CN112461907B - Application of nano zinc oxide and graphene oxide composite material in electrochemical detection of dopamine - Google Patents
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Abstract
The invention provides a nano zinc oxide and reduced graphene oxide composite material and a preparation method and application thereof. The surface of the nano zinc oxide is pretreated, and then the nano zinc oxide and the prepared redox graphene are stirred and mixed, the nano zinc oxide and the prepared redox graphene are self-assembled and uniformly dispersed, so that ZnO is uniformly dispersed, and an electrochemical sensor prepared by the composite material in the follow-up process has higher sensitivity to a measured substance; the electrochemical sensor has simple experimental method and easily-achieved experimental conditions, and effectively improves the specific surface area and the active sites of the electrode material of the sensor, thereby improving the detection sensitivity and reducing the detection limit.
Description
Technical Field
The invention relates to the technical field of electrochemical sensing, in particular to a nano zinc oxide and reduced graphene oxide composite material electrochemical sensor and a preparation method and application thereof.
Background
Graphene is a two-dimensional material with excellent performance because of its unique structure, which provides excellent electron transport capability. Zinc oxide has various structures and good thermal stability, and is widely used for biosensing due to its bionic property and high electron transmission capability. The nano-zinc oxide and reduced graphene oxide composite electrode is also developed for detecting substances such as dopamine, ascorbic acid and the like. However, most of the adopted methods are one-pot methods, and ZnO is dispersed unevenly, so that the sensitivity of the composite electrode to a measured substance is reduced.
Disclosure of Invention
The invention overcomes the defects in the prior art, and provides a nano zinc oxide and reduced graphene oxide composite material, a preparation method and application thereof, wherein gold is used as a conductive substrate, nano zinc oxide (ZnO) and reduced graphene oxide are used as basic materials, the mixed suspension of the two is dripped on the conductive substrate, and an electrochemical sensor is obtained after electrochemical reduction is carried out on the composite electrode, and the sensor has high selectivity on dopamine and obviously improves the sensitivity; more importantly, the method adopts electrochemical reduction instead of hydrothermal method, and the operation steps are simple.
The purpose of the invention is realized by the following technical scheme.
A nano zinc oxide and reduced graphene oxide composite material and a preparation method thereof are carried out according to the following steps:
Ultrasonically dispersing nano zinc oxide particles in absolute ethyl alcohol, then adding 3-Aminopropyltriethoxysilane (APTES) into the dispersion liquid, refluxing in a water bath at 50-90 ℃, centrifuging, washing and drying to obtain pretreated nano zinc oxide, wherein the mass volume ratio of the nano zinc oxide to the 3-Aminopropyltriethoxysilane (APTES) is (0.1-12): (3-60);
Adding concentrated sulfuric acid into a beaker, heating to 80-100 ℃, then sequentially adding dipotassium persulfate and phosphorus pentoxide into the concentrated sulfuric acid, then slowly adding graphite powder, heating and stirring the mixture at 80-100 ℃ for 4-8h, cooling, then slowly diluting the mixture with deionized water, then centrifugally washing the mixture with deionized water to pH =7, and drying the obtained solid product in the air at room temperature (20-25 ℃) to obtain redox Graphene (GO), wherein the volume mass ratio of the added concentrated sulfuric acid, the dipotassium persulfate, the phosphorus pentoxide and the graphite powder is (10-50): (1-8): (3-12): (1-12);
step 3, preparing the nano zinc oxide and redox graphene composite material
Preparing the pretreated nano zinc oxide obtained in the step 1 and water into a nano zinc oxide suspension, preparing the redox Graphene (GO) obtained in the step 2 into a redox Graphene (GO) suspension with the same mass part as the nano zinc oxide suspension, stirring and mixing the nano zinc oxide suspension and the redox Graphene (GO) suspension to obtain a mixed suspension, dripping 4-10 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material, wherein the concentration of the nano zinc oxide suspension is 1-15mg/ml, and the concentration of the redox Graphene (GO) suspension is 1-15mg/ml.
