CN109187698A - A kind of hydrogen peroxide electrochemical sensor based on nanometer nickel sulfide enzyme - Google Patents
A kind of hydrogen peroxide electrochemical sensor based on nanometer nickel sulfide enzyme Download PDFInfo
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- CN109187698A CN109187698A CN201810902200.4A CN201810902200A CN109187698A CN 109187698 A CN109187698 A CN 109187698A CN 201810902200 A CN201810902200 A CN 201810902200A CN 109187698 A CN109187698 A CN 109187698A
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Abstract
The present invention discloses a kind of hydrogen peroxide electrochemical sensor based on nanometer nickel sulfide enzyme.The present invention uses electrochemical deposition and ion-exchange to synthesize NiS nano material using metal ion match as precursor.Then, the electrochemical sensor based on NiS is constructed to detect H2O2.The invention proposes a kind of using metal ion complex as the novel electro-deposition method of presoma, the metal ion complex and S hydrolyzed using thioacetamide2‑Slow ionic reaction control NiS generation rate, make the generating rate of NiS controllable compared with conventional electrodeposition method, provide condition for practical application.Preparation process of the present invention is simple, and the NiS particle size of synthesis is small compared with conventional electrodeposition method, the electrochemical sensor high sensitivity of synthesis, and detection limit is low.
Description
Technical field
The present invention relates to electrochemical sensor and electro-deposition techniques fields, and in particular to one kind is based on novel electro-deposition techniques
The nanometer nickel sulfide material of preparation is used to detect the electrochemical sensor of hydrogen peroxide.
Background technique
Hydrogen peroxide is widely used in food, medicine, faces as a kind of strong oxidizer due to its unique electrochemical properties
The fields such as bed diagnosis and environmental monitoring.Various analysis at present, such as fluorescent spectrometry, chemoluminescence method, electrochemical process by
Applied to the detection of hydrogen peroxide, wherein for electrochemical process due to high sensitivity, detection limit is low, at low cost to be widely used.
Upike and Hicks in 1967 develops first glucose oxidase electrode in the world, for grape wine in quantitative detection serum
Content.Hereafter, enzyme electrochemical sensor has obtained the great attention of the scientist in each field.Hydrogen peroxide currently used in the market
Sensor is mostly Electrochemical enzyme biosensor, although the advantages that the sensitivity with higher of such sensor and selectivity, enzyme
The features such as difficulty of preparation and purification and the affected by environment larger activity of enzyme, causes Electrochemical enzyme biosensor cost larger, make
Shorter with the service life, stability is poor.Recently, people utilize transition metal oxide (such as MnO2、Co3O4) modified electrode constructs
A variety of no enzyme electrochemistry hydrogen peroxide sensors.As BSaha et al. utilizes Mn (CH3COO)2、Na2SO4For electrolyte, electro-deposition is used
Method is prepared for MnO2Modified electrode, construct with higher sensitivity hydrogen peroxide sensor (B.S, S.K.J, S.B,
Electrodeposited nanostructured MnO2 for non-enzymatic hydrogen peroxide
sensing,Solid State Physics(2015),050097-1–050097-2.).However it current is passed without enzyme electrochemistry
The disadvantage that there are still sensitivity is lower for sensor, selectivity is poor, therefore, industrial circle is badly in need of a kind of at low cost, and stability is good, inspection
It surveys and limits low hydrogen peroxide sensor.
In recent years, transient metal sulfide (TMS) is attracted wide public concern due to its high conductivity.With transition metal hydrogen-oxygen
Compound is compared with transition metal oxide, and TMS has the Inherent advantages such as low cost, hypotoxicity and good biocompatibility, mesh
It is preceding to be just more and more used for the fields such as lithium ion battery, photocatalysis.In these TMS compounds, NiS has excellent charge
Storage capacity and electron conductivity are commonly used for supercapacitor and sensitization solar battery.Recently, many reports find NiS
With excellent electrochemical catalysis performance, and it is used as detecting the electrode active material of various substances.
