CN114577871A - Application of Au/ZnO composite material in photoelectrochemical sensor electrode - Google Patents
Application of Au/ZnO composite material in photoelectrochemical sensor electrode Download PDFInfo
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- 238000001514 detection method Methods 0.000 claims abstract description 21
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 19
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 12
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Abstract
The invention provides an application of an Au/ZnO composite material in a photoelectrochemical sensor electrode. The Au/ZnO composite material provided by the invention is applied to the photoelectrochemical sensor electrode, the local surface plasma resonance of Au nano particles is utilized to widen the absorption light wavelength of wide bandgap semiconductor ZnO, so that the photoelectric property of the ZnO material is improved, and the Au/ZnO composite material can realize specific response and high-sensitivity detection on 4-nitrophenol (PNP) after being applied to a photoelectrochemical sensor.
Description
Technical Field
The invention relates to the technical field of photoelectrochemical detection, in particular to application of an Au/ZnO composite material in an electrode of a photoelectrochemical sensor.
Background
4-nitrophenol (PNP) is an important intermediate raw material, and plays an important role in chemical production of pesticides, medicines and the like. However, PNPs are chemically stable and have long half-lives and are long-lived in the environment, so that since the environment is severely damaged by the large amount of PNPs used in production, EPA and EEA have listed PNPs in the list of industrial wastewater pollutants which are preferably monitored in 1980 and 2000.
At present, the conventional detection modes of PNP are gas chromatography, high performance liquid chromatography and surface enhanced Raman scattering, and because the instruments and equipment used in the conventional detection modes are large and expensive, the operation cost is high, potential safety hazards exist, the detection timeliness is not strong, and the online detection is difficult to realize. Although researchers have developed fluorescence, electrochemistry, electrophoresis and other detection methods, these methods also have the disadvantages of insufficient detection limit and insufficient rapid transient response, and therefore, it is necessary to develop another transient detection method with high sensitivity and low detection limit.
The photocatalytic technology is considered to be one of the most promising technologies for solving the problem of environmental pollution in the next 50 years, and reports show that the photocatalytic degradation of 4-nitrophenol has been widely researched, so that a photoelectrochemical sensor combining photocatalysis and electrocatalysis brings a new opportunity for accurate analysis of 4-nitrophenol.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the application of the Au/ZnO composite material in the photoelectrochemical sensor electrode, the light absorption wavelength of the wide bandgap semiconductor ZnO is widened by utilizing the local surface plasma resonance of Au nano particles, so that the photoelectric property of the ZnO material is improved, and when the Au/ZnO composite material is used in the photoelectrochemical sensor, the specific response and the high-sensitivity detection on the 4-nitrophenol can be realized.
The invention provides an application of an Au/ZnO composite material in a photoelectrochemical sensor electrode.
Preferably, the particle size of the Au nanoparticles is 2 to 10 nm.
The invention also provides a photoelectrochemical sensor electrode which comprises the Au/ZnO composite material and an ITO substrate, wherein the Au/ZnO composite material is uniformly loaded on the surface of the ITO substrate.
Preferably, the preparation method of the electrode comprises the following steps:
s1, mixing Au source with ZnSe.0.5N2H4Nano-belt mixing reaction to obtain Au/ZnSe.0.5N2H4A composite material;
s2, mixing Au/ZnSe.0.5N2H4The composite material is assembled on the ITO surface to obtain Au/ZnSe.0.5N2H4And calcining the/ITO composite material to obtain the photoelectrochemical sensor electrode.
Preferably, step S1 specifically includes: adding HAuCl4Adding the aqueous solution of (A) to ZnSe.0.5N2H4Mixing the nanometer belt with ethanol solution, stirring at 10-50 deg.C, and reacting for 30-60min to obtain Au/ZnSe.0.5N2H4A composite material;
preferably, HAuCl4And ZnSe.0.5N2H4The molar ratio of the nanoribbons is not more than 0.03:1, preferably 0.01: 1.
