CN112198203A - Preparation method of titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid - Google Patents
Preparation method of titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid Download PDFInfo
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- CN112198203A CN112198203A CN202010970532.3A CN202010970532A CN112198203A CN 112198203 A CN112198203 A CN 112198203A CN 202010970532 A CN202010970532 A CN 202010970532A CN 112198203 A CN112198203 A CN 112198203A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3277—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction being a redox reaction, e.g. detection by cyclic voltammetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention provides a preparation method of a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid, which comprises the following steps: packaging the side and the back of the pretreated titanium sheet; anodizing the packaged titanium sheet; cleaning and drying the titanium sheet after anodic oxidation; annealing the cleaned and dried titanium sheet to form anatase TiO on the surface of the titanium sheet2(ii) a Subjecting the annealed titanium sheet to NH treatment3And carrying out heat treatment in the atmosphere to obtain the titanium nitride nanowire/nanotube array integrated electrode. The preparation method of the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid provided by the invention has the advantages of easily obtained materials, simple and controllable process, capability of respectively detecting lower detection limits of dopamine and uric acid and simultaneously detecting dopamine, uric acid and ascorbic acidExhibit good resolving power.
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to a preparation method of a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid.
Background
Dopamine (DA) is a very important neurotransmitter in the central nervous system of the human body, is mainly responsible for helping cells to transmit pulses, can control people to generate different emotions, can treat depression by moderate dopamine, and is generally 0.01-1 mu mol/L in the human body. The content of Uric Acid (UA) in human body can reflect the function and metabolic condition of human body, and when the produced uric acid is accumulated in the human body, the body fluid of the human body is acidified, a series of diseases such as gout and the like can be caused, and the content of the uric acid in the human body is generally 0.2-0.5 mmol/L. When the content of the Ascorbic Acid (AA) is insufficient, various diseases can be caused, small diseases such as gingival bleeding and oral ulcer can be slightly caused, and scurvy can be caused in serious cases; however, excessive intake of the composition can also cause a series of diseases such as diarrhea and calculi. Therefore, the method has great significance for detecting dopamine, uric acid and ascorbic acid.
At present, methods for measuring dopamine, uric acid and ascorbic acid include chromatographic methods, photometric methods, electrochemical methods and the like. The chromatographic method has the advantages of simplicity, accuracy and quickness, but the qualitative capability is not high. The photometry has the advantages of low cost, simplicity, good reproducibility, accuracy and the like, and simultaneously has the defects of long time consumption, high possibility of being interfered by impurities, large harm of used reagents to human bodies and the like. Compared with the methods, the electrochemical method is unique due to the characteristics of low detection limit, low cost, simple operation, real-time analysis and the like.
Titanium nitride is a novel multifunctional material with wide application, and becomes a research hotspot in the electrochemical field because of the advantages of high chemical stability, good conductivity and the like. The titanium nitride nano material has larger specific surface area and excellent electrochemical performance, and has wide application in the fields of microelectronics, capacitors, electrocatalysis, sensors and the like. Currently, dopamine, uric acid and ascorbic acid can be detected by using a glassy carbon electrode modified by a titanium nitride material, but the current detection needs to be carried out by using the glassy carbon electrode, so that the process is complicated, and large-scale and flow preparation is not facilitated. And the titanium sheet is subjected to anodic oxidation and nitridation, the prepared titanium nitride array is used as an active material, the titanium sheet substrate which is not nitrided is used as a current collector, and the prepared titanium nitride array is used as an integrated electrode for electrochemical detection, so that the electrode preparation process can be simplified, and large-scale production is possible. At present, there is a report that the titanium nitride integrated electrode detects the three electrodes simultaneously. Therefore, the titanium nitride nanowire/nanotube array integrated electrode is constructed and applied to electrochemical detection, and has important practical significance for simultaneously detecting dopamine, uric acid and ascorbic acid.
Disclosure of Invention
The invention aims to solve the technical problem of providing a simple and feasible preparation method of a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid.
In order to solve the technical problems, the invention provides a preparation method of a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid, which comprises the following steps:
packaging the side and the back of the pretreated titanium sheet;
the packaged titanium sheet is used as an anode, a platinum sheet is used as a cathode, and the packaged titanium sheet is subjected to anodic oxidation for 50-60min in electrolyte at an oxidation voltage of 55-65V;
cleaning and drying the titanium sheet after anodic oxidation;
annealing the cleaned and dried titanium sheet to form anatase TiO on the surface of the titanium sheet2；
NH of annealed titanium sheet3Heating to 300 ℃ at the heating rate of 3 ℃/min, heating to 800-900 ℃ at the heating rate of 2 ℃/min, and carrying out heat treatment for 2-3h to obtain the titanium nitride nanowire/nanotube array integrated electrode.
