Boron-doped diamond modified attenuated total reflection wafer and preparation method and application thereof

A boron-doped diamond and attenuated total reflection technology, applied in the field of attenuated total reflection wafers, can solve the problems of low catalytic activity, low electrode conductivity, narrow application range, etc., and achieve simple experimental operation, not easy to fall off, and strong repeatability Effect

Active Publication Date: 2018-12-21
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the above defects or improvement needs of the prior art, the invention provides a boron-doped diamond film (BDD) modified ATR wafer for infrared in-situ electrochemical detection, the purpose of which is to make infrared light in the ATR crystal of the wafer Refraction and reflection occur inside, and total reflection occurs in the BDD film to enhance the infrared signal and make the BDD film have a certain degree of conductivity. The BDD film is used as the working electrode and put into the electrolytic cell, and the reference electrode and the counter electrode are inserted at the same time to form an electrochemical cell. Spectrum three-electrode system, thus solving the problem of low catalytic activity, low oxygen evolution potential, low electrode conductivity, short service life and wide application range of existing metal electrodes, carbon electrodes and metal oxide electrodes deposited on the surface of ATR crystals narrow technical issues

Method used

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  • Boron-doped diamond modified attenuated total reflection wafer and preparation method and application thereof
  • Boron-doped diamond modified attenuated total reflection wafer and preparation method and application thereof
  • Boron-doped diamond modified attenuated total reflection wafer and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Steps of BDD film deposition on silicon wafer by hot wire chemical vapor phase:

[0050] (1) Substrate pretreatment. Prepare an ATR made of Si material as the substrate, with a length of 8cm, a width of 5cm, and a height of 1cm. The infrared light can be reflected and refracted in the lower ATR in the range of incident angle 23-45°, and can be totally reflected in the upper BDD film. The surface is mechanically polished to Mirror finish. Then apply 0.1-0.5 μm diamond abrasive paste on the polished upper surface of Si and grind for 10 minutes to increase the nucleation density. Then use alcohol to ultrasonically clean for 30 minutes to remove oil stains on the surface of the substrate. In order to increase the diamond nucleation point on the crystal surface, put the cleaned sample into the acetone suspension of diamond nanopowder for ultrasonic seeding for 30 minutes, and then dry it in the air. It can leave defects and high-energy sites on the surface.

[0051] (2) ...

Embodiment 2

[0056] The BDD film prepared in Example 1 was used as a working electrode for electrochemical in-situ infrared spectroscopy detection: figure 2 It is one of the schematic diagrams of the cooperating use of the boron-doped diamond-modified ATR chip for infrared in-situ electrochemical detection and the electrochemical device.

[0057] (1) The BDD film 5 is used as the anode, and the working electrode of the electrochemical workstation is connected through the copper sheet 4 . The wafer of the present invention is placed in the supporting disc 7, on which an electrochemical cell 9 is installed, and the electrochemical cell and the BDD membrane are connected through a rubber ring 8 to prevent the solution in the reaction zone from flowing out. There are openings 3 and 10 on both sides of the electrochemical cell, and the central opening 1 is the main electrochemical reaction area. The opening 10 on one side is used to inject and absorb the solution, the opening 3 on the other s...

Embodiment 3

[0062] Prepare BDD loading wafer with the method of embodiment 1, obtain BDD film thickness 4.5 μm, boron doping amount is 1.8×10 19 boron atoms per cubic centimeter of BDD, and the BDD film resistivity is 10 -1 Ω·cm, surface roughness Rα is 120nm.

[0063] (1) The device diagram is as follows Figure 4 As shown, the BDD film 5 is used as a conductive carrier, and an electrode sheet coated with PAN / S (sulfur and polyacrylonitrile heat treatment product) is spread in the center as the positive electrode 12. One end of the stainless steel foil 13 is connected to the BDD film, and one section is connected to the electrochemical electrode. The workstation makes the positive electrode conductive. The upper surface of the positive electrode is covered with a thin film 15, which can effectively prevent the positive and negative electrodes from being short-circuited. The upper surface of the diaphragm covers the lithium electrode 14, which is also connected to the electrochemical w...

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Abstract

The invention belongs to the technical field of infrared spectroscopy, in particular to a boron-doped diamond modified attenuated total reflection wafer and a preparation method and application thereof. The attenuated total reflection wafer serves as a substrate, a boron-doped diamond thin film layer is arranged on the surface of the substrate, and the electrical resistivity of the boron-doped diamond thin film layer is 10<-3>-1 Ohm.cm; infrared light is incident into the inner surface of the attenuated total reflection wafer by a certain angle, the inner surface is adjacent to the boron-dopeddiamond thin film layer, the infrared light is refracted and reflected on the inner surface, the refracted light enters the boron-doped diamond thin film layer, and total reflection occurs in the boron-doped diamond thin film layer. The boron-doped diamond modified attenuated total reflection wafer enables infrared signal detection to be possible while achieving a good electricity conducting effect, in-situ electrochemical detection of molecules to be detected on the surfaces of BDD electrodes in the electrochemical process can be achieved, and wide application prospects are achieved in the in-situ infrared detection field.

Description

technical field [0001] The invention belongs to the technical field of infrared spectroscopy, and more specifically relates to a boron-doped diamond-modified attenuation total reflection wafer, its preparation and application. Background technique [0002] Various intermediate products are produced during the electrochemical catalytic oxidation or reduction process, and some intermediate products exist for a short time. Some conventional non-situ detection techniques such as high performance liquid chromatography (HPLC), gas chromatography (GC), etc. And the intermediate products were detected in situ, because some intermediate products did not exist before sampling and detection. Therefore, in situ detection is very important in this case. Infrared spectroscopy is an effective means to detect the information and mechanism analysis of functional groups of substances. [0003] Common infrared spectroscopy detection techniques include transmission mode and reflection mode. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/26G01N21/35C23C16/27
CPCC23C16/278G01N21/35G01N27/26
Inventor 胡敬平陈思静帕乌刘斯·波贝丁斯卡斯约翰·福德肯·哈嫩武龙胜侯慧杰刘冰川杨家宽
Owner HUAZHONG UNIV OF SCI & TECH
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