Preferably, step S2 specifically includes: mixing Au/ZnSe.0.5N2H4Dispersing the composite material in a mixed solution of N, N-dimethylformamide and chloroform, assembling the composite material on the ITO surface by adopting a Langmuir-Blodgett self-assembly method, and drying the ITO surface for 10min at the temperature of between 40 and 60 ℃ to obtain Au/ZnSe.0.5N2H4And calcining the ITO composite material at the temperature of 350-580 ℃ for 30-60min to obtain the Au/ZnO/ITO composite material, namely the photoelectrochemical sensor electrode.
Preferably, the calcination specifically comprises: heating to 400 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 20-40min, heating to 580 ℃ at a heating rate of 1-3 ℃/min, and preserving heat for 10-20 min.
The invention provides a photoelectrochemical sensor which comprises the photoelectrochemical sensor electrode.
Preferably, the sensor consists of three electrodes, the working electrode is the photoelectrochemical sensor electrode, the counter electrode is a Pt wire electrode, and the reference electrode is a saturated Ag/AgCl electrode.
Preferably, the photoelectrochemical sensor is for the detection of 4-nitrophenol.
The invention provides an application of an Au/ZnO composite material in a photoelectrochemical sensor electrode. After the Au nano-particles are modified, the photoelectric property of the ZnO semiconductor material is greatly improved due to the local surface plasma effect of the noble metal and the metal oxide, so that when the Au/ZnO composite material is used for a photoelectrochemical sensor and an electrode thereof, the detection sensitivity of the Au/ZnO composite material to 4-nitrophenol can be improved through the cooperative sensitivity enhancement mechanism of the noble metal nano-particles and the porous nano-structure.
Compared with the traditional detection method, when the Au/ZnO composite material is used for the photoelectrochemical sensor electrode and a photoelectrochemical method is adopted to detect the 4-nitrophenol, the latter can realize the transient response, save the detection time and is convenient to operate. The sensor has high sensitivity and low detection line (0.06 mu M) for detecting 4-nitrophenol, good stability and wide linear range (0.2-67.6 mu M) through testing.
Drawings
FIG. 1 is a schematic diagram of the construction process of the electrode of the photoelectric sensor according to the present invention.
FIG. 2 is a schematic diagram of a 4-nitrophenol photoelectric sensing process of the photoelectrochemical sensor electrode pair of the present invention.
FIG. 3 is an SEM image of an electrode of a photoelectrochemical sensor according to the present invention; (a) is Au/ZnSe 0.5N obtained in example 12H4SEM images of the composite; (b) is an SEM image of the photoelectrochemical sensor electrode obtained in comparative example 1; (c) is an SEM photograph of the photoelectrochemical sensor electrode obtained in example 2; (d) is an SEM photograph of the photoelectrochemical sensor electrode obtained in example 1; (e) is an SEM photograph of the photoelectrochemical sensor electrode obtained in example 3; (f) is an SEM photograph of the electrode of the photoelectrochemical sensor obtained in example 4.
FIG. 4 is a graph showing UV-VIS absorption spectra of the electrodes of the photoelectrochemical sensors obtained in example 1 of the present invention and comparative example 1.
FIG. 5 is a diagram of an optimized test of photoelectric properties of the photoelectrochemical sensor electrode of the present invention; (a) the photocurrent curves of the photoelectrochemical sensor electrodes obtained in the examples and the comparative examples under different Au loading amounts are shown; (b) the photoelectric current line graphs of the photoelectrochemical sensor electrode obtained in the example 1 under different electron donor TEOA concentrations; (c) is a light current line graph of the photoelectrochemical sensor electrode obtained in the example 1 under different calcination temperatures.
FIG. 6 is an SEM photograph of an electrode of a photoelectric chemical sensor obtained in example 5 of the present invention.
