CN116124850B - Preparation method and application of electrode composite material - Google Patents
Preparation method and application of electrode composite material Download PDFInfo
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Abstract
The invention provides aThe preparation method and application of the electrode composite material comprise the following steps: s1, preparing SnO by adopting a sol-gel method 2 Nano particles, adding rGO into the nano particles, and calcining to obtain rGO/SnO 2 A composite material; s2, synthesizing MoS by adopting a hydrothermal method 2 The method comprises the steps of carrying out a first treatment on the surface of the S3, rGO/SnO 2 And MoS 2 Dispersing in ethanol-water mixture, annealing to obtain SnO 2 /rGO/MoS 2 A composite material; s4, adding SnO into the Au nano-particles 2 /rGO/MoS 2 In the sample, the sample is irradiated by a xenon lamp and stirred to obtain Au modified SnO 2 /rGO/MoS 2 A composite material; compared with the existing electrode composite material, the invention adopts the xenon lamp to improve the adhesion deposition effect and the photocatalysis efficiency of Au, and the composite material is used for H 2 The S electrochemical sensor has high sensitivity at low temperature, and has quicker and more obvious response.
Description
Technical Field
The invention relates to the technical field of electrochemical sensors, in particular to a preparation method and application of an electrode composite material.
Background
Sulfur hexafluoride is widely used for gas-insulated switchgear due to its excellent insulation and arc extinguishing properties. However, when the gas insulated switchgear is partially discharged due to a defect in insulation of equipment, sulfur hexafluoride gas is decomposed and reacts with trace oxygen and water existing in the gas insulated switchgear to generate H 2 S gas and several other deleterious compounds. H is well known 2 The S gas has extremely toxic and can cause harm to human health even at low concentration. H 2 S has a wide combination effect with physiological functions and is related to a plurality of pathologies such as neurodegenerative diseases, hypertension, diabetes mellitus and the like. Thus, H is detected 2 The S gas, especially the ppb level gas, is of great significance. Conventional analytical techniques such as chromatography, mass spectrometry, chemiluminescence and spectrophotometry have heretofore failed to meet the requirements of high efficiency H 2 S gas sensing requirements. Therefore, in recent years, electrochemical sensing technology has proven to be a highly efficient sensing technology for detecting harmful substances. The electrochemical technology is used as a substitute of the traditional analysis technology, has the advantages of low price, reliable analysis, high sensitivity, quick response, simple operation condition and the like, and can be used as a selective hydrogen sulfide physical examinationAnd (5) measuring technology.
The patent with publication number CN 107941867A discloses a four-electrode electrochemical gas sensor capable of simultaneously measuring nitric oxide and hydrogen sulfide in expired air, which comprises two working electrodes, an auxiliary electrode, a reference electrode, a hydrogen sulfide filter and electrolyte, and is characterized in that: the two working electrodes are positioned on the same horizontal plane and are independent in space, the two working electrodes are made of the same electrode material, and the hydrogen sulfide filter is positioned above one of the working electrodes. The working electrode is semicircular in shape, and the electrode material is gold-doped carbon nano tube, graphite or graphene. The gold-doped working electrode is sensitive to hydrogen sulfide, a mixed response signal of nitric oxide and hydrogen sulfide can be obtained, and only the response signal of nitric oxide can be obtained on the working electrode provided with the hydrogen sulfide filter, so that the response signals of nitric oxide and hydrogen sulfide can be obtained on the sensor simultaneously through difference value calculation. The sensor can realize the simultaneous detection of expired nitric oxide and expired hydrogen sulfide.
Patent publication No. CN113933359A discloses a preparation of a nanocomposite photosensitive electrode, which is used for rapidly detecting the glucose content in black rice by modifying the electrode with a nanocomposite of gold and tin dioxide.
However, most of the current patents focus on the study of a complete set of detection equipment, but the defects of the electrode materials are not fully solved. Research shows that electrochemical sensors are affected by various factors such as humidity and temperature under severe conditions, and the performance of electrochemical devices is directly affected. Therefore, it is a great challenge to safely and effectively operate and design highly stable and efficient electrochemical devices under these conditions.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of an electrode composite material, which solve the technical problem of sensitivity reduction of the existing electrochemical sensing material caused by low temperature.
