CN112858427B - Nickel monoatomic anchoring carbon-nitrogen material modified electrode and preparation method and application thereof - Google Patents
Nickel monoatomic anchoring carbon-nitrogen material modified electrode and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nickel monatomic anchoring carbon-nitrogen material modified electrode and a preparation method and application thereof, and belongs to the technical field of sensors. The preparation method of the nickel monatomic anchoring carbon-nitrogen material modified electrode comprises the following steps: dissolving nickel salt and 2,3,5, 6-tetra (amino) p-benzoquinone in an organic solvent, and performing ultrasonic dispersion to obtain a mixed solution; adding carbon black into the mixed solution to obtain a dispersion liquid; heating the dispersion to obtain a black solid; grinding the black solid, heating the black solid at a high temperature, and cooling to obtain a Ni monatomic catalyst; dispersing the nickel monoatomic carbon nitride material modified electrode in an ethanol water solution, adding a Nafion solution, uniformly mixing to obtain a nickel monoatomic suspension, dripping the suspension on the surface of a conductive substrate, and drying to obtain the nickel monoatomic carbon nitride material modified electrode. The invention optimizes the deposition potential and deposition time to ensure that H is2O2The detection limit of the sensor can reach the magnitude of pM, and the prepared sensor shows good stability.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to a nickel monatomic anchoring carbon-nitrogen material modified electrode and a preparation method and application thereof.
Background
Hydrogen peroxide (H)2O2) Is a common representative active oxygen, is a byproduct of cell metabolism, and plays a role in turning off in the process of biological consumptionThe important role is. In cellular metabolism, the appropriate amount of H2O2Essential for cell proliferation, differentiation and protein synthesis; and excess of H2O2Can disrupt cell homeostasis and cause cell damage, which can lead to a range of diseases including alzheimer's disease, cardiovascular disease and cancer, among others, and pose potential threats to human health. Therefore, there is an urgent need to develop a rapid, accurate and sensitive assay for H2O2The method of (1). Currently, a number of analytical methods have been used to detect H2O2For example, chemiluminescence, photometry, high performance liquid chromatography, electrochemical methods, and the like. In recent years, electrochemical methods have attracted much attention because of their ease of operation, high response speed, and high sensitivity. Wherein the working electrode is used as the core of the electrochemical sensor. Thus, the performance of an electrochemical sensor depends on efficient electron transport between the electrode and the target molecule. In recent years, a monatomic catalyst has received much attention, and exhibits atom-dispersed active sites on a carrier, which allows better atom utilization efficiency and excellent electron transport activity, as compared to nanoparticles. However, no modification of the electrode with a nickel (Ni) monoatomic anchoring carbon nitrogen material has been found and used for detecting hydrogen peroxide.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a nickel monatomic anchoring carbon-nitrogen material modified electrode.
The invention also aims to provide the nickel monoatomic anchoring carbon-nitrogen material modified electrode prepared by the preparation method.
The invention further aims to provide application of the nickel monoatomic anchoring carbon-nitrogen material modified electrode.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a nickel monatomic anchoring carbon-nitrogen material modified electrode comprises the following steps:
(1) dissolving nickel salt and 2,3,5, 6-tetra (amino) p-benzoquinone in an organic solvent, and performing ultrasonic dispersion to obtain a mixed solution;
(2) adding carbon black into the mixed solution obtained in the step (1), stirring and heating to obtain a dispersion liquid;
(3) heating the dispersion liquid obtained in the step (2) to obtain a black solid;
(4) grinding the black solid obtained in the step (3), heating the black solid at a high temperature, and cooling to obtain a Ni single atom catalyst (Ni-SAC) loaded on carbon black;
(5) and (3) dispersing the Ni monatomic catalyst obtained in the step (4) in an ethanol water solution, adding a Nafion solution, uniformly mixing to obtain a nickel monatomic suspension, dripping the suspension on the surface of a conductive substrate, and drying to obtain the nickel monatomic anchoring carbon nitrogen material modified electrode (namely the Ni-SAC electrode).
The nickel salt in step (1) preferably includes at least one of nickel sulfate, nickel acetate and nickel chloride.
The nickel salt and the 2,3,5, 6-tetra (amino) p-benzoquinone in the step (1) are preferably calculated according to the mass ratio of 11-13: 12-14; more preferably in a mass ratio of 12.4: 13.8.
The organic solvent described in step (1) preferably comprises ethanol.