FIG. 7 is a photoelectrochemical test pattern of an electrode of the photoelectrochemical sensor of the present invention; (a) i-t graphs of photocurrent versus time for different concentrations of 4-nitrophenol when the electrode obtained in example 1 was used in a photoelectrochemical sensor; (b) the linear relationship graph of the photocurrent and the concentration of the electrode obtained in example 1 for different concentrations of 4-nitrophenol when the electrode is used in a photoelectrochemical sensor is shown; (c) the anti-interference test chart of the electrode obtained in the embodiment 1 when the electrode is used for a photoelectrochemical sensor is shown; (d) the electrode stability test chart of the electrode obtained in example 1 when used in a photoelectrochemical sensor was shown.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
Referring to fig. 1, the present embodiment provides a photoelectrochemical sensor electrode, and a method for manufacturing the photoelectrochemical sensor electrode includes the following steps:
(1) adding 0.01mol/L zinc chloride aqueous solution (0.2mmol ZnCl) into 0.02mol/L selenium powder solution (obtained by dissolving 0.4mmol Se powder in 20mL 80 wt% hydrazine hydrate solution)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain ZnSe.0.5N)2H4A nanoribbon;
(2) adding 0.2mmol ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, and slowly adding 400 μ L HAuCl with concentration of 5mmol/L4Stirring the solution for reaction for 30min, washing with water and ethanol for 5 times, and drying to obtain 1 at% Au/ZnSe.0.5N2H4A composite material;
(3) 0.2mmol Au/ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, and washing with deionized water five timesThen, the mixture was washed with N, N-dimethylformamide three times, and the obtained solid was dispersed in 1mL of a mixed solvent composed of N, N-dimethylformamide and chloroform in a volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) adopting Langmuir-Blodgett assembly technology to assemble the Au/ZnSe.0.5N2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is ultrasonically cleaned for 5min by acetone, ethanol and water respectively, water stain is blown by nitrogen, and then the ITO substrate is placed in an L-B self-assembly tank, wherein 10 mu LAu/ZnSe.0.5N is treated every time2H4Dripping the dispersion liquid on the surface of ITO, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, wherein Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying at 50 ℃ for 10min to obtain Au/ZnSe.0.5N2H4An ITO composite material;
(5) mixing Au/ZnSe.0.5N2H4the/ITO composite material is placed in a muffle furnace, an Au/ZnO/ITO electrode is obtained by a two-stage program heating method, specifically, the temperature is increased to 350 ℃ at the heating rate of 2 ℃/min, and is maintained for 30min, then the temperature is increased to 500 ℃ at the heating rate of 1 ℃/min, and is maintained for 10min, and the photoelectrochemical sensor electrode is obtained.
For Au/ZnSe 0.5N obtained in example 12H4The composite material and the photoelectrochemical sensor electrode are respectively detected by a scanning electron microscope, and the results are shown in figure 3: FIG. 3(a) shows Au/ZnSe 0.5N obtained in example 12H4As can be seen from the SEM image of the composite material, the presence of Au was not observed under the scanning electron microscope due to the small size of Au nanoparticles, but Au/ZnSe 0.5N was observed2H4The topography of the composite; FIG. 3(d) is the SEM image of the electrode of the photoelectrochemical sensor obtained in example 1, which shows the morphology of the Au/ZnO/ITO electrode of this example, which has a rough porous structure.
Example 2
The embodiment provides a photoelectrochemical sensor electrode, and a preparation method thereof comprises the following steps:
(1) adding 0.4mmol Se powder into selenium powder solution with the concentration of 0.02mol/LDissolved in 20mL of 80 wt% hydrazine hydrate solution) is added dropwise with 0.01mol/L zinc chloride aqueous solution (0.2mmol ZnCl)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain white ZnSe.0.5N)2H4A nanoribbon;
(2) adding 0.2mmol ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, and slowly adding 200 μ L HAuCl with concentration of 5mmol/L4Stirring the solution for reaction for 30min, washing with water and ethanol for 5 times, and oven drying to obtain 0.5 at% Au/ZnSe.0.5N2H4A composite material;
(3) adding 0.2mmol Au/ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, washing the centrifuge tube with deionized water for five times, then washing the centrifuge tube with N, N-dimethylformamide for three times, dispersing the obtained solid in 1mL of mixed solvent consisting of N, N-dimethylformamide and trichloromethane with the volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) adopting Langmuir-Blodgett assembly technology to assemble the Au/ZnSe.0.5N2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is ultrasonically cleaned for 5min by acetone, ethanol and water respectively, water stain is blown by nitrogen, and then the ITO substrate is placed in an L-B self-assembly tank, wherein 10 mu LAu/ZnSe.0.5N is treated every time2H4Dripping the dispersion liquid on the surface of ITO, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, wherein Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying at 50 ℃ for 10min to obtain Au/ZnSe.0.5N2H4An ITO composite material;
(5) mixing Au/ZnSe.0.5N2H4Placing the ITO composite material in a muffle furnace, obtaining an Au/ZnO/ITO electrode by a two-stage programmed heating method, specifically, heating to 350 ℃ at a heating rate of 2 ℃/min, preserving heat for 30min,heating to 500 ℃ at the heating rate of 1 ℃/min, and preserving the heat for 10min to obtain the photoelectrochemical sensor electrode.