To overcome the problems described above, include MoS 2 The layered material is due to its unique physical and chemical propertiesAnd is widely used in electrochemical sensing. MoS (MoS) 2 Has a graphite-like structure with three atomic layers, one Mo layer sandwiched between two S layers, the layers being interconnected by weak van der waals forces. Graphene has unique physical and chemical properties such as high specific surface area, excellent conductivity, high chemical stability, excellent mechanical strength and the like. The graphene in the composite material provides an effective way for modifying various nano particles and a new strategy for designing an electrochemical sensing material.
The technical scheme of the invention is realized as follows:
in one aspect, the invention provides a method for preparing an electrode composite material, comprising the following steps:
s1, firstly, preparing SnO by adopting a sol-gel method 2 A nanoparticle; adding rGO into the mixture, and calcining the mixture in a nitrogen atmosphere to obtain rGO/SnO 2 A composite material;
s2, synthesizing MoS by adopting a hydrothermal method 2 ；
S3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 Dispersing in ethanol-water mixture in proportion, annealing to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in an organic solvent, adding Au nano particles into the organic solvent according to a proportion, and irradiating and stirring the sample by using a xenon lamp under an inert atmosphere to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
SnO 2 As an n-type semiconductor having a wide forbidden bandwidth (3.6 eV), which has high thermal stability and chemical stability, it is considered to be an excellent sensor material, and SnO is selected 2 As a substrate; moS (MoS) 2 Is an n-type semiconductor with a direct band gap of 1.9eV and is widely used for detecting NH 3 Triethylamine, NO vapor and H 2 S gas. In addition, reduced graphene oxide (rGO) is commonly used as an electron transport channel material due to its superior electrical conductivity, and is widely used as a material for various sensing devicesA support material.
Further preferably, the specific process of step S1 includes the following steps:
s1, snCl 2 ·2H 2 Dissolving O in absolute ethanol, stirring for 0.5-1h, dripping acetylacetone, stirring for 0.5-1h, refluxing at 80-90deg.C for 4-5h to obtain SnO 2 Adding polyethylene glycol into the sol solution, aging at 20-25deg.C for 2-3d, drying at 100-110deg.C, annealing at 600-700deg.C for 2-4h to obtain SnO 2 A nanoparticle;
further preferably, in step S1 SnCl 2 ·2H 2 The mass ratio of O to acetylacetone to polyethylene glycol is 1: (0.5-0.61): (0.15-0.18).
Further preferably, the molecular weight of the polyethylene glycol comprises 300 or 4000.
Further preferably, the specific process of step S2 includes the following steps:
s2, CH at 20-25 DEG C 4 N 2 S and Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 200-220deg.C for 18-24 hr, heat treating, washing the obtained black product with absolute ethanol, vacuum drying in oven at 60-65deg.C for 6-8 hr, and calcining at 700-750deg.C under nitrogen atmosphere for 3-4 hr to obtain MoS 2 ；
Further preferably, CH is removed in step S2 4 N 2 S and Na 2 MoO 4 .2H 2 The mass ratio of O is (1.31-1.4): 1.
SnO 2 /rGO/MoS 2 the composite material will be prepared by simple wet chemistry, further preferably, the specific process of step S3 further comprises the steps of:
s3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in the step S2 2 Dispersing in ethanol-water mixture at a certain proportion, stirring at 20-25deg.C for 3-4 hr, vacuum drying at 60-70deg.C for 12-18 hr, and annealing at 350-400deg.C in muffle furnace for 1-2 hr to obtain SnO 2 /rGO/MoS 2 A composite material.
Further preferred, the rGO/SnO 2 And MoS 2 The mass ratio of (2) is 1: (0.05-0.2).
Further preferably, the ethanol-water mixture has a volume ratio of ethanol to water of 1 (1-1.5).
