CN110967384A - Simple preparation method of transparent electrode of ultralow-concentration hydrogen peroxide sensor - Google Patents
Simple preparation method of transparent electrode of ultralow-concentration hydrogen peroxide sensor Download PDFInfo
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Abstract
The invention provides a simple and convenient preparation method of a transparent electrode of an ultralow-concentration hydrogen peroxide sensor, which comprises the following steps: depositing graphene on the surface of quartz glass by using methane as a carbon source gas by using a normal-pressure chemical vapor deposition method to prepare quartz glass graphene; and then sputtering platinum nano particles on the surface of the quartz glass graphene by using a vacuum magnetron sputtering process by using a platinum sheet as a sputtering target to prepare the graphene glass composite platinum nano particle transparent electrode. The preparation method is simple, the obtained electrode can be used as an independent transparent electrode to be applied to a sensor, the ultralow-concentration hydrogen peroxide can be detected, the lower detection limit is 3.3nmol/L, the detection linear range is 10nmol/L-80 mu mol/L, and H is fully expanded2O2The application interval of the sensor; meanwhile, the kit has stronger anti-interference performance on dopamine, ascorbic acid and uric acid, and can be applied to the detection of actual biological samples.
Description
Technical Field
The invention relates to a simple preparation method of a transparent electrode of an ultralow-concentration hydrogen peroxide sensor, belonging to the technical field of chemical sensors.
Background
Hydrogen peroxide (H)2O2) Is an important intermediate in biomedicine and chemical industry, and has important application value in the fields of clinical medicine, environment, food detection and the like; biologically, hydrogen peroxide is also an important index for serious diseases such as cancer, alzheimer disease, and parkinson disease. Therefore, the low concentration H is accurately measured2O2Has important practical significance. In recent years, chemiluminescence, spectroscopy, chromatography, enzymatic chemistry, and the like have been widely used for effective detection of hydrogen peroxide;however, the detection methods involve complicated equipment and complicated detection process, and the limitations of detection limit and detection linearity limit H2O2And (5) expanding the application scene of the sensor.
The non-enzymatic electrochemical hydrogen peroxide sensor overcomes the defects of the method, and is widely applied to the detection of hydrogen peroxide due to the advantages of simple equipment, easiness in miniaturization, high sensitivity, good selectivity, quick response and the like. The electrochemical hydrogen peroxide sensor method for detecting the sample to be detected is an analysis method for determining the concentration of the substance to be detected in a certain range and the linear relation between the concentration and the electric parameter. However, the existing electrochemical hydrogen peroxide sensor has the defects of high detection limit on hydrogen peroxide and incapability of effectively detecting low-concentration hydrogen peroxide. For example, chinese patent document CN103792271A discloses a hydrogen peroxide non-enzymatic electrochemical sensor and a preparation method thereof, which comprises pretreating and activating a glassy carbon electrode, and then depositing an Ag nanoparticle beam on the glassy carbon electrode by magnetron sputtering to obtain an electrode material. The electrode constructed by the method can enable the catalyst to have good dispersibility, crystallinity and a clean surface on the surface of the electrode, but the lower limit of detection on hydrogen peroxide is 1mol/L, the lower limit of detection is higher, low-concentration hydrogen peroxide cannot be detected, and the anti-interference performance is not involved. For another example, chinese patent document CN109298050A discloses a method for preparing a hydrogen peroxide enzyme-free sensor based on a laser-induced graphene-precious metal nanocomposite; firstly, carving or burning the surface of a polyimide film by adopting a high-intensity laser beam, and removing the residual materials of the polyimide film to obtain patterned laser-induced graphene; secondly, transferring the laser-induced graphene into a vacuum magnetron sputtering device for sputtering of noble metal to obtain a laser-induced graphene-noble metal nano composite; and finally, taking the laser-induced graphene-noble metal nano composite as a working electrode, and jointly constructing the hydrogen peroxide electrochemical sensor with an auxiliary electrode and a reference electrode. The sensor can realize rapid and sensitive detection of hydrogen peroxide on an aqueous solution containing trace hydrogen peroxide, but the lower detection limit is 0.1 mu mol/L, and the sensor is still higher and cannot detect hydrogen peroxide with lower concentration.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a simple and convenient preparation method of a transparent electrode of an ultralow-concentration hydrogen peroxide sensor. The preparation method is simple, the quartz glass graphene is prepared by utilizing direct chemical vapor deposition, then the graphene glass composite platinum nanoparticles are obtained by combining the vacuum magnetron sputtering process, the graphene glass composite platinum nanoparticles can be used as independent transparent electrodes to be applied to sensors, the ultralow-concentration hydrogen peroxide can be detected, the lower detection limit is 3.3nmol/L, the detection linear range is 10nmol/L-80 mu mol/L, and H is fully expanded2O2The application interval of the sensor; meanwhile, the kit has stronger anti-interference performance on dopamine, ascorbic acid and uric acid, and can be applied to the detection of actual biological samples.