Scanning electron microscope detection is performed on the photoelectrochemical sensor electrode obtained in example 2, and the result is shown in fig. 3: FIG. 3(c) is the SEM image of the photoelectrochemical sensor electrode obtained in example 2, which shows that the Au/ZnO/ITO electrode of this example has the morphology characteristics of rough porous structure.
Example 3
The embodiment provides a photoelectrochemical sensor electrode, and a preparation method thereof comprises the following steps:
(1) adding 0.01mol/L zinc chloride aqueous solution (0.2mmol ZnCl) into 0.02mol/L selenium powder solution (obtained by dissolving 0.4mmol Se powder in 20mL 80 wt% hydrazine hydrate solution)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain white ZnSe.0.5N)2H4A nanoribbon;
(2) adding 0.2mmol ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, and slowly adding 600 μ L HAuCl with concentration of 5mmol/L4Stirring the solution for reaction for 30min, washing with water and ethanol for 5 times, and drying to obtain 1.5 at% Au/ZnSe.0.5N2H4A composite material;
(3) adding 0.2mmol Au/ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, washing with deionized water for five times, then washing with N, N-dimethylformamide for three times, dispersing the obtained solid in 1mL of mixed solvent consisting of N, N-dimethylformamide and trichloromethane with the volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) adopting Langmuir-Blodgett assembly technology to assemble the Au/ZnSe.0.5N2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is respectively treated with acetone and acetone BUltrasonically cleaning with alcohol and water for 5min, blowing off water stain with nitrogen, and placing in L-B self-assembled tank, each time adding 10 μ LAu/ZnSe.0.5N2H4Dripping the dispersion liquid on the surface of ITO, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, wherein Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying at 50 ℃ for 10min to obtain Au-ZnSe.0.5N2H4An ITO composite material;
(5) mixing Au/ZnSe.0.5N2H4the/ITO composite material is placed in a muffle furnace, an Au/ZnO/ITO electrode is obtained by a two-stage program heating method, specifically, the temperature is increased to 350 ℃ at the heating rate of 2 ℃/min, and is maintained for 30min, then the temperature is increased to 500 ℃ at the heating rate of 1 ℃/min, and is maintained for 10min, and the photoelectrochemical sensor electrode is obtained.
Scanning electron microscope detection is performed on the photoelectrochemical sensor electrode obtained in example 3, and the result is shown in fig. 3: FIG. 3(e) is the SEM image of the photoelectrochemical sensor electrode obtained in example 3, which shows the morphology of the Au/ZnO/ITO electrode of this example, wherein Au is uniformly dispersed on the surface of ZnO but the nanometer size is very small.