The preferred mass (mg) to volume (mL) ratio of the nickel salt to the organic solvent in the step (1) is 11-13: 0.5-6; more preferably in terms of a mass (mg) to volume (mL) ratio of 12.4: 2.
The condition of ultrasonic dispersion in the step (1) is preferably ultrasonic dispersion at room temperature for 25-35 min; more preferably, ultrasonic dispersion is carried out for 30min at the temperature of 25-35 ℃.
The carbon black and the nickel acetate in the step (2) are preferably calculated according to the mass ratio of 65-75: 10-15; more preferably as 69.6: 12.4.
The stirring in the step (2) is preferably magnetic stirrer stirring.
The heating in step (2) is preferably oil bath heating; the heating temperature of the oil bath is preferably 50-70 ℃; more preferably 55-65 ℃; most preferably 60 deg.c.
The heating time in the step (2) is preferably 1-5 h; more preferably 2-4 h; most preferably 3 hours.
The heating temperature in the step (3) is 60-100 ℃, and the time is 13-17 h; more preferably, the temperature is 80 ℃ and the time is 15 h. Under the heating condition, ethanol can be effectively evaporated to obtain black solid.
Preferably, the high-temperature heating treatment in the step (4) is carried out by heating to 550 ℃ in an argon atmosphere and preserving the heat for 2 hours; more preferably at a rate of 10 ℃/min to 550 ℃ and then held at 550 ℃ for 2 h.
The degree of cooling described in step (4) is preferably to room temperature.
The mass (mg) volume (mL) ratio of the Ni monatomic catalyst and the ethanol aqueous solution in the step (5) is preferably 1-2: 1.
The water and the ethanol in the ethanol water solution in the step (5) are preferably calculated according to the volume ratio of 1: 0.5-2; more preferably in a volume ratio of 1: 1.
The Nafion solution and the ethanol water solution in the step (5) are preferably calculated according to the volume ratio of 5-15: 1000; more preferably as 10: 1000.
The concentration of the Nafion solution in the step (5) is preferably 4-6 wt%; more preferably 5 wt%.
The uniformly mixing in the step (5) is preferably uniformly mixed by ultrasonic dispersion; the time for ultrasonic dispersion and uniform mixing is preferably 30 min.
The preferable dosage of the suspension liquid in the step (5) on the surface of the conductive substrate is 25-50 mu L/cm2。
The conductive substrate in step (5) preferably comprises at least one of a glassy carbon electrode, a carbon rod electrode and a titanium electrode.
A nickel monatomic anchoring carbon-nitrogen material modified electrode is prepared by the preparation method.
The nickel monoatomic electrode anchored with carbon and nitrogen material modified electrode is used for detecting H2O2The use of (1).
The method for detecting H by using the nickel monoatomic anchored carbon-nitrogen material modified electrode2O2The principle of (1) is as follows: the hydrogen peroxide is decomposed at an accelerated rate in the electrocatalytic process, so that a redox reaction occurs. And get lostAnd displaying an electrochemical signal on an electrochemical workstation so as to finish quantitative detection of the hydrogen peroxide. The Ni-SAC solves the problem of low utilization rate of the heterogeneous catalyst, and increases the active sites of atoms, thereby presenting good performance for electrochemical detection of hydrogen peroxide.
Compared with the prior art, the invention has the following advantages and effects:
(1) compared with nano particles, the single-atom catalyst shows active sites with dispersed atoms on a carrier by introducing nickel single atoms to load on the non-metallic carbon black, so that the single-atom catalyst has better atom utilization efficiency and excellent electron transport activity.
(2) The invention optimizes the deposition potential and deposition time to ensure that H is2O2The detection limit of the sensor can reach the magnitude of pM, and the prepared sensor shows good stability.
(3) And conventional detection H2O2Compared with the methods such as high performance liquid chromatography and chemiluminescence, the method of the invention has the characteristics of simple operation and rapid detection.
Drawings
FIG. 1 is a process diagram of the preparation of a nickel monatomic anchoring carbon nitrogen material modified electrode.
FIG. 2 is a graph showing the results of measuring the performance of different electrodes in example 1; FIG. 2A is a Ni-SAC high angle annular dark field image scanning transmission electron microscope (HAADF-STEM) result graph; FIG. 2B is a graph of the X-ray absorption near edge structure (XANES) spectra of NiO, nickel foil (i.e., Ni foil), and Ni-SAC; FIG. 2C is an extended X-ray absorption fine structure (EXAFS) spectrum of NiO, nickel foil (i.e., Ni foil), and Ni-SAC; FIG. 2D is a Ni-SAC and Ni-SAC fitted extended X-ray absorption fine structure (EXAFS) spectra.