For this purpose, the present invention provides a kind of hydrogen peroxide sensors based on nanometer nickel sulfide enzyme.In the present invention, S2-And lemon
Lemon acid sodium is used to form stable metal ion match.Then use electrochemistry heavy using metal ion match as precursor
Long-pending and ion-exchange synthesizes NiS nano material.Then, the electrochemical sensor based on NiS is constructed to detect H2O2。
Summary of the invention
The object of the present invention is to provide a kind of nanometer nickel sulfide enzyme hydrogen peroxide electrochemical sensors and preparation method thereof.
The present invention provides a kind of nanometer nickel sulfide enzyme hydrogen peroxide electrochemical sensors, and the sensor is by glass-carbon electrode and electricity
The nanometer nickel sulfide material of pole surface electro-deposition forms.The range of linearity of the sensor is 1 μm of ol/L~1000 μm ol/L, detection
Limit is 0.3 μm of ol/L.
Above-mentioned nanometer nickel sulfide enzyme hydrogen peroxide electrochemical sensor uses following preparation method, specific as follows:
(1) glass-carbon electrode after grinding homogeneity, is successively used into 1,0.3,0.05 μm of partial size of Al on polishing paper2O3Powder is thrown
Light.Then dehydrated alcohol is used respectively, and glass-carbon electrode is cleaned each 3~5min by deionized water in Ultrasound Instrument.With being dried with nitrogen.
(2) nickel compound containing and sodium citrate that molar ratio is 2:3 are dissolved in 50ml deionized water and stir 1h.
(3) being added in the mixed liquor obtained in (2) with nickel compound containing molar ratio is the thioacetamide of 5:1 and ultrasound
10~15min obtains reaction solution.
(4) with three-electrode electro Chemical work station, (Ag/AgCl is reference electrode, and platinum electrode is to electrode, and glass-carbon electrode is
Working electrode) with cyclic voltammetry carry out electro-deposition, the sedimentation potential of NiS is -0.9mv~0.7mv, is swept with the speed of sweeping of 5mv/s
Retouch 10 periods.
(5) glass-carbon electrode is cleaned with ultrapure water, removes foreign ion.
(6) glass-carbon electrode cleaned is shone 30~40 minutes under infrared lamp.
Compared with the existing technology, of the invention to have the prominent advantages that:
(1) the invention proposes a kind of using metal ion complex as the novel electro-deposition method of presoma, uses
The metal ion complex and S of thioacetamide hydrolysis2-Slow ionic reaction control NiS generation rate, relatively conventional electricity is heavy
Area method makes the generating rate of NiS controllable, provides condition for practical application.
(2) preparation process of the present invention is simple, and the NiS particle size of synthesis is small compared with conventional electrodeposition method, the electrochemistry of synthesis
Transducer sensitivity is high, and detection limit is low.
Detailed description of the invention
The FESEM that Fig. 1 is NiS schemes, and wherein a and b is adding citric acid sodium in electro-deposition substrate in 2 μm and 200nm resolution ratio
Under electron microscope, c is that 2 μm of resolution ratio electron microscopes of sodium citrate are not added in electro-deposition substrate, and d is in electro-deposition substrate plus lemon
The EDX of sour sodium schemes；
Fig. 2 is NiS Electrochemical Properties figure, and wherein a is in [the Fe (CN) containing 0.5mM6]3-With it is naked in 0.1MKCl solution
The Cyclic voltamogram curve of glass-carbon electrode and NiS modified electrode, b are to contain 0.5mM [Fe (CN)6]3-/4-It is molten with 0.5MKCl
The electrochemical impedance spectroscopy analysis chart of bare glassy carbon electrode and NiS modified electrode in liquid (insertion figure is equivalent circuit diagram)；
Fig. 3 is to probe into the concentration of different electro-deposition substrates to the electrocatalysis characteristic of NiS, and wherein a, b, c are respectively to contain
NiS modified electrode in 0.1M NaOH solution (sodium citrate, double nickel compound containing and sodium citrate is not added in adding citric acid sodium)
VA characteristic curve；
Fig. 4 is the performance analysis chart that the sensor detects hydrogen peroxide, and wherein a is to repair containing NiS in 0.1MNaOH solution
The time current curve of electrode detection various concentration hydrogen peroxide is adornd, b is the linear relationship of hydrogen peroxide peak point current and respective concentration.