Example 4
The embodiment provides a photoelectrochemical sensor electrode, and a preparation method thereof comprises the following steps:
(1) adding 0.01mol/L zinc chloride aqueous solution (0.2mmol ZnCl) into 0.02mol/L selenium powder solution (obtained by dissolving 0.4mmol Se powder in 20mL 80 wt% hydrazine hydrate solution)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain white ZnSe.0.5N)2H4A nanoribbon;
(2) adding 0.2mmol ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, and slowly adding 1200 μ L HAuCl with concentration of 5mmol/L4Stirring the solution for reaction for 30min, washing with water and ethanol for 5 times, and drying to obtain 3 at% Au/ZnSe.0.5N2H4A composite material;
(3) adding 0.2mmol Au/ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, washing with deionized water for five times, then washing with N, N-dimethylformamide for three times, dispersing the obtained solid in 1mL of mixed solvent consisting of N, N-dimethylformamide and trichloromethane with the volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) adopting Langmuir-Blodgett assembly technology to assemble the Au/ZnSe.0.5N2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is ultrasonically cleaned for 5min by acetone, ethanol and water respectively, water stain is blown by nitrogen, and then the ITO substrate is placed in an L-B self-assembly tank, wherein 10 mu LAu/ZnSe.0.5N is treated every time2H4Dripping the dispersion liquid on the ITO surface, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, and adding Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying at 50 ℃ for 10min to obtain Au/ZnSe.0.5N2H4An ITO composite material;
(5) mixing Au-ZnSe.0.5N2H4the/ITO composite material is placed in a muffle furnace, an Au/ZnO/ITO electrode is obtained by a two-stage program heating method, specifically, the temperature is increased to 350 ℃ at the heating rate of 2 ℃/min, and is maintained for 30min, then the temperature is increased to 500 ℃ at the heating rate of 1 ℃/min, and is maintained for 10min, and the photoelectrochemical sensor electrode is obtained.
The photoelectrochemical sensor electrode obtained in example 4 was subjected to scanning electron microscope detection, and the results are shown in fig. 3: fig. 3(f) is an SEM image of the photoelectrochemical sensor electrode obtained in example 4, which shows that the Au/ZnO/ITO electrode of this example has morphology features in which Au is uniformly dispersed on the surface of ZnO and the nano-size is relatively significant.
Example 5
The embodiment provides a photoelectrochemical sensor electrode, and a preparation method thereof comprises the following steps:
(1) adding selenium powder solution (obtained by dissolving 0.4mmol Se powder in 20mL 80 wt% hydrazine hydrate solution) with concentration of 0.02mol/L dropwise0.01mol/L aqueous zinc chloride solution (0.2mmol ZnCl)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain white ZnSe.0.5N)2H4A nanoribbon;
(2) adding 0.2mmol ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, and slowly adding 1200 μ L HAuCl with concentration of 5mmol/L4Stirring the solution for reaction for 30min, washing with water and ethanol for 5 times, and drying to obtain 5 at% Au/ZnSe.0.5N2H4A composite material;
(3) adding 0.2mmol Au/ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, washing the centrifuge tube with deionized water for five times, then washing the centrifuge tube with N, N-dimethylformamide for three times, dispersing the obtained solid in 1mL of mixed solvent consisting of N, N-dimethylformamide and trichloromethane with the volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) the Au/ZnSe.0.5N is assembled by adopting a Langmuir-Blodgett assembly technology2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is ultrasonically cleaned for 5min by acetone, ethanol and water respectively, water stain is blown by nitrogen, and then the ITO substrate is placed in an L-B self-assembly tank, wherein 10 mu LAu/ZnSe.0.5N is treated every time2H4Dripping the dispersion liquid on the surface of ITO, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, wherein Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying for 10min at 50 ℃ to obtain Au/ZnSe.0.5N2H4An ITO composite material;
(5) mixing Au/ZnSe.0.5N2H4Placing the ITO composite material in a muffle furnace, obtaining an Au/ZnO/ITO electrode by a two-stage programmed heating method, specifically, heating to 350 ℃ at a heating rate of 2 ℃/min, preserving heat for 30min, heating to 500 ℃ at a heating rate of 1 ℃/min, and preserving heat for 1And 0min is the photoelectrochemical sensor electrode.
