectively are
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hydrogen peroxide (H2O2) sensing as it has excellent selectivity, described to (111), (200), (220), (311) and (222) planes of
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high catalytic rate and to not easy to absorb intermediates and reflection of NiO. Analysis of XRD result confirms that the
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Cl ions[27,28] besides having other well dispersion properties.[29] nanofibers have crystallized in cubic structure and their XRD
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Moreover, NiO is one of the most studied material for bio- pattern matches very well with the standard PCPDF reference
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sensing as it has several advantages such as good chemical number 47–1049. All the reflections are indexed to face-
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stability, easy tuning the morphology and structure. In this centered cubic (fcc) NiO phase with lattice constant 4.175 Å
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present work, we have developed a simple, robust and (space group). Moreover, sharpness of the peaks indicates the
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economical electrospinning process for fabrication of NiO well crystallinity nature of the nanofibers.
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nanofibers and their structural and morphology have been The surface morphology of fabricated nanofibers was
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systematically investigated. The synthesized NiO nanofibers analyzed by scanning electron microscopy (SEM). SEM images
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have well-defined morphology and high surface to volume of as-spun and after calcination nanofibers are shown in
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ratio. Furthermore, we developed NiO nanofibers modified GCE Figure 1(b) and 1(c). The electrospinning parameters such as
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for an electrocatalytic as a potential detection of H2O2 sensing. flowrate, voltage and distance were optimized to obtain
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The proposed H2O2 sensor exhibiting high sensitivity and wide uniform polymeric fibers with diameters in the range of 250–
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range of detection with a low limit of detection. 400 nm. PAN and Ni(NO3)2.6H2O concentrations were also
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optimized to fabricate a bead free continuous uniform
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diameter fiber mat. The collected nanofibers were further
50 Electrode preparation
calcined at 450°C. After the calcination, the average diameters
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The glassy carbon electrode is polished using 0.3 micron of the nanofibers shrunk to 100–150 nm. Furthermore, struc-
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alumina slurries, washed with deionized water, and finally tural and morphological features of the NiO nanofibers are
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sonicated for 10 minutes in acetone. Calcined nickel oxide confirmed by TEM measurement. Figure 1(d) clearly shows the
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nanofibers are dispersed in ethanol and ultrasonicated for 10 formation of nanofibers and diameter of nanofibers is around
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minutes. 6 microliters of nickel oxide nanofibers were drop 100–150 nm. Figure 1(e) shows the adjacent lattice fringes are
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casted on glassy carbon electrode and dried at 40 °C for 1 hour. at 0.21 nm corresponding to the (200) lattice plane of NiO
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ChemistrySelect 2018, 3, 12263 – 12268 12264 © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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Figure 2. (a & b) Represents the FTIR and UV-Visible absortion spectroscopy of NiO nanofibers, (c) indicates direct optical bandgap of nanofibers spectra of NiO
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nanofibers.
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nanofibers. Moreover, the select area electron diffraction
18 Electrochemical sensing and detection
(SAED) pattern (Figure 1(f)) exhibits well defined diffractions
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rings, indicating the crystalline characteristics of the NiO In order to illustrate the electrochemical responses of the nickel
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nanofibers which is very well match with XRD results. There- oxide nanofibers towards hydrogen peroxide, cyclic voltamme-
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fore, XRD and TEM analysis clearly reveals that NiO nanofibers try studies were carried out using a glassy carbon working
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exhibiting single phase crystalline structure. electrode, standard calomel reference electrode, a platinum
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The FTIR spectrum of as synthesized NiO nanofibers is wire counter electrode and standard PBS buffer as the electro-
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shown in Figure 2(a). NiO nanofibers shows the absorption lyte. Cyclic voltammograms of a bare and polished GCE and the
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region 530.38 cm 1 to 555.38 cm 1 corresponds to the peaks of NiO nanofiber modified GCE (GCE/NO) are presented below in
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metal-oxygen vibrational modes. The metal-oxygen frequencies figure 3(a). For a scan rate of 80 mV/s, the bare GCE electrode
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observed in this study are well matched with reported expressed no redox peaks for the buffer electrolyte, due to the
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results.[30] The mode present at 1135 cm 1 corresponding to the absence of any electroactive redox couple. On the contrary, the
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C N stretching and remaining two modes 1615, 2348 cm 1 are GCE/NO electrode recorded distinct redox peaks, correspond-
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assigned to the vibrations of water molecules.[31] ing to the oxidation-reduction reaction of Ni + /Ni2 + involving a
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It is well known that band gap is a vital parameter in single electron transfer. For a scan rate of 20 mV/s, the
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determining the characteristics of semiconductor materials oxidation reaction occurs at the anodic peak potential of 0.28 V
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which is recorded by UV absorption spectrum. Figure 2(b) whereas the reduction reaction corresponds to a cathodic peak
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shows the optical absorption spectrum of the NiO nanofibers at potential of 0.16 V.