FIG. 3 shows CB, Ni (OH) in a three-electrode system2And a nickel monoatomic electrode (Ni-SAC electrode) modified by anchoring carbon and nitrogen materials in 0.1M NaOH solution to detect 2mM H2O2Differential pulse voltammetry profile of (a).
FIG. 4 shows the results of example 3 in which a Ni-SAC electrode (Ni-SAC electrode) as an electrochemical sensor was coated with a 0.1M NaOH solutionDetection of H2O2Differential pulse voltammetry profile of the detection limit of (1).
FIG. 5 shows the results of the electrochemical sensor of example 4 using a modified electrode (Ni-SAC electrode) made of a nickel monoatomic anchoring carbon nitride material for 2mM H in a 0.1M NaOH solution2O2And repeatedly scanning a differential pulse voltammogram result graph for 100 circles.
FIG. 6 shows the measurement of H in calf serum using a modified electrode (Ni-SAC electrode) with a nickel monoatomic carbon nitride material as an electrochemical sensor in example 52O2The detection result chart of (1).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
A preparation method of a nickel monatomic anchoring carbon nitrogen material modified electrode is shown in figure 1, and specifically comprises the following steps:
(1) dissolving 12.4mg of nickel acetate and 13.8mg of 2,3,5, 6-tetra (amino) p-benzoquinone in 2mL of ethanol, and performing ultrasonic dispersion at room temperature for 30min to obtain a mixed solution;
(2) adding 69.6mg of carbon black into the mixed solution obtained in the step (1), and heating in an oil bath at 60 ℃ for 3h under magnetic stirring to obtain a dispersion liquid;
(3) heating the dispersion liquid obtained in the step (2) at 80 ℃ for 15h, thereby evaporating ethanol to obtain a black solid;
(4) slightly grinding the black solid obtained in the step (3), placing the black solid in a tube furnace, heating the black solid to 550 ℃ at the speed of 10 ℃/min in the argon atmosphere, then keeping the temperature at 550 ℃ for 2h, and cooling the black solid to room temperature to obtain a Ni single atom catalyst (Ni-SAC) loaded on carbon black;
(5) dispersing 2mg of Ni-SAC obtained in step (4) in 1mL of an aqueous ethanol solution (V)Ethanol:VWater (W)To 1:1) 10 μ L Nafion solution (5 wt%, available from Sigma, cat #: 274704), ultrasonic dispersing for 30min to obtain nickel monoatomic suspension, and applying 5 μ L of the suspension onto glassy carbon electrode (diameter 3mm) by using micro liquid feederAnd naturally airing the surface in the air to obtain the nickel monoatomic electrode anchored with the carbon and nitrogen material modified electrode (Ni-SAC electrode).
The Ni foil, NiO, and the Ni monatomic catalyst supported on carbon black obtained in step (4) were subjected to high-angle annular dark field image scanning transmission electron microscope (HAADF-STEM) (fig. 2A), X-ray absorption near edge structure (XANES) (fig. 2B), and extended X-ray absorption fine structure (EXAFS) (fig. 2C and 2D), respectively, and the results are shown in fig. 2. Specific results are described below:
as can be seen from fig. 2A, the nickel monatomic catalysts are all dispersed. As can be seen from FIG. 2B, for the Ni monatomic catalyst supported on carbon black (Ni-SAC), the absorption edge was slightly higher than the Ni foil and slightly lower than NiO, indicating that Ni in the Ni-SAC exhibits a cationic form (possibly +2 valency); as can be seen from FIG. 2C, the Ni monatomic sample is approximately at
Shows a strong peak, which corresponds to Ni-N coordination; as can be seen from fig. 2D, one Ni atom coordinates to 4N atoms; the above results are sufficient to indicate that Ni monatomic catalyst (Ni-SAC) supported on carbon black was successfully produced.
Example 2
H in NaOH solution was detected using the nickel monoatomic electrode anchored carbon nitrogen material modified electrode (Ni-SAC electrode) prepared in example 1 as an electrochemical sensor2O2Sensors with other references (CB, Ni and Ni (OH))2) As a control; in the detection process, the nickel monoatomic anchoring carbon nitrogen material modified electrode is used as an electrochemical sensor, and Differential Pulse Voltammetry (DPV) is used for reduction scanning in the detection process to enable H to be generated2O2The current-voltage curve of this process is decomposed and recorded.