Comparative example 1
The comparative example provides a photoelectrochemical sensor electrode, and the preparation method thereof comprises the following steps:
(1) adding 0.01mol/L zinc chloride aqueous solution (0.2mmol ZnCl) into 0.02mol/L selenium powder solution (obtained by dissolving 0.4mmol Se powder in 20mL 80 wt% hydrazine hydrate solution)2Dissolving in 20mL of ultrapure water), stirring and mixing for 1h, performing hydrothermal reaction at 180 ℃ for 12h, centrifugally washing and precipitating with hydrazine hydrate for 3 times to remove excessive selenium powder, centrifugally washing and precipitating with water to neutrality, and finally washing and precipitating with ethanol for 2 times to remove water to obtain white ZnSe.0.5N)2H4A nanoribbon;
(2) 0.2mmol of ZnSe.0.5N2H4Dissolving the nanobelt in 70mL ethanol solution, stirring for 10min, sequentially washing with water and ethanol for 5 times, and oven drying to obtain ZnSe.0.5N2H4A material;
(3) 0.2mmol of ZnSe.0.5N2H4Dissolving the composite material in 10mL of ethanol solution, fully dispersing, adding 1mL of the obtained solution into a 1.5mL centrifuge tube, washing with deionized water for five times, then washing with N, N-dimethylformamide for three times, dispersing the obtained solid in 1mL of mixed solvent consisting of N, N-dimethylformamide and trichloromethane with the volume ratio of 1:1 to obtain Au/ZnSe.0.5N2H4A dispersion liquid;
(4) adopting Langmuir-Blodgett assembly technology to carry out ZnSe.0.5N2H4The composite material is uniformly assembled on the ITO surface, specifically, the ITO substrate is ultrasonically cleaned for 5min by acetone, ethanol and water respectively, water stain is blown by nitrogen, and then the ITO substrate is placed in an L-B self-assembly tank, wherein 10 mu LAu/ZnSe.0.5N is treated every time2H4Dripping the dispersion liquid on the surface of ITO, after the dispersion liquid is dispersed into a layer of compact film, extracting ultrapure water in the self-assembly tank, wherein Au/ZnSe.0.5N2H4Transferring the composite material to the surface of an ITO electrode, and drying at 50 ℃ for 10min to obtain ZnSe.0.5N2H4An ITO composite material;
(5) zn is addedSe·0.5N2H4And (2) placing the/ITO composite material in a muffle furnace, obtaining a ZnO/ITO electrode by a two-stage program heating method, specifically, heating to 350 ℃ at a heating rate of 2 ℃/min, preserving heat for 30min, heating to 500 ℃ at a heating rate of 1 ℃/min, and preserving heat for 10min to obtain the photoelectrochemical sensor electrode.
Scanning electron microscope detection is performed on the photoelectrochemical sensor electrode obtained in comparative example 1, and the result is shown in fig. 3: FIG. 3(b) is an SEM image of the photoelectrochemical sensor electrode obtained in comparative example 1, from which it can be seen that the ZnO/ITO electrode of the comparative example has morphological characteristics and shows a porous nanobelt structure.
The results of measuring the uv-vis spectra of the electrodes obtained in example 1 and comparative example 1 are shown in fig. 4, fig. 4 is a uv-vis absorption spectrum of the photoelectrochemical sensor electrode obtained in example 1 and comparative example 1, and it can be seen from the graph that the electrode in example 1 widens the light absorption range of ZnO from the uv region (occupying only 5% of sunlight) to the visible region due to the localized surface plasmon effect of Au nanoparticles and ZnO semiconductor.