Finally, modifying the SnO with Au nano particles by a photo-deposition method 2 /rGO/MoS 2 For this purpose, it is further preferred that the specific process of step S4 further comprises the following steps:
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and adding HAuCl 4 ·4H 2 O is added in proportion to eliminate dissolved O 2 Bubbling inert gas for 20-30min, irradiating sample with xenon lamp, stirring for 2-3 hr, centrifuging, washing, and drying at 60-70deg.C to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
Further preferably, the SnO 2 /rGO/MoS 2 The mass ratio of the sample to the methanol is 1: (100-126.5).
Further preferably, the SnO 2 /rGO/MoS 2 Sample and HAuCl 4 ·4H 2 The mass ratio of O is 1: (0.01-0.4).
Further preferably, the xenon lamp has a power of 300-400W and a wavelength of 200-400nm.
On the other hand, the invention also provides an application of the electrode composite material, and the composite material obtained by the preparation method of the electrode composite material in the first aspect is used for H 2 S electrochemical sensor.
H 2 S molecule and Au modified SnO 2 /rGO/MoS 2 Between chemisorbed oxygen on the electrode surface the following reactions will occur:
2H 2 S + 3O − 2(ads) → 2H 2 O + 2SO 2 + 3e −
the reaction mechanism is shown in the figure, and gold nanoparticles generally show excellent electrical and catalytic properties due to the local surface plasmon resonance effect. Inspired by the specific characteristics of each material, the group of materials in a single flexible nano-assembly systemThe combination will enhance the electrochemical H 2 S gas sensitive properties.
Compared with the prior art, the preparation method and application of the electrode composite material have the following beneficial effects:
the preparation method of the electrode composite material prepares the composite material SnO by a sol-gel method, a hydrothermal method and a wet method successively 2 /rGO/MoS 2 And is mainly prepared by adopting a photo-deposition method irradiated by a xenon lamp to prepare the composite material Au nano particle modified SnO 2 /rGO/MoS 2 Has high sensitivity to nitrite ions even at low temperature, can effectively promote the deposition and adhesion effects of Au, and the Au nano-particles formed by deposition are helpful for improving SnO 2 /rGO/MoS 2 The charge transfer on the interface of the composite material promotes the improvement of the photocatalysis efficiency; meanwhile, the method is simple, the preparation cost is low, and the method has good application prospect;
compared with the existing electrochemical sensor material, the reaction speed is reduced under the low-temperature condition, the electrode composite material is not affected by low temperature, and the electrode composite material can play a better role in severe cold weather; meanwhile, the sensitivity of the device is not affected by alkali metal or even organic silicon vapor, and the sensitivity is not irreversibly inhibited;
the composite material prepared by the invention is used for H 2 S electrochemical sensor, electrode material with fast heterogeneous electron transfer rate will lead to electrochemical H 2 The overpotential of S sensing is obviously reduced, and the local surface plasma resonance effect caused by noble metal components can generate strong current, which can obviously promote H 2 The catalytic oxidation of S, the sensor response is faster and more pronounced.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the reaction mechanism of the electrode composite material of the invention when the electrode composite material is used in a sensor.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Examples
The preparation method of the electrode composite material comprises the following steps:
s1, 8g of SnCl 2 ·2H 2 Dissolving O in 70ml absolute ethanol, stirring for 0.5h, dripping 4g acetylacetone, stirring for 0.5h, refluxing at 80deg.C for 4h to obtain SnO 2 Adding 1.2g of polyethylene glycol 300 into the sol solution, aging for 2 days at 20 ℃, drying at 100 ℃, and annealing at 600 ℃ for 2 hours to obtain SnO 2 A nanoparticle;
s2, at 20℃1.9. 1.9gCH 4 N 2 S and 1.45g Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 200deg.C for 18 hr, heat treating, washing the obtained black product with absolute ethanol, vacuum drying in oven at 60deg.C for 6 hr, and calcining at 700deg.C under nitrogen atmosphere for 3 hr to obtain MoS 2 ；
S3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 According to the following steps of 1:0.05 in a mixture of ethanol and water, ethanol and water in a volume ratio of 1:1, stirring for 3h at 20 ℃, vacuum drying for 12h at 60 ℃, and annealing for 1h in a muffle furnace at 350 ℃ to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and then using SnO 2 /rGO/MoS 2 Sample: HAuCl 4 ·4H 2 O=1: 0.01 mass ratio of HAuCl 4 ·4H 2 O, in order to eliminate dissolved O 2 Bubbling inert gas for 20min, irradiating the sample with 300W xenon lamp with wavelength of 200nm, stirring for 2 hr, centrifuging, washing, and drying at 60deg.C to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
Examples
The preparation method of the electrode composite material comprises the following steps:
s1, 8g of SnCl 2 ·2H 2 Dissolving O in absolute ethanol, stirring for 1h, dripping 4.88g of acetylacetone, stirring for 1h, refluxing at 90 ℃ for 5h to generate SnO 2 Adding 1.44g polyethylene glycol 4000 into the sol solution, aging at 25deg.C for 3d, drying at 110deg.C, annealing at 700deg.C for 4h to obtain SnO 2 A nanoparticle;
s2, 1.9g of CH at 25 ℃ 4 N 2 S and 1.35g Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 220deg.C for 24 hr, heat treating, washing the obtained black product with absolute ethanol, vacuum drying in 65 deg.C oven for 8 hr, and calcining at 750deg.C under nitrogen atmosphere for 4 hr to obtain MoS 2 ；
S3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 According to the following steps of 1:0.2 in a mixture of ethanol and water, ethanol and water in a volume ratio of 1:1.5 stirring at 25 ℃ for 4 hours, vacuum drying at 70 ℃ for 18 hours, and annealing at 400 ℃ in a muffle furnace for 2 hours to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and then using SnO 2 /rGO/MoS 2 Sample: HAuCl 4 ·4H 2 O=1: 0.4 mass ratio of HAuCl 4 ·4H 2 O, in order to eliminate dissolved O 2 Bubbling inert gas for 30min, irradiating the sample with 400W xenon lamp with wavelength of 400nm, stirring for 3 hr, centrifuging, washing, and drying at 70deg.C to obtain Au-modified SnO 2 /rGO/MoS 2 A composite material.
Examples
The preparation method of the electrode composite material comprises the following steps:
s1, 8g of SnCl 2 ·2H 2 Dissolving O in absolute ethanol, stirring for 0.8h, dripping 4.5g of acetylacetone, stirring for 0.8h, refluxing at 80 ℃ for 3h to generate SnO 2 Adding 1.28g of polyethylene glycol 300 into the sol solution, aging for 2 days at 22 ℃, drying at 105 ℃, and annealing for 2 hours at 650 ℃ to obtain SnO 2 A nanoparticle;
s2, 1.9g of CH at 22 DEG C 4 N 2 S and 1.4g Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 210 ℃ for 18h, washing the obtained black product with absolute ethyl alcohol after heat treatment, finally drying the product in a 63 ℃ oven in vacuum for 7h, and calcining at 720 ℃ under nitrogen atmosphere for 3.5h to obtain MoS 2 ；
S3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 According to the following steps of 1:0.1 in a mixture of ethanol and water, ethanol and water in a volume ratio of 1:1.2 stirring at 22 ℃ for 3.5h, vacuum drying at 65 ℃ for 16h, and annealing in a muffle furnace at 360 ℃ for 1.5h to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and then using SnO 2 /rGO/MoS 2 Sample: HAuCl 4 ·4H 2 O=1: 0.2 mass ratio of HAuCl 4 ·4H 2 O, in order to eliminate dissolved O 2 Bubbling inert gas for 25min, irradiating the sample with 300W xenon lamp with wavelength of 200nm, stirring for 2.5 hr, centrifuging, washing, and drying at 65deg.C to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
Examples
The preparation method of the electrode composite material comprises the following steps:
s1, 8g of SnCl 2 ·2H 2 Dissolving O in absolute ethanol, stirring for 0.5h, dripping 4.88g of acetylacetone, stirring for 1h, refluxing at 90 ℃ for 5h to generate SnO 2 Adding 1.44g polyethylene glycol 4000, aging at 25deg.C for 3d, drying at 110deg.C, and annealing at 700deg.C for 4h to obtain the final productSnO 2 A nanoparticle;
s2, 1.9g of CH at 25 ℃ 4 N 2 S and 1.35g Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 220deg.C for 24 hr, heat treating, washing the obtained black product with absolute ethanol, vacuum drying in 65 deg.C oven for 8 hr, and calcining at 750deg.C under nitrogen atmosphere for 4 hr to obtain MoS 2 ；
S3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 According to the following steps of 1: dispersing in ethanol-water mixture at a mass ratio of 0.05, stirring at 25deg.C for 4 hr, vacuum drying at 70deg.C for 18 hr, and annealing at 400deg.C in muffle furnace for 2 hr to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and then using SnO 2 /rGO/MoS 2 Sample: HAuCl 4 ·4H 2 O=1: 0.01 mass ratio of HAuCl 4 ·4H 2 O, in order to eliminate dissolved O 2 Bubbling inert gas for 30min, irradiating the sample with xenon lamp, stirring for 3 hr, centrifuging, washing, and drying at 70deg.C to obtain Au-modified SnO 2 /rGO/MoS 2 A composite material.
Comparative example 1
The preparation method of the electrode composite material is different from example 1 in that the composite material is not subjected to Au modification by a xenon lamp.
Comparative example 2
The preparation method of the electrode composite material is different from example 1 in that a xenon lamp is used for irradiating the platinum modified composite electrode material.
Comparative example 3
A preparation method of an electrode composite material, and the preparation method refers to a method with a publication number of CN113933359A for preparing an electrode material of nano-gold modified tin dioxide.
Comparative example 4
A method for preparing an electrode composite material, which is different from example 1 in that the power of a xenon lamp is 500W.
Comparative example 5
A method for preparing an electrode composite material, which is different from example 1 in that the wavelength of a xenon lamp is 467nm.
The composite material prepared in each example was used for H 2 S sensor for detecting use performance thereof
Table 1 composite materials of the examples are used for H 2 S-type sensor
Table 2 composite materials of various embodiments are used in sensors to detect different target gases
As can be seen from Table 1, in comparison between example 1 and comparative example 1, the composite material prepared by the photo-deposition method using xenon lamp irradiation can effectively improve the Au deposition adhesion effect, and the charge transfer at the interface of the composite material, because the design principle of the composite electrode is based on H 2 Oxidation of S gas, H 2 S and O 2 Surplus electrons remain after the reaction, wherein the surplus electrons are generated by lattice oxygen and oxygen vacancies, and the transport efficiency of the composite electrode to the electrode can influence the sensitivity of the sensor, so that the improvement of the photocatalysis efficiency is promoted; example 1 and comparative example 2 compare, platinum modified SnO 2 /rGO/MoS 2 The performance of the composite electrode material is relatively similar to that of the composite material, but the former has scarce sources and high preparation cost; example 1 and comparative example 3 comparison of Au modified SnO of the present invention 2 /rGO/MoS 2 Composite electrode material, compared with the existing nano gold and SnO 2 The compound modified electrode material has high sensitivity at low temperature and good detection limit accuracy; compared with comparative examples 4 and 5, the embodiment 1 has obvious influence on the deposition effect and response time of Au due to the irradiation power and wavelength of the xenon lamp, and the in-situ deposition method by the irradiation of the xenon lamp has the advantages that: the generation of surfactant or additional linker molecules can be avoided, which not only means that the tedious growth process is simplified, but also the performance of the sensing response is improved at the same time; the method has more powerful intermolecular force and more sufficient reaction sites, and can fully utilize the surface plasma effect of the Au nano-particles; as can be seen from Table 2, the composite material of the present invention was used for a sensor except for H 2 In addition to S gas, for detecting NH 3 The triethylamine and NO vapor also have better detection limits.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
1. The preparation method of the electrochemical sensor electrode composite material is characterized by comprising the following steps of:
s1, firstly, preparing SnO by adopting a sol-gel method 2 A nanoparticle; adding rGO into the mixture, and calcining the mixture in a nitrogen atmosphere to obtain rGO/SnO 2 A composite material;
s2, synthesizing the layered MoS by adopting a hydrothermal method 2 The method comprises the steps of carrying out a first treatment on the surface of the The specific process of step S2 includes the following steps:
s2, CH at 20-25 DEG C 4 N 2 S and Na 2 MoO 4 .2H 2 Mixing and stirring O precursor, dissolving in deionized water, heating at 200-220deg.C for 18-24 hr, heat treating, washing the obtained black product with absolute ethanol, vacuum drying in oven at 60-65deg.C for 6-8 hr, and calcining at 700-750deg.C under nitrogen atmosphere for 3-4 hr to obtain MoS 2 ；
In step S2, CH 4 N 2 S and Na 2 MoO 4 .2H 2 The mass ratio of O is (1.31-1.4): 1, a step of;
s3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 Dispersing in ethanol-water mixture in proportion, annealing to obtain SnO 2 /rGO/MoS 2 A composite material;
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in an organic solvent, adding Au nano particles in proportion, and irradiating and stirring the sample by using a xenon lamp under an inert atmosphere to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
2. The method for preparing an electrode composite material for an electrochemical sensor according to claim 1, wherein the specific process of step S3 specifically comprises the following steps:
s3, rGO/SnO prepared in the step S1 is prepared 2 And MoS prepared in step S2 2 Dispersing in ethanol-water mixture at a certain proportion, stirring at 20-25deg.C for 3-4 hr, vacuum drying at 60-70deg.C for 12-18 hr, and annealing at 350-400deg.C in muffle furnace for 1-2 hr to obtain SnO 2 /rGO/MoS 2 A composite material.
3. The method for preparing an electrochemical sensor electrode composite material according to claim 2, wherein the rGO/SnO is prepared by the following steps 2 And MoS 2 The mass ratio of (2) is 1: (0.05-0.2).
4. The method for preparing an electrochemical sensor electrode composite material according to claim 2, wherein the volume ratio of ethanol to water in the ethanol-water mixture is 1 (1-1.5).
5. The method for preparing an electrode composite material for an electrochemical sensor according to claim 1, wherein the specific process of step S4 specifically comprises the following steps:
s4, snO prepared in the step S3 2 /rGO/MoS 2 Dispersing the sample in methanol, and adding HAuCl 4 ·4H 2 Adding O into the mixture in proportion, bubbling inert gas for 20-30min, irradiating the sample with xenon lamp, stirring for 2-3h, centrifuging, washing, and drying at 60-70deg.C to obtain Au modified SnO 2 /rGO/MoS 2 A composite material.
6. The method for preparing an electrochemical sensor electrode composite material according to claim 5, wherein the SnO 2 /rGO/MoS 2 The mass ratio of the sample to the methanol is 1: (100-126.5).
7. The method for preparing an electrochemical sensor electrode composite material according to claim 5, wherein the SnO 2 /rGO/MoS 2 Sample and HAuCl 4 ·4H 2 The mass ratio of O is 1: (0.01-0.4).
8. The method for preparing an electrode composite material for an electrochemical sensor according to claim 5, wherein the xenon lamp has a power of 300-400W and a wavelength of 200-400nm.
9. The composite material in H obtained by the preparation method of the electrochemical sensor electrode composite material according to any one of claims 1 to 8 2 S application in electrochemical sensors.
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| GB201706805D0 (en) * | 2017-04-28 | 2017-06-14 | Cambridge Entpr Ltd | Composite metal organic framework materials, processes for their manufacture and uses thereof |
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| CN112871185B (en) * | 2021-01-18 | 2023-04-14 | 武汉梓强生态科技有限公司 | SnO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel and preparation method thereof |
| CN115753905A (en) * | 2022-10-11 | 2023-03-07 | 伊犁师范大学 | For detecting H 2 Gas sensor for S gas |
| CN115753894A (en) * | 2022-12-01 | 2023-03-07 | 上海理工大学 | SnO (stannic oxide) -based composite material 2 @MoS 2 Gas sensor of nano composite material and preparation method |
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