In the step 1, the nano zinc oxide is 0.2 to 10 parts by mass, the particle size is 20 to 70nm, the ultrasonic time is 10 to 120min, the volume fraction of the APTES is 98 percent, the volume is 5 to 50 parts by volume, and the water bath reflux temperature is 60 to 80 ℃.
In step 2, concentrated sulfuric acid (H) 2 SO 4 ) 15-40 parts by volume of (A), heating temperature is 90 ℃, and the volume of the potassium persulfate (K) is 2 S 2 O 4 ) 2 to 7 parts by mass of phosphorus pentoxide (P) 2 O 5 ) The mass of the graphite powder is 4-10 parts by mass, and the mass of the graphite powder is 2-10 parts by mass.
In the step 3, the concentration of the nano zinc oxide suspension is 1-10mg/ml, and the concentration of the redox Graphene (GO) suspension is 1-10mg/ml.
Wherein 1 part by mass means 1g, and one part by volume means 1ml.
The application of the nano zinc oxide and reduced graphene oxide composite material in electrochemical detection of dopamine is characterized in that the nano zinc oxide and reduced graphene oxide composite material is placed in a solution to be detected for electrochemical reduction, a downward peak current value is generated, the downward peak current value is recorded, and a concentration curve with good linearity is obtained after the downward peak current value is analyzed, wherein the curve formula is y = -0.26x-1.23, y is the peak current value, x is the dopamine concentration, and R is the dopamine concentration 2 =0.998, sensitivity 260nA/μmol.
The solution to be detected is a dipotassium hydrogen phosphate and potassium dihydrogen Phosphate Buffer Solution (PBS) of dopamine, the concentration of the dopamine is 1-70 mu mol/L, the voltage of electrochemical reduction is-1.2-0V, the scanning speed is 40-100mv/s, and the cycle number is 15-30 circles.
The invention has the beneficial effects that: the surface of the nano zinc oxide and reduced graphene oxide composite material prepared by the invention is pretreated, and then the nano zinc oxide and the reduced graphene oxide composite material are stirred and mixed, and the nano zinc oxide and the reduced graphene oxide composite material are self-assembled and uniformly dispersed, so that ZnO is uniformly dispersed, and an electrochemical sensor prepared by the composite material is higher in sensitivity to a measured substance; the nano-zinc oxide and reduced graphene oxide composite electrochemical sensor prepared by the invention has the advantages of simple experimental method and easily-achieved experimental conditions, effectively improves the specific surface area and the active sites of the electrode material of the sensor, thereby improving the detection sensitivity, reducing the detection limit and providing a new method for the practical detection application of the electrochemical sensor.
Drawings
Fig. 1 is a photograph of a suspension of a nano zinc oxide and redox graphene composite prepared according to the present invention;
FIG. 2 is a scanning electron micrograph of the nano-zinc oxide purchased from the present invention;
FIG. 3 is an electron micrograph of redox graphene prepared according to the present invention;
FIG. 4 is an electron microscope photograph of the nano-zinc oxide and redox graphene composite material prepared by the present invention;
fig. 5 is a picture of the differential pulse voltammetry detection of dopamine with different concentrations in an electrochemical workstation using the nano zinc oxide and redox graphene composite prepared by the present invention, wherein (1) is a DPV curve, and (2) is a concentration curve;
fig. 6 is a sweep rate diagram of the electrode of the electrochemical sensor made of the nano zinc oxide and redox graphene composite material, wherein (1) is a cyclic voltammetry curve, and (2) is a current intensity curve.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1:
ultrasonically dispersing 0.5g of nano zinc oxide particles in 200ml of absolute ethyl alcohol, then adding 0.5ml of APTES, carrying out water bath reflux treatment at 60 ℃ for 4h, then centrifuging ZnO nano particles, cleaning the ZnO nano particles for a plurality of times by using the absolute ethyl alcohol, then placing the ZnO nano particles in a 70 ℃ drying oven for full drying, carrying out water bath reflux, centrifuging, washing and drying to obtain the pretreated nano zinc oxide particles.