Specific embodiment
The present invention is further analyzed with attached drawing combined with specific embodiments below.
Embodiment 1:
It is a kind of that nanometer nickel sulfide material is prepared and the electrochemistry biography for detecting hydrogen peroxide based on novel one step of electrodeposition process
The preparation method of sensor
(1) glass-carbon electrode after grinding homogeneity, is successively used into 1,0.3,0.05 μm of partial size of Al on polishing paper2O3Powder is thrown
Light.Then dehydrated alcohol is successively used, glass-carbon electrode is cleaned each 5~10min by deionized water in Ultrasound Instrument.It is used after the completion of cleaning
It is dried with nitrogen.
(2) nickel compound containing and sodium citrate that molar ratio is 2:3 are dissolved in 50ml deionized water and stir 1h.
(3) being added in the mixed liquor obtained in (2) with nickel compound containing molar ratio is the thioacetamide of 5:1 and ultrasound
Obtain reaction solution within 10~15 minutes.
(4) reaction solution is poured into electrolytic cell, connects work station, (Ag/AgCl is ginseng with three-electrode electro Chemical work station
Than electrode, platinum electrode is to electrode, and glass-carbon electrode is working electrode) electro-deposition, the deposition electricity of NiS are carried out with cyclic voltammetry
Position is -0.9mv~0.7mv, sweeps speed 10 periods of scanning with 5mv/s.
(5) glass-carbon electrode is cleaned with ultrapure water, removes foreign ion.
(6) glass-carbon electrode cleaned is shone 30~40 minutes under infrared lamp.
The NiS of synthesis is as shown in figure 1 shown in a and b, and d is energy dispersion X-ray spectrum (EDX), it can be seen that prepared rubs
You are certified as NiS by the nanoparticle than 1:1.
Embodiment 2:
Research of the sodium citrate to the NiS granular size of synthesis is added in electro-deposition substrate
By being operated in embodiment 1, difference is that sodium citrate is not added in step (2), can as shown in figure 1 shown in a and c
Particle diameter to see the NiS that sodium citrate is not added is bigger than adding citric acid sodium.
Embodiment 3:
The chemical property of nanometer nickel sulfide enzyme hydrogen peroxide electrochemical sensor is analyzed
Prepare 0.5mM [Fe (CN)6]3-/4-With the mixed solution of 0.5M KCl, mixed solution is poured into electrolytic cell, is connected
Good berth station, using three electrode work stations, (for Ag/AgCl for reference electrode, platinum electrode is to electrode, and glass-carbon electrode is work electricity
Pole) use cyclic voltammetry to carry out I-V Characteristic Analysis to bare glassy carbon electrode and NiS modified electrode, sweeping speed is 50mv/s, scanning
Current potential is 0~0.8v, and as shown in a of Fig. 2, the redox peaks of bare electrode are 0.225v and 0.153v, corresponds to Fe3+/Fe2+
Oxidation-reduction pair, a pair of of Strong oxdiative reduction peak of NiS modified electrode is 0.618v and 0.534v, corresponds to NiS/NiSOH
Oxidation-reduction pair, the reduction of a pair of of weak oxide is to being 0.465v and 0.432v, corresponding to Fe3+/Fe2+Oxidation-reduction pair.
The kinetics that the NiS modified electrode in addition to CV is further studied using EIS, using equivalent circuit diagram and soft
Part is fitted to obtain nyquist plot, and as shown in the b of Fig. 2, it is 208.30 Ω that analysis, which obtains NiS modified electrode electronics transfer impedance,
cm-2, than 18.83 Ω cm of bare electrode-2Much bigger, this may be that NiS modified electrode electric conductivity compared with bare electrode is weaker, from
And hinder electron transmission.