Further, the titanium sheet is pretreated by polishing the titanium sheet with sand paper until no trace is formed, then performing ultrasonic treatment in acetone, ethanol and distilled water for 8-10min respectively, and finally drying the titanium sheet.
Further, the packaged titanium sheet and the packaged platinum sheet are parallelly inserted into the electrolyte at a distance of 2-3cm, and the packaged titanium sheet is subjected to anodic oxidation.
Further, the electrolyte comprises 90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water.
Further, the step of cleaning and drying the anodized titanium sheet is to wash the anodized titanium sheet with distilled water and perform ultrasonic treatment for 10-15 s.
Further, the titanium sheet annealing treatment is to place the titanium sheet in an air atmosphere and anneal the titanium sheet for 1.5 to 2.5 hours at the temperature of 400-500 ℃.
Further, the heat treatment of the titanium sheet is carried out in a chemical vapor deposition apparatus.
Further, the method comprises the steps of taking a titanium nitride nanowire/nanotube array integrated electrode as a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, 0.1mol/L, pH of 5-9 phosphate buffer solution as electrolyte, adding dopamine and uric acid into the electrolyte respectively, and detecting the oxidation current.
Further, the method comprises the steps of taking a titanium nitride nanowire/nanotube array integrated electrode as a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, 0.1mol/L, pH of 5-9 phosphate buffer solution as an electrolyte, simultaneously adding dopamine, uric acid and ascorbic acid into the electrolyte, and detecting the characteristic oxidation peaks of the three substances by using a differential pulse voltammetry method.
The preparation method of the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid adopts a widely-applied titanium sheet, and optimizes and controls the voltage and time of anodic oxidation and the heating rate during heat treatment by a simple anodic oxidation and nitridation method, so that the titanium nitride nanowire/nanotube array integrated electrode is prepared. The preparation method has the advantages of easily obtained materials, simple and controllable process, good repeatability and easy realization of industrial production. Moreover, the titanium nitride nanowire/nanotube array integrated electrode prepared by the method is applied to the detection of dopamine, uric acid and ascorbic acid, under the condition of not using a glassy carbon electrode, the detection limits of dopamine and uric acid can respectively reach 0.152 mu mol/L and 0.331 mu mol/L, and are lower than the content of human body fluid, namely, the detection limit of dopamine and uric acid is lower. Meanwhile, the titanium nitride nanowire/nanotube array integrated electrode prepared by the method can simultaneously detect the characteristic oxidation peaks of dopamine, uric acid and ascorbic acid, namely, the titanium nitride nanowire/nanotube array integrated electrode can also show good resolution capability for simultaneous detection of dopamine, uric acid and ascorbic acid.
Drawings
Fig. 1 is a flowchart of a method for preparing an integrated electrode of a titanium nitride nanowire/nanotube array for simultaneously detecting dopamine, uric acid and ascorbic acid according to an embodiment of the present invention;
FIG. 2 is an SEM image of an integrated electrode of a titanium nitride nanowire/nanotube array made according to an embodiment of the present invention;
FIG. 3 is an XRD diagram of an integrated electrode of a titanium nitride nanowire/nanotube array prepared by the embodiment of the invention;
FIG. 4 is a linear graph of the concentration of dopamine and uric acid detected by the titanium nitride nanowire/nanotube array integrated electrode manufactured in the embodiment of the present invention;
fig. 5 is a differential pulse voltammetry curve for detecting ascorbic acid, dopamine and uric acid by using the titanium nitride nanowire/nanotube array integrated electrode prepared in the embodiment of the invention.
Detailed Description
Referring to fig. 1, a method for preparing a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to an embodiment of the present invention includes the following steps:
step 1) polishing a titanium sheet by using sand paper until no mark exists, respectively carrying out ultrasonic treatment for 8-10min in acetone, ethanol and distilled water, and drying, wherein in order to facilitate the final arrangement of the nanowire/nanotube array of titanium nitride which can be formed on the surface of the titanium sheet, transparent adhesive tapes are adhered to the side face and the back face of the titanium sheet for packaging for later use.