25ml of concentrated sulfuric acid was added to a 250ml beaker and heated to 90 ℃. Then sequentially adding 5gK 2 S 2 O 8 And 5gP 2 O 5 Then, 5g of graphite powder was slowly added. The mixture was heated at 90 ℃ with stirring for 5h. After cooling, the mixture was slowly diluted with deionized water. The mixture was then washed with deionized water to PH =7 and the resulting product was dried at room temperature.
And respectively preparing 5mg/ml suspension of the obtained nano zinc oxide particles and redox graphene with water, stirring and mixing to obtain the suspension shown in figure 1, dripping 6 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material.
The nano zinc oxide in example 1 is morphologically scanned by a Scanning Electron Microscope (SEM), and the nano zinc oxide is found to have a particle size of 10-40nm, as shown in fig. 2.
The redox graphene prepared in example 1 was scanned by a Scanning Electron Microscope (SEM) and found to be a lamellar layer, as shown in fig. 3.
As shown in fig. 4, the nano zinc oxide is found to be uniformly dispersed on the surface of the graphene by scanning of the scanning electron microscope.
Example 2:
ultrasonically dispersing 1g of nano zinc oxide particles in 250ml of absolute ethyl alcohol, then adding 1ml of APTES, carrying out water bath reflux treatment for 4 hours at the temperature of 60 ℃, then centrifuging ZnO nano particles, cleaning the ZnO nano particles for a plurality of times by using the absolute ethyl alcohol, then placing the ZnO nano particles in a 70 ℃ drying oven for fully drying, carrying out water bath reflux, centrifuging, washing and drying to obtain the pretreated nano zinc oxide particles.
20ml of concentrated sulfuric acid was added to a 250ml beaker and heated to 80 ℃. Then sequentially adding 2.5gK 2 S 2 O 8 And 2.5gP 2 O 5 Then, 5g of graphite powder was slowly added. The mixture was heated at 80 ℃ with stirring for 5h. After cooling, the mixture was slowly diluted with deionized water. The mixture was then washed with deionized water to PH =7 and the resulting product was dried at room temperature.
And respectively preparing the obtained nano zinc oxide particles and redox graphene with water into 3mg/ml suspension, stirring and mixing to obtain suspension, dripping 4 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material.
Example 3:
ultrasonically dispersing 2.5g of nano zinc oxide particles in 200ml of absolute ethyl alcohol, then adding 5ml of APTES, carrying out water bath reflux treatment for 4h at 60 ℃, then centrifuging ZnO nano particles, cleaning the ZnO nano particles for a plurality of times by using the absolute ethyl alcohol, then placing the ZnO nano particles in a 70 ℃ drying oven for fully drying, carrying out water bath reflux, centrifuging, washing and drying to obtain the pretreated nano zinc oxide particles.
25ml of concentrated sulfuric acid was added to a 250ml beaker and heated to 100 ℃. Then add 5gK in turn 2 S 2 O 8 And 5gP 2 O 5 Then, 5g of graphite powder was slowly added. The mixture was heated at 100 ℃ with stirring for 5h. After cooling, the mixture was slowly diluted with deionized water. The mixture was then washed with deionized water to PH =7 or so and the resulting product was dried at room temperature.
And respectively preparing 5mg/ml suspension of the obtained nano zinc oxide particles and redox graphene with water, stirring and mixing to obtain suspension, dripping 10 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material.
Example 3:
ultrasonically dispersing 0.1g of nano zinc oxide particles in 200ml of absolute ethyl alcohol, then adding 3ml of APTES, carrying out water bath reflux treatment for 4 hours at 60 ℃, then centrifuging the ZnO nano particles, cleaning the ZnO nano particles by the absolute ethyl alcohol for several times, then placing the ZnO nano particles in a 70 ℃ drying oven for fully drying, carrying out water bath reflux, centrifuging, washing and drying to obtain the pretreated nano zinc oxide particles.