Embodiment 4:
Influence of the electro-deposition concentration of substrate to NiS electrocatalysis characteristic
Nickel compound containing, sodium citrate, NaOH (0.1mol), thioacetamide are prepared respectively；Nickel compound containing, NaOH
(0.1mol), thioacetamide；Double nickel compound containing, double sodium citrate, NaOH, the electro-deposition substrate of thioacetamide are molten
Liquid, a, b, c in corresponding diagram 3.3 kinds of substrates are poured into electrolytic cell respectively, connect work station, using three electrode work stations
(Ag/AgCl is reference electrode, and platinum electrode is to electrode, and glass-carbon electrode is working electrode) repairs NiS using cyclic voltammetry
It adorns electrode and carries out I-V Characteristic Analysis, sweeping speed is 50mv/s, and scanning current potential is 0~0.8v, as shown in a and b in Fig. 3, in substrate
The oxidation peak current that the NiS for having sodium citrate to obtain is catalyzed hydrogen peroxide is big, this is because the NiS particle that adding citric acid sodium obtains
Size is small, and large specific surface area, electron transmission efficiency is higher, and as shown in Figure 3c, the NiS that double concentration of substrate obtains is to hydrogen peroxide
Oxidation peak current it is small compared with a, this is because the NiS particle size that double concentration of substrate obtains is larger, electron transmission efficiency is reduced.
Embodiment 5:
The detection range and detection limit of nanometer nickel sulfide enzyme hydrogen peroxide sensor are probed into
Compound concentration is 1 μm of ol/L, 5 μm of ol/L, 10 μm of ol/L, 100 μm of ol/L, 200 μm of ol/L, 500 μm of ol/L, 1000
The hydrogen peroxide solution of μm ol/L, the hydrogen peroxide of this series of concentrations is poured into electrolytic cell, add 0.1MNaOH, magnetic force respectively
After five minutes, connection work station uses three electrode work stations, and (for Ag/AgCl for reference electrode, platinum electrode is to electrode, glass for stirring
Carbon electrode is working electrode) NiS modified electrode is analyzed using chronoamperometry, as shown in fig. 4 a, in reaction solution
The concentration of hydrogen peroxide increases, and corresponding electric current is gradually increased.Fig. 4 b illustrates the line of hydrogen peroxide concentration and corresponding peak point current
Sexual intercourse, it is seen that the sensor has the preferable range of linearity in 1 μM~1000 μM, and detection is limited to 0.3 μM.
Above-described embodiment is not for limitation of the invention, and the present invention is not limited only to above-described embodiment, as long as meeting
The present invention claims all belong to the scope of protection of the present invention.
Claims (1)
1. a kind of hydrogen peroxide electrochemical sensor based on nanometer nickel sulfide enzyme, it is characterised in that be prepared into using following methods
It arrives:
(1) glass-carbon electrode after grinding homogeneity, is successively used into 1,0.3,0.05 μm of partial size of Al on polishing paper2O3Powder polishing；So
Use dehydrated alcohol respectively afterwards, glass-carbon electrode is cleaned each 3~5min by deionized water in Ultrasound Instrument；With being dried with nitrogen；
(2) nickel compound containing and sodium citrate that molar ratio is 2:3 are dissolved in 50ml deionized water and stir 1h；
(3) thioacetamide and ultrasound 10 that addition and nickel compound containing molar ratio are 5:1 in the mixed liquor obtained in (2)~
15min obtains reaction solution；
(4) with three-electrode electro Chemical work station, (Ag/AgCl is reference electrode, and platinum electrode is to electrode, and glass-carbon electrode is work
Electrode) with cyclic voltammetry carry out electro-deposition, the sedimentation potential of NiS is -0.9mv~0.7mv, sweeps speed scanning 10 with 5mv/s
A period；
(5) glass-carbon electrode is cleaned with ultrapure water, removes foreign ion；
(6) glass-carbon electrode cleaned is shone 30~40 minutes under infrared lamp.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
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