Description of terms:
room temperature: having the meaning known in the art, in particular 25 ℃. + -. 5 ℃.
The technical scheme of the invention is as follows:
a simple preparation method of a transparent electrode of an ultra-low concentration hydrogen peroxide sensor comprises the following steps:
(1) using methane as a carbon source gas, and depositing and growing graphene on the surface of quartz glass by adopting a normal-pressure chemical vapor deposition method at the temperature of 800-;
(2) and sputtering platinum nano particles on the surface of the quartz glass graphene by using a vacuum magnetron sputtering process by taking a platinum sheet as a sputtering target to prepare the graphene glass composite platinum nano particle transparent electrode.
Preferably, in step (1), the carrier gas used in the atmospheric pressure chemical vapor deposition method is argon gas, and the reducing gas used in the atmospheric pressure chemical vapor deposition method is hydrogen gas; the volume ratio of the argon gas to the hydrogen gas to the carbon source gas is 28-32:3-8: 1; argon gas, hydrogen gas and carbon source gas are mixed and introduced into the system in the form of mixed gas, wherein the flow rate of the mixed gas is 100-500 sccm.
Preferably, the volume ratio of the argon gas, the hydrogen gas and the carbon source gas is 30:5: 1; the flow rate of the mixed gas is 200sccm and 400 sccm.
According to the invention, in step (1), the atmospheric pressure chemical vapor deposition method is carried out according to the prior art.
According to the invention, in the step (1), before use, the quartz glass is subjected to ultrasonic cleaning by acetone, absolute ethyl alcohol and deionized water respectively. The quartz glass is SiO with the purity of 99.9wt percent2。
Preferably, in step (1), the deposition growth time is 2-4 h.
Preferably, the deposition temperature is 1000 ℃, and the deposition growth time is 3 h.
Preferably, in step (1), 2 to 3 layers of graphene are deposited and grown on the surface of the quartz glass.
According to the invention, the vacuum magnetron sputtering process in the step (2) is carried out according to the prior art.
Preferably, in the step (2), in the vacuum magnetron sputtering process, the sputtering pressure is 0.2-0.8Pa, the sputtering power is 100-300W, the sputtering time is 10s-2min, and the sputtering temperature is room temperature.
Preferably, the sputtering power is 200W, and the sputtering time is 1 min.
The graphene glass composite platinum nanoparticle transparent electrode prepared by the invention is used as H2O2Independent transparent electrode of sensor, applicable to H2O2The low concentration detection of (2).
The invention has the following technical characteristics and beneficial effects:
1. the method only relates to the direct chemical vapor deposition and vacuum magnetron sputtering process of the graphene, has simple preparation method, and can realize the industrial production and optimization; and other toxic and harmful reagents are not used, so that the preparation method is a green preparation process. The graphene glass composite platinum nanoparticle transparent electrode prepared by the method can be directly used as H2O2Independent transparent electrode of sensor, applied to H2O2The low concentration detection of (2).
2. According to the method, 2-3 layers of graphene prepared by combining a specific carbon source with specific conditions through direct chemical vapor deposition are coated on the surface of quartz glass, so that the complex transfer process of the traditional CVD graphene is avoided, and the excellent electrochemical performance of the CVD graphene is fully reserved; compared with the patent document CN109298050A, the prepared graphene has the advantages of thinner thickness, higher crystallinity, integrity and uniformity, and more excellent electrochemical performance. The prepared quartz glass graphene is sputtered with platinum nanoparticles by a vacuum magnetron sputtering process under specific conditions, and the platinum nanoparticles with the particle size of 3-5nm are uniformly dispersed on the surface of the quartz glass graphene, so that the catalytic performance of the quartz glass graphene can be better exerted. The graphene with the specific structure assists the platinum nanoparticles with specific forms, so that the prepared electrode has more excellent catalytic activity. The electrode prepared by the invention is a transparent electrode and has a good application prospect.