And 2) taking the packaged titanium sheet as an anode and the packaged platinum sheet as a cathode, and inserting the titanium sheet and the platinum sheet into the prepared electrolyte at a distance of 2-3cm in parallel for anodic oxidation. The electrolyte is prepared from 90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water. In addition, in order to be beneficial to the final formation of the titanium nitride with the nanowire/nanotube array arrangement on the surface of the titanium sheet, the oxidation voltage is set to be 55-65V and the oxidation time is set to be 50-60min in the anodic oxidation process of the titanium sheet.
And 3) taking out the titanium sheet after the anodic oxidation of the titanium sheet is finished, washing with distilled water and carrying out ultrasonic treatment for 10-15s to remove residual fluorine ions on the titanium sheet.
Step 4) placing the cleaned titanium sheet in an air atmosphere, and annealing at the temperature of 400-500 ℃ for 1.5-2.5h to obtain anatase type TiO2。
Step 5) placing the annealed titanium sheet in a chemical vapor deposition instrument in NH3And carrying out heat treatment under the atmosphere. In order to be beneficial to forming the titanium nitride with the nanowire/nanotube array arrangement on the surface of the titanium sheet, the heat treatment method is designed as follows: the temperature is raised to 300 ℃ at the speed of 3 ℃/min, then raised to 900 ℃ at the speed of 2 ℃/min and kept for 2-3 h. Finally obtaining the titanium nitride nanowire/nanotube array integrated electrode.
And scanning the prepared titanium nitride nanowire/nanotube array integrated electrode by using a field emission scanning electron microscope to represent the morphology and the structure of the integrated electrode. As can be seen from FIG. 2, the titanium nitride nanowire/nanotube array integrated electrode prepared by the invention uniformly covers a layer of nanowires on the surface of the compact nanotube array, and obviously belongs to a single crystal structure. As can be shown in FIG. 3, the nanowire/nanotube array homojunction of the titanium nitride nanowire/nanotube array integrated electrode prepared by the method is a pure titanium nitride phase, and no TiO is present2And the titanium sheet which is not nitrided is left at the bottom of the titanium nitride, and due to the metal characteristic of the titanium sheet, the titanium sheet can play a role of a current collector and is beneficial to charge transmission. Therefore, the titanium nitride nanowire/nanotube array integrated electrode can be prepared by an anodic oxidation method.
The titanium nitride nanowire/nanotube array integrated electrode prepared by the method is used as a working electrode, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, phosphate buffer solution with pH of 5-9 and concentration of 0.1mol/L is used as electrolyte, dopamine and uric acid are respectively added into the electrolyte, and oxidation current is detected. Referring to fig. 4, according to the graph, it can be calculated that the detection limits of the titanium nitride nanowire/nanotube array integrated electrode to dopamine and uric acid are respectively 0.152 μmol/L and 0.331 μmol/L, which are lower than the content of dopamine and uric acid in the body fluid, so that the titanium nitride nanowire/nanotube array integrated electrode prepared by the invention can be used for detecting dopamine and uric acid in the human body.
The titanium nitride nanowire/nanotube array integrated electrode prepared by the method is used as a working electrode, a platinum wire is used as a counter electrode, Ag/AgCl is used as a reference electrode, phosphate buffer solution with pH of 5-9 and concentration of 0.1mol/L is used as electrolyte, dopamine, uric acid and ascorbic acid are added into the electrolyte at the same time, and the characteristic oxidation peaks of the three substances are detected by using a differential pulse voltammetry method. Referring to fig. 5, three well-separated characteristic oxidation peaks belonging to ascorbic acid, dopamine and uric acid respectively can be observed, and the peak positions of the three peaks are not interfered with each other, so that the titanium nitride nanowire/nanotube array integrated electrode prepared by the invention has the capability of simultaneously detecting ascorbic acid, dopamine and uric acid, and has the potential of practical application.
Example 1
(1) Polishing the titanium sheet with sand paper until no mark exists, performing ultrasonic treatment in acetone, ethanol and distilled water for 8min, drying, and sticking transparent adhesive tapes on the side and back of the titanium sheet for packaging.
(2) The titanium sheet is used as an anode, the platinum sheet is used as a cathode, the titanium sheet and the platinum sheet are inserted into the prepared electrolyte (90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water) in parallel at a distance of 2cm for anodic oxidation, the anodic oxidation voltage is 55V, and the oxidation time is 60 min. The titanium sheet was removed, rinsed with distilled water and sonicated for 10s to remove residual fluoride ions.
(3) Placing the anodized titanium sheet in air, and annealing at 400 deg.C for 2.5h to obtain anatase type TiO2。
(4) Placing the annealed titanium sheet in a chemical vapor deposition instrument in NH3And (3) carrying out heat treatment under the atmosphere, raising the temperature to 300 ℃ at a speed of 3 ℃/min, then raising the temperature to 800 ℃ at a speed of 2 ℃/min, and carrying out heat preservation for 3h to obtain the titanium nitride nanowire/nanotube array integrated electrode.
(5) The method comprises the steps of taking a titanium nitride nanowire/nanotube array integrated electrode as a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, 0.1mol/L phosphate buffer solution (pH is 5-9) as electrolyte, respectively adding 5-175 mu mol/L dopamine and 30-215 mu mol/L uric acid into the electrolyte, and detecting oxidation current to obtain a current density which is in a linear relation with the concentrations of the dopamine and the uric acid.
(6) Under the detection condition of the step (5), 3 mu mol/L dopamine, 10 mu mol/L uric acid and 50 mu mol/L ascorbic acid are added into the electrolyte at the same time, the characteristic oxidation peaks of the three substances are detected by using a differential pulse voltammetry method, the obtained result can obviously distinguish the oxidation peaks of the three substances with good separation, and the simultaneous detection capability of the electrode on dopamine, uric acid and ascorbic acid is proved.
Example 2
(1) Polishing the titanium sheet with sand paper until no mark exists, performing ultrasonic treatment in acetone, ethanol and distilled water for 9min, drying, and sticking transparent adhesive tapes on the side and back of the titanium sheet for packaging.
(2) The titanium sheet is used as an anode, the platinum sheet is used as a cathode, the titanium sheet and the platinum sheet are parallelly inserted into the prepared electrolyte (90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water) at a distance of 2.5cm for anodic oxidation, the anodic oxidation voltage is 60V, and the oxidation time is 55 min. The titanium plate was removed, rinsed with distilled water and sonicated for 13s to remove residual fluoride ions.
(3) Placing the anodized titanium sheet in air, and annealing at 450 deg.C for 2h to obtain anatase type TiO2。
(4) Placing the annealed titanium sheet in a chemical vapor deposition instrument in NH3And (3) carrying out heat treatment under the atmosphere, raising the temperature to 300 ℃ at a speed of 3 ℃/min, then raising the temperature to 850 ℃ at a speed of 2 ℃/min, and carrying out heat preservation for 2.5h to obtain the titanium nitride nanowire/nanotube array integrated electrode.
(5) The method comprises the steps of taking a titanium nitride nanowire/nanotube array integrated electrode as a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, 0.1mol/L phosphate buffer solution (pH is 5-9) as electrolyte, respectively adding 5-175 mu mol/L dopamine and 30-215 mu mol/L uric acid into the electrolyte, and detecting oxidation current to obtain a current density which is in a linear relation with the concentrations of the dopamine and the uric acid.
(6) Under the detection condition of the step (5), 3 mu mol/L dopamine, 10 mu mol/L uric acid and 50 mu mol/L ascorbic acid are added into the electrolyte at the same time, the characteristic oxidation peaks of the three substances are detected by using a differential pulse voltammetry method, the obtained result can obviously distinguish the oxidation peaks of the three substances with good separation, and the simultaneous detection capability of the electrode on dopamine, uric acid and ascorbic acid is proved.
Example 3
(1) Polishing the titanium sheet with sand paper until no mark exists, performing ultrasonic treatment in acetone, ethanol and distilled water for 10min, drying, and sticking transparent adhesive tapes on the side and back of the titanium sheet for packaging.
(2) The titanium sheet is used as an anode, the platinum sheet is used as a cathode, the titanium sheet and the platinum sheet are inserted into the prepared electrolyte (90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water) in parallel at a distance of 3cm for anodic oxidation, the anodic oxidation voltage is 65V, and the oxidation time is 50 min. The titanium plate was removed, rinsed with distilled water and sonicated for 15s to remove residual fluoride ions.