20ml of concentrated sulfuric acid was added to a 250ml beaker and heated to 95 ℃. Then 1gK was added in sequence 2 S 2 O 8 And 3gP 2 O 5 Then, 1g of graphite powder was slowly added. The mixture was heated to 95 ℃ with stirring for 5h. After cooling, it is deionizedThe water slowly diluted the mixture. The mixture was then washed with deionized water to PH =7 and the resulting product was dried at room temperature.
And respectively preparing the obtained nano zinc oxide particles and redox graphene with water into 15mg/ml suspension, stirring and mixing to obtain suspension, dripping 9 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material.
Example 4:
ultrasonically dispersing 12g of nano zinc oxide particles into 200ml of absolute ethyl alcohol, then adding 3ml of APTES, carrying out water bath reflux treatment for 4h at the temperature of 60 ℃, then centrifuging ZnO nano particles, cleaning the ZnO nano particles for a plurality of times by using the absolute ethyl alcohol, then placing the ZnO nano particles into a 50 ℃ drying oven for fully drying, carrying out water bath reflux, centrifuging, washing and drying to obtain the pretreated nano zinc oxide particles.
50ml of concentrated sulfuric acid was added to a 250ml beaker and heated to 85 ℃. Then sequentially adding 8gK 2 S 2 O 8 And 12gP 2 O 5 Then, 12g of graphite powder was slowly added. The mixture was heated at 90 ℃ with stirring for 5h. After cooling, the mixture was slowly diluted with deionized water. The mixture was then washed with deionized water to PH =7 and the resulting product was dried at room temperature.
And respectively preparing the obtained nano zinc oxide particles and redox graphene with water into 1mg/ml suspension, stirring and mixing to obtain suspension, dripping 8 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain the nano zinc oxide and redox graphene composite material.
Example 5:
and (4) placing the nano zinc oxide and reduced graphene composite material finally obtained in the embodiment 3 in a buffer solution for electrochemical reduction, wherein the voltage of the electrochemical reduction is-1.5-0V, the scanning speed is 30-120mv/s, and the cycle number is 10-40 circles, so that the nano zinc oxide and reduced graphene composite material electrochemical sensor is obtained. And performing electrochemical reduction and test on the sample by adopting a three-electrode test system, and performing electrochemical reduction and test by using an electrochemical workstation CHI-660E.
(1) The dried electrode was subjected to electrochemical reduction in PBS solution (PH = 7): the voltage range is: 1.2-0V, scanning speed of 50mv/s and cycle number of 15.
(2) Performing electrochemical test on the reduced electrode obtained in the step (1) by adopting differential pulse voltammetry: the electrode is placed in PBS buffer solution to carry out differential pulse voltammetry to test peak current, the voltage range is 0-0.5V, the scanning speed is 100mv/s, and the pulse period is 0.05s -1 . The substance to be detected is dopamine, the concentration range of the dopamine is 1-70 mu mol/L, the specific concentration is 5 10 15 20 25 30 35 40 45 50 60 mu mol/L, and a DPV curve is finally obtained, as shown in fig. 5 (1), when the voltage is 0.15 +/-0.01V, the current has a downward peak, and through analysis, a concentration curve with good linearity can be obtained as shown in fig. 5 (2), y = -0.26x-1.23, wherein y is the current peak, x is the dopamine concentration, R is 2 =0.998, sensitivity 260nA/μmol.
(3) And (3) performing sweeping speed electrochemical test on the reduced electrode obtained in the step (1), placing the electrode in a PBS (phosphate buffer solution) buffer solution to perform cyclic voltammetry to test peak current, wherein the voltage range is-0.2-0.6V, and the scanning speed is 20-40 60 100mv/s. The cyclic voltammogram shown in fig. 6 (1) was obtained, and the sweep rate and the current intensity were well linear as shown in fig. 6 (2).