And (3) performance testing:
optimization of photoelectric properties
When the photoelectrochemical sensor electrodes obtained in the embodiments and the comparative examples are used for a photoelectrochemical sensor, the specific method is that a copper wire is led out from the surface of the electrode, the electrode is subjected to end-capping treatment by utilizing silver paste, the copper wire is ensured to be tightly connected with the surface of the electrode, the electrode is dried for 24 hours at room temperature, the silver paste is ensured to be dried, then end-capping protection is carried out on the silver paste by utilizing AB glue, and the electrode for the photoelectrochemical sensor is obtained after the electrode is dried for 12 hours at room temperature;
placing the electrode for the photoelectrochemical sensor as a working electrode in a photoelectrochemical system of a xenon lamp-electrochemical workstation for photoelectrochemical test, taking a 7ILX500C xenon lamp purchased from Saifen photoelectricity as a light source, taking a platinum (Pt) wire as a counter electrode, taking a saturated Ag/AgCl electrode as a reference electrode, and collecting and recording a photoelectric signal by an electrochemical workstation CHI 760E purchased from Chenghua instruments; in the test process, the electrochemical workstation applies a bias voltage of 0V, the electrolyte solution is 0.1M KCl, and the electron donor TEOA concentration is 0.1M; after the test, the result is shown in fig. 5(a), fig. 5(a) is a photocurrent broken line graph of the photoelectrochemical sensor electrodes obtained by the embodiment of the present invention and the comparative example under different Au loading amounts, and it can be known that when the doping amount of Au is 1%, the photoelectrochemical sensor electrodes have the best photocurrent response; referring to fig. 6, when the doping amount of Au is 5%, the introduction of Au may start to destroy the intrinsic structure of the ZnO material, thereby causing the decrease of the photoelectric properties.
And then the photoelectrochemical sensor electrode obtained in the embodiment 1 is independently used as a working electrode and placed in a photoelectrochemical system of a xenon lamp-electrochemical workstation for photoelectrochemical test, in the test process, the electrochemical workstation applies bias voltage of 0V, the electrolyte solution is 0.1M KCl, and the concentration range of electron donor TEOA is 0-0.2M; after the test, the results are shown in fig. 5(b), and fig. 5(b) is a graph showing the photocurrent curves of the photoelectrochemical sensor electrode obtained in example 1at different electron donor TEOA concentrations, and it can be seen that the photoelectrochemical sensor electrode obtained in example 1 has the best photocurrent response at the TEOA concentration of 0.1M.
Referring to the preparation method of the photoelectrochemical sensor electrode of example 1, the photoelectrochemical sensor electrodes under the calcination conditions of different temperatures were obtained at the calcination temperatures of 480 ℃, 520 ℃, 540 ℃, 560 ℃ and 560 ℃ respectively, with only the calcination temperature of the second step in the step (5) changed; placing the photoelectrochemical sensor electrode under different temperature calcination conditions as a working electrode in a photoelectrochemical system of a xenon lamp-electrochemical workstation for photoelectrochemical test, wherein in the test process, the electrochemical workstation applies a bias voltage of 0V, an electrolyte solution is 0.1M KCl, and the concentration of electron donor TEOA is 0.1M; after the test, the result is shown in fig. 5(c), fig. 5(c) is a light current line graph of the photoelectrochemical sensor electrode obtained in example 1at different calcination temperatures, and it can be seen that the photoelectrochemical sensor electrode has the best photoelectric response when the calcination temperature is 500 ℃.
Photoelectrochemical testing
Placing the photoelectrochemical sensor electrode obtained in example 1 as a working electrode in a photoelectrochemical system of a xenon lamp-electrochemical workstation for photoelectrochemical testing, taking a 7ILX500C xenon lamp purchased from Saifen photoelectricity as a light source, taking a platinum (Pt) wire as a counter electrode, taking a saturated Ag/AgCl electrode as a reference electrode, and collecting and recording a photoelectric signal by an electrochemical workstation CHI 760E purchased from Chenghua instruments; measuringIn the test process, the electrochemical workstation applies a bias voltage of 0V, the electrolyte solution is 0.1M KCl, the electron donor TEOA concentration is 0.1M, 4-nitrophenol (0.2-67.6 μ M) with different concentrations is added, and the relationship between the 4-nitrophenol concentration and the photocurrent can be obtained by outputting a current signal through the electrochemical workstation, and the result is shown in FIG. 7: FIG. 7(a) is an i-t graph showing the change of photocurrent with time of the electrode obtained in example 1 when used in a photoelectrochemical sensor, and it can be seen from FIG. 7(a) that the photocurrent was instantaneously decreased when 4-nitrophenol was added, and the linear range was 0.2-67.6. mu.M; FIG. 7(b) is a graph showing the linear relationship between the photocurrent and the concentration of 4-nitrophenol at different concentrations when the electrode obtained in example 1 is used in a photoelectrochemical sensor, and it can be seen from FIG. 7(b) that the logarithmic value of the concentration of 4-nitrophenol (logcPNP) is linearly related to the decrease rate of the photocurrent, and the linear equation is that Δ I is 0.36log c +0.27, and R is20.987; FIG. 7(c) is a graph showing the anti-interference test of the electrode obtained in example 1 when it is used in a photoelectrochemical sensor, and it can be seen from FIG. 7(c) that other interfering ions (Na)+、Cl-、Cd2+Etc.) without any interference with the response of 4-nitrophenol; fig. 7(d) is a graph illustrating stability of the electrode obtained in example 1 when the electrode is used in a photoelectrochemical sensor, and it can be seen from fig. 7(d) that the photocurrent does not significantly decrease after fifteen times of repeated scans of the electrode obtained in example 1, and the surface electrode has higher stability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The application of the Au/ZnO composite material in the photoelectrochemical sensor electrode is characterized in that the Au/ZnO composite material comprises Au nano-particles and porous ZnO nano-belts, and the Au nano-particles are uniformly loaded on the surfaces of the porous ZnO nano-belts.