The specific detection steps are as follows: firstly, grinding and polishing the glassy carbon electrode on alumina polishing powder with the particle size of 50nm, and then sequentially carrying out ultrasonic washing by deionized water and absolute ethyl alcohol; in a three-electrode system, a platinum wire electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, CB, Ni and Ni (OH)2And nickel monoatomic anchoring carbon nitrogen material modified electrode (Ni-SAC electrode)) Respectively as working electrode, containing 2mM H2O2The 0.1M NaOH solution is used as a supporting electrolyte solution, an electrochemical workstation is used as a detection instrument, and current-voltage scanning detection is carried out by means of differential pulse voltammetry, wherein detection parameters of the differential pulse voltammetry are as follows: the deposition potential was 0.0V and the deposition time was 150 s.
The results are shown in FIG. 3. As seen in fig. 3: detection of H by using nickel monoatomic anchoring carbon nitrogen material modified electrode (Ni-SAC electrode)2O2The peak value of the electrode is far higher than that of other working electrodes, which shows that the nickel monoatomic anchoring carbon nitrogen material modified electrode (Ni-SAC electrode) prepared by the invention has better detection effect on H in NaOH solution2O2The ability of the cell to perform.
Example 3
The purpose of this example is to detect H in 0.1M NaOH solution by differential pulse voltammetry curve study using a nickel monoatomic electrode modified with carbon nitride material (Ni-SAC electrode) as an electrochemical sensor2O2The detection limit of (2). The specific detection steps are as follows: in a three-electrode system, a platinum wire electrode was used as a counter electrode, a calomel electrode was used as a reference electrode, and the nickel monoatomic anchor carbon nitrogen material modified electrode (Ni-SAC electrode) prepared in example 1 was used as a working electrode, containing H2O2The 0.1M NaOH solution is used as a supporting electrolyte solution, an electrochemical workstation is used as a detection instrument, and current-voltage scanning detection is carried out by means of differential pulse voltammetry, wherein detection parameters of the differential pulse voltammetry are as follows: the deposition potential was 0.0V and the deposition time was 150 s. Wherein H in the supporting electrolyte solution2O2The concentrations were 0pM, 20pM, 220pM, 2.2nM, 22nM, 222nM, 2.22. mu.M, respectively, from low to high.
As a result, as shown in FIG. 4, it can be seen from FIG. 4 that the nickel monoatomic layer-anchored carbon nitride material-modified electrode (Ni-SAC electrode) detects H2O2The detection range of the electrode is 20 pM-2.22 mu M, and the lowest detection limit can reach 20pM, so that the nickel monoatomic anchoring carbon nitrogen material modified electrode (Ni-SAC electrode) prepared by the invention has a lower detection limit and a wide linear range.
Example 4
The purpose of this example is to study the detection of H in 0.1M NaOH solution by using a nickel monoatomic electrode (Ni-SAC electrode) modified with carbon-nitrogen material2O2The specific detection steps of the stability of (1) are as follows: in a three-electrode system, a platinum wire electrode was used as a counter electrode, a calomel electrode was used as a reference electrode, and a nickel monoatomic electrode anchored carbon nitrogen material modified electrode (Ni-SAC electrode) prepared in example 1, containing 2mM H, was used as a working electrode2O2The 0.1M NaOH solution is used as a supporting electrolyte solution, an electrochemical workstation is used as a detection instrument, and current-voltage scanning detection is carried out by means of differential pulse voltammetry, wherein detection parameters of the differential pulse voltammetry are as follows: the deposition potential was 0.0V and the deposition time was 150 s. The entire scanning cycle lasts 100 revolutions.
As a result, as shown in FIG. 5, the nickel monoatomic electrode modified with an anchored carbon nitride material (Ni-SAC electrode) was tested for H100 times in 0.1M NaOH2O2After that, the peak current thereof hardly changes. Therefore, the nickel monoatomic anchoring carbon nitrogen material modified electrode prepared by the method has good stability and can be repeatedly used.
Example 5
The purpose of this example is to study the use of a nickel monatomic anchored carbon nitrogen material modified electrode (Ni-SAC electrode) as an electrochemical sensor for detecting H in calf serum2O2The effect of (1).