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (5)
1. An application of a nano zinc oxide and graphene oxide composite material in electrochemical detection of dopamine is characterized in that: the nano zinc oxide and graphene oxide composite material is prepared according to the following steps:
step 1, carrying out pretreatment on nano zinc oxide
Ultrasonically dispersing nano zinc oxide particles in absolute ethyl alcohol, then adding 3-aminopropyltriethoxysilane APTES into dispersion liquid, refluxing in a water bath at 50-90 ℃, centrifugally washing and drying to obtain pretreated nano zinc oxide, wherein the addition mass volume ratio of the nano zinc oxide to the 3-aminopropyltriethoxysilane APTES is (0.1-12): (3-60); the mass of the nano zinc oxide particles is 0.2-10 parts, and the particle size is 20-70 nm;
step 2, preparing graphene oxide GO
Adding concentrated sulfuric acid into a beaker, heating to 80-100 ℃, then sequentially adding dipotassium persulfate and phosphorus pentoxide into the concentrated sulfuric acid, then slowly adding graphite powder, heating and stirring the mixture at 80-100 ℃ for 4-8h, cooling, slowly diluting the mixture with deionized water, then centrifugally washing the mixture with deionized water to pH =7, and drying the obtained solid product in air at room temperature of 20-25 ℃ to obtain graphene oxide GO, wherein the adding volume-mass ratio of the concentrated sulfuric acid, the dipotassium persulfate, the phosphorus pentoxide and the graphite powder is (10-50): (1-8): (3-12): (1-12);
step 3, preparing the nano zinc oxide and graphene oxide composite material
Preparing the pretreated nano zinc oxide obtained in the step 1 and water into a nano zinc oxide suspension, preparing the graphene oxide GO obtained in the step 2 into a graphene oxide GO suspension with the same mass part as the nano zinc oxide suspension, stirring and mixing the nano zinc oxide suspension and the graphene oxide GO suspension to obtain a mixed suspension, dripping 4-10 mu L of the mixed suspension on the surface of a gold electrode, and air-drying to obtain a nano zinc oxide and graphene oxide composite material, wherein the concentration of the nano zinc oxide suspension is 1-15mg/ml, and the concentration of the graphene oxide GO suspension is 1-15mg/ml;
placing the nano zinc oxide and graphene oxide composite material in a solution to be detected for electrochemical reduction, recording the downward peak value of current when the current appears at the downward peak value, and analyzing the downward peak value of current to obtain a concentration curve with good linearity, wherein the curve formula is y = -0.26x-1.23, y is the current peak value, x is the dopamine concentration, and R is the dopamine concentration 2 =0.998, sensitivity 260nA/μmol.
2. The application of the nano zinc oxide and graphene oxide composite material in the electrochemical detection of dopamine according to claim 1 is characterized in that: in step 1, the ultrasonic time is 10-120min, the volume fraction of APTES is 98%, the volume is 5-50 parts, and the reflux temperature of the water bath is 60-80 ℃.
3. The application of the nano zinc oxide and graphene oxide composite material in the electrochemical detection of dopamine according to claim 1 is characterized in that: in step 2, concentrated sulfuric acid H 2 SO 4 15-40 parts by volume of (A), the heating temperature is 90 ℃, and the dipotassium persulfate K 2 S 2 O 4 2-7 parts by mass of phosphorus pentoxide P 2 O 5 The mass of the graphite powder is 4-10 parts by mass, and the mass of the graphite powder is 2-10 parts by mass.
4. The application of the nano zinc oxide and graphene oxide composite material in the electrochemical detection of dopamine according to claim 1 is characterized in that: in step 3, the concentration of the nano zinc oxide suspension is 1-10mg/ml, and the concentration of the graphene oxide GO suspension is 1-10mg/ml.
5. The application of the nano zinc oxide and graphene oxide composite material in the electrochemical detection of dopamine according to claim 1 is characterized in that: the solution to be detected is buffer solution PBS of dipotassium hydrogen phosphate and potassium dihydrogen phosphate of dopamine, the concentration of dopamine is 1-70 mu mol/L, the voltage of electrochemical reduction is-1.2-0V, the scanning speed is 40-100mv/s, and the cycle number is 15-30 circles.
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