2. The use of the Au/ZnO composite material in the photoelectrochemical sensor electrode according to claim 1, wherein the Au nanoparticles have a particle size of 2-10 nm.
3. The photoelectrochemical sensor electrode is characterized by comprising an Au/ZnO composite material and an ITO substrate, wherein the Au/ZnO composite material is uniformly loaded on the surface of the ITO substrate.
4. The photoelectrochemical sensor electrode according to claim 2 or 4, characterized in that said electrode is prepared by a method comprising the steps of:
s1, mixing Au source with ZnSe.0.5N2H4Nano-belt mixing reaction to obtain Au/ZnSe.0.5N2H4A composite material;
s2, mixing Au/ZnSe.0.5N2H4The composite material is assembled on the ITO surface to obtain Au/ZnSe.0.5N2H4And calcining the/ITO composite material to obtain the photoelectrochemical sensor electrode.
5. The photoelectrochemical sensor electrode according to claim 4, wherein step S1 specifically comprises: adding HAuCl4To ZnSe.0.5N2H4Mixing the nanometer belt with ethanol solution, stirring at 10-50 deg.C, and reacting for 30-60min to obtain Au/ZnSe.0.5N2H4A composite material;
preferably, HAuCl4And ZnSe.0.5N2H4The molar ratio of the nanoribbons is not more than 0.03:1, preferably 0.01: 1.
6. The photoelectrochemical sensor electrode according to claim 4 or 5, wherein step S2 specifically comprises: mixing Au/ZnSe.0.5N2H4Dispersing the composite material in a mixed solution of N, N-dimethylformamide and chloroform, assembling the composite material on the ITO surface by adopting a Langmuir-Blodgett self-assembly method, and drying the ITO surface for 10min at the temperature of between 40 and 60 ℃ to obtain Au/ZnSe.0.5N2H4Calcining the ITO composite material at the temperature of 350-580 ℃ for 30-60min to obtain the ITO composite materialAnd obtaining the Au/ZnO/ITO composite material as the photoelectrochemistry sensor electrode.
7. The photoelectrochemical sensor electrode according to any one of claims 4 to 6, characterized in that said calcination comprises in particular: heating to 400 ℃ at a heating rate of 1-3 ℃/min, preserving heat for 20-40min, heating to 580 ℃ at a heating rate of 1-3 ℃/min, and preserving heat for 10-20 min.
8. A photoelectrochemical sensor, characterized in that it comprises a photoelectrochemical sensor electrode according to any one of claims 3 to 7.
9. The photoelectrochemical sensor of claim 8, wherein the sensor consists of three electrodes, the working electrode is the photoelectrochemical sensor electrode, the counter electrode is a Pt wire electrode, and the reference electrode is a saturated Ag/AgCl electrode.
10. The photoelectrochemical sensor of claim 8 or 9, wherein the sensor is for the detection of 4-nitrophenol.
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