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the room temperature. As shown in Figure 2(b), a strong Cyclic-voltammograms for the GCE/NO electrode at differ-
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absorption in the UV region has observed at wavelengths ent scan rates ranging from 20 mV/s to 120 mV/s are also
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about 373 nm, which is due to the band gap absorption in NiO presented in figure 3(a). As can be seen, the peak currents,
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nanofibers.[32] Moreover, a strong absorption was observed at both anodic and cathodic, increase with the increasing scan
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394 nm in the visible region, which is attributed to intra-3d rate, a behaviour which can be the explained in terms of the
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transition of Ni2 + in the cubic structure of NiO.[33] Indeed, the size of the diffusion layer at the electrode surface. A linear
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optical band gap of the NiO nanofibers measured using Tauh’s relationship exists between the anodic and cathodic peak
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plot with the following equation: currents and the square root of the scanning potentials, as
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shown in figure 3(b). Also, it is to be noted that with increase in
44 ahn ¼ Aðhn Eg Þm the scan rate, both the cathodic and anodic peak potentials
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shift to higher values. A change in the peak potentials with the
46 Where is the incident photon energy, is a constant, is the scan rate indicates a non-ideal reversibility of the GCE/NO
47 energy bandgap of the material, and the exponent determines system.
48 the type of electronic transition, causing the absorption to take
49 a value between 1/2 and 2. The optical bandgap which is
50 calculated with the help of Talc’s plot by extrapolating the Electrochemical detection of H2O2 using GCE/NiO
51 straight line part of the curves at = 0, is shown in Figure 2(c). Detection of H2O2 using the nickel oxide nanofiber modified
52 The direct bandgap for NiO nanofibers is found to be 3.3 eV, glassy carbon working electrodes was carried out using electro-
53 which is consistent with the previous reports.[34] chemical studies performed using a similar setup as explained
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in the previous section. As shown in figure 3(c), in presence of
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H2O2, the cyclic voltammograms changed their shape in the
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anodic potential range, showing an increasing current trend
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ChemistrySelect 2018, 3, 12263 – 12268 12265 © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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concentration, the overall amperometric current increases as
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expected.
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We have correlated the amperometric peak currents to the
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H2O2 concentrations, to develop a calibration system as
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presented in Figure 3(e). In the figure, we have also presented
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a four-parameter logistics based sigmoidal fitting model to
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mathematically describe the correlation between the individual
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peak currents with their corresponding doses. The four-
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parameter logistics model used for developing the sigmoidal fit
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is described through the fallowing.
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11 A1 A2
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x
1þ x0
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15 Where A1, A2, x, x0 and p correspond to the minimum
16 asymptote, the maximum asymptote, concentration of H2O2,
17 H2O2 concentration corresponding to 50% of the maximum
18 signal change (inflection point) and slope at the inflection point
19 of the sigmoid, respectively.
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We have calculated the limit of detection and the sensitivity
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of the proposed hydrogen peroxide sensor, using the 3.3σ and
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10σ methods respectively. The proposed sensor accounts for
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an excellent sensitivity of 42.09 μA μM 1cm 2 with a wide
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dynamic detection range varying from 10 μM to 50 mM. The
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limit of detection (LoD) of the proposed sensor is found to be
26 Figure 3. (a) represents the CVs measurement of NiO nanofibers/GCE in
0.01 M PBS at pH 7.4 at room temperature with different scan rates (20- 0.33 μM. The comparison characteristics of the NiO nanofibers
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120 mV/s), (b) relation between current vs V1/2, (c) indicates CVs measure- with relevant devices found in literature is provided in Table 1.