Calf serum was purchased from hong quan biotechnology limited, guangzhou and the serum had been centrifuged. Calf serum was diluted 100-fold with 0.1M NaOH solution for electrochemical testing. The specific detection steps are as follows: in a three-electrode system, a platinum wire electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, a nickel monoatomic anchoring carbon nitrogen material modified electrode prepared in the embodiment 1 is used as a working electrode, a glassy carbon electrode is firstly polished on alumina polishing powder with the particle size of 50nm, and then ultrasonic washing is sequentially carried out on the polished electrode by deionized water and absolute ethyl alcohol; the method comprises the following steps of taking calf serum diluted by NaOH solution as supporting electrolyte solution, taking an electrochemical workstation as a detection instrument, and carrying out current-voltage scanning detection by means of differential pulse voltammetry, wherein detection parameters of the differential pulse voltammetry are as follows: the deposition potential is 0.0V,the deposition time was 150 s. The specific operation is as follows: to the diluted calf serum with NaOH solution was added 2. mu. M H2O2After the solution, voltage-current scanning was performed using differential pulse voltammetry.
The results are shown in FIG. 6. As can be seen from FIG. 6, there was a small peak around-0.21V in the calf serum after dilution with NaOH solution, which we could not confirm is H2O22 μ M H was added to calf serum diluted with NaOH solution2O2After that, it can be seen that the peak of-0.21V becomes large. Thus, the nickel monoatomic anchored carbon-nitrogen material modified electrode (Ni-SAC electrode) is used as an electrochemical sensor for H in calf serum2O2Has certain potential.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a nickel monatomic anchoring carbon-nitrogen material modified electrode is characterized by comprising the following steps:
(1) dissolving nickel salt and 2,3,5, 6-tetra (amino) p-benzoquinone in an organic solvent, and performing ultrasonic dispersion to obtain a mixed solution;
(2) adding carbon black into the mixed solution obtained in the step (1), stirring and heating to obtain a dispersion liquid;
(3) heating the dispersion liquid obtained in the step (2) to obtain a black solid;
(4) grinding the black solid obtained in the step (3), heating the black solid at a high temperature, and cooling to obtain a Ni monatomic catalyst (Ni-SAC) loaded on carbon black;
(5) and (3) dispersing the Ni monatomic catalyst obtained in the step (4) in an ethanol water solution, adding a Nafion solution, uniformly mixing to obtain a nickel monatomic suspension, dripping the suspension on the surface of a conductive substrate, and drying to obtain the nickel monatomic anchoring carbon nitrogen material modified electrode, namely the Ni-SAC electrode.
2. The method according to claim 1, wherein the nickel salt in step (1) comprises at least one of nickel sulfate, nickel acetate and nickel chloride;
the nickel salt and the 2,3,5, 6-tetra (amino) p-benzoquinone in the step (1) are calculated according to the mass ratio of 11-13: 12-14.
3. The production method according to claim 1,
the organic solvent in the step (1) comprises ethanol;
calculating the ratio of the nickel salt to the organic solvent in the step (1) according to the mass mg volume mL ratio of 11-13: 0.5-6;
the ultrasonic dispersion condition in the step (1) is ultrasonic dispersion for 25-35 min at room temperature.
4. The preparation method according to claim 1, wherein the carbon black and the nickel acetate in the step (2) are calculated according to a mass ratio of 65-75: 10-15;
the heating in the step (2) is oil bath heating; the oil bath heating temperature is 50-70 ℃;
and (3) heating for 1-5 hours in the step (2).
5. The preparation method according to claim 1, wherein the heating in the step (3) is performed at a temperature of 60 to 100 ℃ for 13 to 17 hours;
and (4) heating to 550 ℃ in an argon atmosphere, and keeping the temperature for 2 h.
6. The preparation method according to claim 1, wherein the Ni monatomic catalyst and the ethanol aqueous solution in the step (5) are calculated in a mass mg volume mL ratio of 1-2: 1;
and (3) calculating the volume ratio of water to ethanol in the ethanol aqueous solution in the step (5) to be 1: 0.5-2.
7. The production method according to claim 1,
calculating the Nafion solution and the ethanol water solution in the step (5) according to the volume ratio of 5-15: 1000;
the concentration of the Nafion solution in the step (5) is 4-6 wt%.
8. The production method according to claim 1,
the dosage of the suspension liquid on the surface of the conductive substrate in the step (5) is 25-50 mu L/cm2；
The conductive substrate in the step (5) comprises at least one of a glassy carbon electrode, a carbon rod electrode and a titanium electrode.
9. A nickel monatomic anchored carbon-nitrogen material modified electrode, characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. The nickel monoatomic electrode modified by carbon nitrogen material and anchored as claimed in claim 9 for detecting H2O2The use of (1).
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