3. The transparent electrode of the hydrogen peroxide sensor prepared by the invention is used as an independent transparent electrode to be applied to the hydrogen peroxide sensor, can detect ultralow-concentration hydrogen peroxide, has the lower detection limit of 3.3nmol/L and the linear detection range of 10nmol/L-80 μmol/L, and is compared with commercial (100 μmol/L) and other developed H2O2The sensor has lower detection limit, and the H is fully expanded2O2The application interval of the sensor. Meanwhile, the sensor prepared by the invention has stronger anti-interference performance on dopamine, ascorbic acid and uric acid, has strong detection selectivity, and can be applied to the detection of actual biological samples.
Drawings
Fig. 1(a) is an SEM image of quartz glass graphene prepared in example 1; fig. 1(b) is a raman spectrum of the quartz glass graphene prepared in example 1; fig. 1(c) is a TEM image of the platinum nanoparticles prepared in example 1.
Fig. 2 is an XPS chart of the graphene glass composite platinum nanoparticle transparent electrode prepared in example 1.
Fig. 3(a) is a time-current curve diagram of the graphene glass composite platinum nanoparticle transparent electrode prepared in example 1 applied to a hydrogen peroxide sensor, wherein an inset is a partially enlarged view; fig. 3(b) and (c) are fitted graphs between current and hydrogen peroxide concentration.
Fig. 4 is an anti-interference test chart of the graphene glass composite platinum nanoparticle transparent electrode prepared in example 1 applied to a hydrogen peroxide sensor.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following specific examples.
The raw materials used in the examples are conventional and commercially available. Wherein the quartz glass used is SiO with a purity of 99.9 wt%2The size is 10 multiplied by 5 multiplied by 0.5 mm; the product is ultrasonically cleaned by acetone, absolute ethyl alcohol and deionized water in sequence before use.
Chemical vapor deposition equipment used in the examples was sold by Xiamene New Material science and technology Co., Ltd; vacuum magnetron sputtering equipment, available from danton vacuum equipment limited, model number: DESK V; other devices or methods used are known in the art unless otherwise specified.
Example 1
A simple preparation method of a transparent electrode of an ultra-low concentration hydrogen peroxide sensor comprises the following steps:
(1) forming mixed gas by taking methane as a carbon source gas, argon as a carrier gas and hydrogen as a reducing gas, introducing the mixed gas into chemical vapor deposition equipment, and depositing and growing graphene on the surface of quartz glass for 3 hours at the temperature of 1000 ℃ by adopting a normal-pressure (one atmospheric pressure) chemical vapor deposition method to prepare the quartz glass graphene; the volume ratio of the argon gas, the hydrogen gas and the carbon source gas is 30:5:1, and the flow rate of the mixed gas is 300 sccm.
(2) And (3) sputtering platinum nanoparticles on the surface of quartz glass graphene by using a platinum sheet (with the purity of 99.99 wt%) as a sputtering target and controlling the sputtering pressure of 0.3Pa, the sputtering power of 200W, the sputtering time of 1min and the sputtering temperature to be room temperature by using vacuum magnetron sputtering equipment to prepare the graphene glass composite platinum nanoparticle transparent electrode.
As shown in fig. 1(a), the SEM image of the quartz glass graphene prepared in this example shows that the graphene sheet layer is sufficiently uniformly coated on the surface of the quartz glass.
A raman spectrum of the quartz glass graphene prepared in this example is shown in fig. 1(b), and the raman spectrum has a sharp G peak, which is a characteristic peak of graphene; i is2D/IGApproximately equal to 1, indicating 2-3 layers of graphene.
The TEM image of the platinum nanoparticles prepared in this example is shown in FIG. 1(c), and the nano platinum particles with diameters of 3-5nm are uniformly dispersed.
An XPS chart of the graphene glass composite platinum nanoparticle transparent electrode prepared in this example is shown in fig. 2, which shows that the quartz glass graphene and the nano platinum are perfectly compounded.
The electrode prepared in this example was applied to H2O2A sensor: the prepared graphene glass composite platinum nano particle transparent electrode is used as a working electrode, a counter electrode (platinum electrode) and a reference electrode (saturated calomel electrode) form a three-electrode system, phosphate buffer solution (solute is sodium dihydrogen phosphate and disodium hydrogen phosphate) with the pH of 7.2 and the total salt concentration of 0.1mol/L is used as a reaction tank, and an electrochemical workstation is used for measuring different concentrations H of the working electrode pair2O2Responsiveness of the solution. When the time current curve is tested, the voltage is set to be 0.65V, and H is intermittently added into the reaction tank after the current value is stabilized2O2Solution of H in the system2O2The concentration of the solution is 10nmol/L, 20nmol/L, 50nmol/L, 100nmol/L, 200nmol/L, 500nmol/L, 1. mu. mol/L, 2. mu. mol/L, 5. mu. mol/L, 10. mu. mol/L, 20. mu. mol/L, and 50. mu. mol/L in this order.
The time current curve of the electrode prepared in this example applied to a hydrogen peroxide sensor is shown in fig. 3. As can be seen from FIG. 3(a), the application of the electrode in the present embodiment to the sensor has a response limit as low as 10nmol/L, and considering the influence of the signal-to-noise ratio on the experimental results, the detection limit of the sensor is as low as 3.3nmol/L when the signal-to-noise ratio is equal to 3. FIGS. 3(b) and (c) are graphs fitted between the current and the hydrogen peroxide concentration, and it can be seen that the electrode of the present embodiment has good linear detection ranges in the sensor ranges of 10nmol/L-2000nmol/L and 2 μmol/L-80 μmol/L.
The electrode prepared in this example was applied to H2O2The sensor carries out anti-interference performance test, and the test method comprises the following steps: the prepared graphene glass composite platinum nano particle transparent electrode is used as a working electrode, and a counter electrode (platinum electrode) and a reference electrode (saturated calomel electrode) set are utilizedIn a three-electrode system, phosphate buffer solution (solute is sodium dihydrogen phosphate and disodium hydrogen phosphate) with pH 7.2 and total salt concentration of 0.1mol/L is used as a reaction cell, and an electrochemical workstation is used for measuring the working electrode pair H2O2Dopamine, ascorbic acid and uric acid. When the time current curve is tested, the voltage is set to be 0.65V, after the current value is stabilized, 25 mu L of 50 mu mol/L H is intermittently and sequentially added into the reaction tank2O2500. mu. mol/L dopamine, 500. mu. mol/L ascorbic acid, 500. mu. mol/L uric acid, 50. mu. mol/L H2O2To detect the anti-interference performance of the sensor.
An anti-interference test chart of the graphene glass composite platinum nanoparticle transparent electrode applied to the hydrogen peroxide sensor is shown in fig. 4, and it can be seen from fig. 4 that the graphene glass composite platinum nanoparticle transparent electrode is compared with H2O2The current response caused by the electrode is negligible, and the current fluctuation caused by dopamine, ascorbic acid and uric acid is negligible, so that the electrode has better anti-interference performance when being applied to a hydrogen peroxide sensor.
Example 2
A simple preparation method of a transparent electrode of an ultra-low concentration hydrogen peroxide sensor comprises the following steps:
(1) forming mixed gas by taking methane as a carbon source gas, argon as a carrier gas and hydrogen as a reducing gas, introducing the mixed gas into chemical vapor deposition equipment, and depositing and growing graphene on the surface of quartz glass for 2 hours at 1050 ℃ by adopting a normal-pressure (one atmospheric pressure) chemical vapor deposition method to prepare the quartz glass graphene; the volume ratio of the argon gas, the hydrogen gas and the carbon source gas is 30:5:1, and the flow rate of the mixed gas is 400 sccm.
(2) And (3) sputtering platinum nanoparticles on the surface of quartz glass graphene by using a platinum sheet (with the purity of 99.99 wt%) as a sputtering target and controlling the sputtering pressure of 0.5Pa, the sputtering power of 300W, the sputtering time of 40s and the sputtering temperature at room temperature by using a vacuum magnetron sputtering device to prepare the graphene glass composite platinum nanoparticle transparent electrode.
Example 3
A simple preparation method of a transparent electrode of an ultra-low concentration hydrogen peroxide sensor comprises the following steps:
(1) forming mixed gas by taking methane as a carbon source gas, argon as a carrier gas and hydrogen as a reducing gas, introducing the mixed gas into chemical vapor deposition equipment, and depositing and growing graphene on the surface of quartz glass for 4 hours at the temperature of 950 ℃ by adopting a normal-pressure (one atmospheric pressure) chemical vapor deposition method to prepare the quartz glass graphene; the volume ratio of the argon gas, the hydrogen gas and the carbon source gas is 30:5:1, and the flow rate of the mixed gas is 200 sccm.
(2) And (3) sputtering platinum nanoparticles on the surface of quartz glass graphene by using a platinum sheet (with the purity of 99.99 wt%) as a sputtering target and controlling the sputtering pressure of 0.7Pa, the sputtering power of 100W, the sputtering time of 2min and the sputtering temperature at room temperature by using a vacuum magnetron sputtering device to prepare the graphene glass composite platinum nanoparticle transparent electrode.
Comparative example 1
A preparation method of an electrode comprises the following steps:
(1) forming mixed gas by taking methane as a carbon source gas, argon as a carrier gas and hydrogen as a reducing gas, introducing the mixed gas into chemical vapor deposition equipment, and depositing and growing graphene on the surface of quartz glass for 1h at the temperature of 1000 ℃ by adopting a normal-pressure (one atmospheric pressure) chemical vapor deposition method to prepare the quartz glass graphene; the volume ratio of the argon gas, the hydrogen gas and the carbon source gas is 30:5:1, and the flow rate of the mixed gas is 300 sccm.
(2) And (3) sputtering platinum nanoparticles on the surface of quartz glass graphene by using a platinum sheet (with the purity of 99.99 wt%) as a sputtering target and controlling the sputtering pressure of 0.3Pa, the sputtering power of 200W, the sputtering time of 1min and the sputtering temperature to be room temperature by using vacuum magnetron sputtering equipment to prepare the graphene glass composite platinum nanoparticle transparent electrode.
The electrode prepared in this comparative example was applied to H2O2Sensor, which does not exhibit a contrast to H2O2The electrochemical response of (a); the growth time of graphene deposition is a key factor for preparing the electrode, and the reduction of the growth time causes the poor physicochemical morphology of quartz glass graphene and directly causes H pair2O2The electrochemical response decreases very rapidly.
Claims (9)
1. A simple preparation method of a transparent electrode of an ultra-low concentration hydrogen peroxide sensor comprises the following steps:
(1) using methane as a carbon source gas, and depositing and growing graphene on the surface of quartz glass by adopting a normal-pressure chemical vapor deposition method at the temperature of 800-;
(2) and sputtering platinum nano particles on the surface of the quartz glass graphene by using a vacuum magnetron sputtering process by taking a platinum sheet as a sputtering target to prepare the graphene glass composite platinum nano particle transparent electrode.
2. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide solution sensor according to claim 1, wherein in the step (1), the carrier gas used in the normal-pressure chemical vapor deposition method is argon gas, and the reducing gas used in the normal-pressure chemical vapor deposition method is hydrogen gas; the volume ratio of the argon gas to the hydrogen gas to the carbon source gas is 28-32:3-8: 1; argon gas, hydrogen gas and carbon source gas are mixed and introduced into the system in the form of mixed gas, wherein the flow rate of the mixed gas is 100-500 sccm.
3. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide sensor according to claim 2, wherein the volume ratio of the argon gas to the hydrogen gas to the carbon source gas is 30:5: 1; the flow rate of the mixed gas is 200sccm and 400 sccm.
4. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide solution sensor according to claim 1, wherein in the step (1), the quartz glass is ultrasonically cleaned by acetone, absolute ethyl alcohol and deionized water respectively before use.
5. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide solution sensor according to claim 1, wherein in the step (1), the deposition growth time is 2-4 h.
6. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide solution sensor according to claim 5, wherein the deposition temperature is 1000 ℃ and the deposition growth time is 3 hours.
7. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide sensor according to claim 1, wherein in the step (1), 2-3 layers of graphene are deposited and grown on the surface of quartz glass.
8. The simple preparation method of the transparent electrode of the ultra-low concentration hydrogen peroxide sensor as claimed in claim 1, wherein in the step (2), in the vacuum magnetron sputtering process, the sputtering pressure is 0.2-0.8Pa, the sputtering power is 100-300W, the sputtering time is 10s-2min, and the sputtering temperature is room temperature.
9. The simple preparation method of the transparent electrode of the ultralow-concentration hydrogen peroxide solution sensor according to claim 8, wherein the sputtering power is 200W, and the sputtering time is 1 min.
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| CN115356387A (en) * | 2022-08-18 | 2022-11-18 | 北京大学 | Transparent electrochemical sensor and biosensor, and manufacturing method and application thereof |
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