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ment of NiO nanofibers/GCE with different varying of molarity from 10 μM to
29 20 mM, (d) ammperometric response of NiO nanofibers/GCE with addition of
30 different molarity H2O2 in 0.01 M PBS solution, (e) four parameter logistics Table 1. Comparison of analytical performance of the prepared NiO nano-
31 model used for developing the sigmoidal fit, (f) Selectiviy study of seven fibers with other existing reports.
different kinds disturbance.
32 Type of Sensitivity Limit of Range of Ref
33 electrode μA μM 1 cm 2
detection μM detection μM
34 [35]
Au NPs 14 5.0 5-43000
35 Pt/Ni/C 0.21 31.5 2-2000 [36]
with increasing H2O2 concentration. The behaviour of the GCE/
36 Pt/Pd/C 114 0.24 0-3000 [36]
NO was recorded over a wide range of H2O2, varying from 10 Pt-ZnO — 1.5 20-5000 [37]
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uM to 20 mM in concentration. The increasing trend in the Cu2O (NPs) 0.19 47.2 50-1100 [38]
38 [39]
anodic current was observed over the entire range of the target CuO/GC 0.088 0.167 4-40000
39 Co3O4/GC 0.08 0.01 0-5350 [40]
concentration, and the trend was in-line with the increasing
40 NiO-SPE 0.81 3.22 1.1-2400 [41]
concentration. The cyclic voltammograms presented in figure WS2 NS – 1.5 50-200 [42]
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3(c) were recorded at a scan rate of 80 mV/s at room temper- g-C3N4-Fe3O4 – 0.3 1-200 [43]
42 [44]
ature. The stock solutions of H2O2 for the analysis presented Mil-88 MOF – 0.5 0.2-20
43 NiO NFs 42 0.32 10-50000 PW
herein were prepared in PBS buffer by using serial dilution
44
method. [NPs] nanoparticles, [PW] present work, [NFs] nanofibers, [NS] Nano sheets,
45 [MOF] metal organic framework
Furthermore, we have performed amperometric studies in
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the H2O2 concentration range of 10 μM to 50 mM at a potential
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of 0.6 V. For these experiments, the amperometric analyses
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were performed over a time of 400 seconds. To the electrolyte It can be observed that the performance of our sensors is
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solution (PBS), different concentrations of H2O2 were sequen- comparable, and in some cases, it is better than the reported
50
tially added over fixed intervals, and the resulting responses devices.[35–41] Furhermore, the LOD and linear range of detection
51
were recorded. As can be seen in figure 3(d), upon introduction of our electrochemical sensing is comaprable with colorimetric
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of H2O2 in to the electrolyte medium, the amperometric devices.[42–44] Hence, it is worth mentioning that NiO nanofibers
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response records an instantaneous increase in the current electrode exhibiting remarkable electrocatalytic performance
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value, which then decreases with time. Such behaviour for hydrogen peroxide sensing in terms of their limit of
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establishes the sensitivity of the GCE/NO working electrode detection, and range of detection, although their sensitivity is
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towards H2O2 as an analyte. With increase in the H2O2 comparable with other materials.
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The selectivity of the proposed sensor was addressed by Supporting Information Summary
1
amperometric study. We recorded the amperometric responses
2
of the sensor to several chemicals namely sucrose, glucose, The supporting information contained the details of synthesis
3
sodium nitrate, tartaric acid, glutamic acid and ascorbic acid. As section and different characterization techniues such X-ray
4
can be seen in figure 3(f), the amperometric peak responses diffraction, Transmission electron Microscopy, Scanning Elec-
5
corresponding to all these chemicals are significantly inferior tron Microscopy,UV-Vis NIR spectrophotometer, Fourier trans-
6
when compared to the response recorded for an identical form infrared spectroscopy and Electrochemical measurement.
7
concentration of H2O2. This observation corroborates the fact
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that the GCE/NiO working electrode is essentially selective to
9 Conflict of Interest
H2O2 and can thus be used towards effective sensing of the
10
same. The authors declare no conflict of interest.
11
Furthermore, the stability of the NiO modified electrodes
12
tested for 10 days at a regular interval of 2 days is shown in Keywords: Electrochemical sensor · Electrospinning · Hydrogen
13
Figure 4 (a). As observed, at the end of 10th day, the peak peroxide · Nickel oxide · TEM
14
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ChemistrySelect 2018, 3, 12263 – 12268 12268 © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim