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Preparation method of electrochemical sensor electrode material for detecting aniline

A sensor electrode and electrochemical technology, applied in the direction of material electrochemical variables, gaseous chemical plating, metal material coating technology, etc., can solve the problems of complex coupling and synergistic effects, and achieve large detection range, high detection sensitivity, repeatability The detection effect is stable

Pending Publication Date: 2021-07-16
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Boron-nitrogen co-doped diamond also has good conductivity, and the coupling and synergistic effects of the two doped atoms are complex, and the influence on the electrochemical performance of the diamond film is still in the research stage
At present, no researchers have applied boron-nitrogen co-doped diamond films to the electrochemical detection of aniline.

Method used

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  • Preparation method of electrochemical sensor electrode material for detecting aniline
  • Preparation method of electrochemical sensor electrode material for detecting aniline
  • Preparation method of electrochemical sensor electrode material for detecting aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: boron, nitrogen co-doped diamond film deposition

[0023] A p-type doped (100) single crystal silicon wafer was ground for 15 minutes with diamond powder with a particle size of 500 microns, and then placed in a microwave plasma chemical vapor deposition equipment chamber for boron and nitrogen co-doped diamond film deposition. During the deposition process, the microwave power was 1kW; the gas flow rate was 200 sccm hydrogen, 6 sccm methane, 2 sccm trimethyl borate, and 2 sccm nitrogen; the gas pressure was 8 kPa, the substrate temperature was 900 °C, and the growth time was 6 hours. Scanning electron microscope tests show that the boron and nitrogen co-doped diamond film grain structure obtained by growth is compact and complete, and the grain size is about 1 to 2 microns (see figure 1 ). Denoted as sample 1. The sample has good electrical conductivity, which meets the application requirements of electrochemical electrodes.

Embodiment 2

[0024] Embodiment 2: Boron-doped diamond film growth

[0025] A p-type doped (100) single crystal silicon wafer was ground for 15 minutes with diamond powder with a particle size of 500 microns, and then placed in a microwave plasma chemical vapor deposition equipment chamber for boron-doped diamond film deposition. The deposition gas flow rate is 200 sccm of hydrogen, 6 sccm of methane, and 2 sccm of trimethyl borate. The growth pressure was 8 kPa, the substrate temperature was 900° C., and the growth time was 6 hours. Scanning electron microscopy tests show that the grown boron-doped diamond film grain structure is compact and complete, and the grain size is about 2 to 3 microns (see figure 2 ). Denoted as sample 2. The sample has good conductivity, which meets the application requirements of electrochemical electrodes.

Embodiment 3

[0026] Example 3: Comparison of electrochemical properties of boron-doped and boron-nitrogen co-doped diamond films

[0027] The doped diamond films prepared in Example 1 and Example 2 were used to make electrochemical electrodes respectively, and the electrodes were tested by linear sweep voltammetry in 0.5M sulfuric acid solution. From the test results ( image 3 ) It can be seen that the potential window of the boron-nitrogen co-doped diamond electrode is almost as wide as that of the boron-doped diamond electrode, but its reaction current is much larger than that of the latter. The large reaction current makes the boron-nitrogen co-doped diamond electrode have higher test sensitivity than the boron-doped diamond electrode, so more excellent sensor performance can be obtained.

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Abstract

The invention relates to a preparation method of an electrochemical sensor electrode material for detecting aniline, and belongs to the technical field of electrochemical sensors, wherein the method comprises the specific steps: by taking a P-type doped monocrystalline silicon wafer as a substrate, treating the surface of the silicon wafer by utilizing micron diamond powder through a manual grinding method or an ultrasonic oscillation method, cleaning by utilizing alcohol, and depositing a boron and nitrogen co-doped diamond film by using a microwave plasma chemical vapor deposition method to obtain the electrochemical sensor electrode material for detecting aniline. The prepared electrode material has good electrochemical performance, the electrode material is used as a working electrode for electrochemical detection of aniline, extremely high detection sensitivity is achieved, meanwhile, the detection range is large, and repeatability is good.

Description

technical field [0001] The invention belongs to the technical field of electrochemical sensors, and relates to a boron and nitrogen co-doped conductive diamond sensor electrode capable of detecting aniline and a preparation method thereof. Background technique [0002] Aniline is an important industrial raw material, widely used in printing and dyeing, dyes, rubber, pharmaceuticals, explosives and pesticides and other industries. It can be absorbed into the body through the skin, respiratory tract and digestive tract and cause damage to the central nervous system of animals. It is highly toxic and highly toxic. The minimum lethal concentration for mice inhaled for 4 hours is 250ppm. In the "Environmental Quality Standards for Surface Water" (GB 3838—2002), the standard limit for aniline is 100 μg / L. At present, the methods for detecting aniline in water mainly include spectrophotometry, liquid chromatography / mass spectrometry, gas chromatography / mass spectrometry, etc. Spe...

Claims

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Application Information

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IPC IPC(8): G01N27/30C23C16/27
CPCG01N27/30C23C16/277C23C16/274
Inventor 李红东李佳翰刘钧松高楠王启亮成绍恒
Owner JILIN UNIV
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