(3) Placing the anodized titanium sheet in air, and annealing at 500 deg.C for 1.5h to obtain anatase type TiO2。
(4) Placing the annealed titanium sheet in a chemical vapor deposition instrument in NH3And (3) carrying out heat treatment under the atmosphere, raising the temperature to 300 ℃ at a speed of 3 ℃/min, then raising the temperature to 900 ℃ at a speed of 2 ℃/min, and carrying out heat preservation for 2h to obtain the titanium nitride nanowire/nanotube array integrated electrode.
(5) The method comprises the steps of taking a titanium nitride nanowire/nanotube array integrated electrode as a working electrode, a platinum wire as a counter electrode, Ag/AgCl as a reference electrode, 0.1mol/L phosphate buffer solution (pH is 5-9) as electrolyte, respectively adding 5-175 mu mol/L dopamine and 30-215 mu mol/L uric acid into the electrolyte, and detecting oxidation current to obtain a current density which is in a linear relation with the concentrations of the dopamine and the uric acid.
(6) Under the detection condition of the step (5), 3 mu mol/L dopamine, 10 mu mol/L uric acid and 50 mu mol/L ascorbic acid are added into the electrolyte at the same time, the characteristic oxidation peaks of the three substances are detected by using a differential pulse voltammetry method, the obtained result can obviously distinguish the oxidation peaks of the three substances with good separation, and the simultaneous detection capability of the electrode on dopamine, uric acid and ascorbic acid is proved.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. A preparation method of a titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid is characterized by comprising the following steps:
packaging the side and the back of the pretreated titanium sheet;
the packaged titanium sheet is used as an anode, a platinum sheet is used as a cathode, and the packaged titanium sheet is subjected to anodic oxidation for 50-60min in electrolyte at an oxidation voltage of 55-65V;
cleaning and drying the titanium sheet after anodic oxidation;
annealing the cleaned and dried titanium sheet to form anatase TiO on the surface of the titanium sheet2；
NH of annealed titanium sheet3Heating to 300 ℃ at the heating rate of 3 ℃/min, heating to 800-900 ℃ at the heating rate of 2 ℃/min, and carrying out heat treatment for 2-3h to obtain the titanium nitride nanowire/nanotube array integrated electrode.
2. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 1, which is characterized in that: the pretreatment of the titanium sheet is to polish the titanium sheet by using sand paper until no mark exists, then respectively perform ultrasonic treatment for 8-10min in acetone, ethanol and distilled water, and finally dry the titanium sheet.
3. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 1, which is characterized in that: and the packaged titanium sheet and the packaged platinum sheet are parallelly inserted into the electrolyte at a distance of 2-3cm, and the packaged titanium sheet is subjected to anodic oxidation.
4. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 3, wherein the method comprises the following steps: the electrolyte comprises 90 vol% of ethylene glycol, 0.5 wt% of ammonium fluoride and distilled water.
5. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 1, which is characterized in that: and the step of cleaning and drying the titanium sheet after the anodic oxidation is to wash the titanium sheet after the anodic oxidation with distilled water and perform ultrasonic treatment for 10-15 s.
6. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 1, which is characterized in that: the titanium sheet annealing treatment is to place the titanium sheet in an air atmosphere and anneal the titanium sheet for 1.5 to 2.5 hours at the temperature of 400-500 ℃.
7. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to claim 1, which is characterized in that: the heat treatment of the titanium sheet is carried out in a chemical vapor deposition apparatus.
8. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to any one of claims 1 to 7, wherein the method comprises the following steps: the method also comprises the steps of taking the titanium nitride nanowire/nanotube array integrated electrode as a working electrode, taking a platinum wire as a counter electrode, taking Ag/AgCl as a reference electrode, taking 0.1mol/L, pH phosphate buffer solution of 5-9 as electrolyte, respectively adding dopamine and uric acid into the electrolyte, and detecting the oxidation current.
9. The method for preparing the titanium nitride nanowire/nanotube array integrated electrode for simultaneously detecting dopamine, uric acid and ascorbic acid according to any one of claims 1 to 7, wherein the method comprises the following steps: the method also comprises the steps of taking the titanium nitride nanowire/nanotube array integrated electrode as a working electrode, taking a platinum wire as a counter electrode, taking Ag/AgCl as a reference electrode, taking 0.1mol/L, pH phosphate buffer solution of 5-9 as electrolyte, simultaneously adding dopamine, uric acid and ascorbic acid into the electrolyte, and detecting the characteristic oxidation peaks of the three substances by using a differential pulse voltammetry.
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