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A preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode

A titanium oxide nanotube and photoelectrochemical technology, applied in the field of analysis and detection, can solve the problems of easy agglomeration of active substances, poor conductivity, and high detection cost, and achieve the effects of reducing interfacial tension, fine metal particles, and increasing the number of hydroxyl groups.

Active Publication Date: 2022-06-07
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many methods for detecting heavy metal ions. Instrumental analysis methods such as atomic absorption spectroscopy, mass spectrometry, fluorescence spectroscopy, and Raman spectroscopy require expensive, bulky, and complicated instruments. The detection cost is relatively high, and there are many steps, which take a long time and are not easy to popularize; chemical analysis methods Need to use many chemical reagents, in addition to many steps and long time-consuming, there is also the problem of secondary pollution; the electrochemical analysis method is based on the amount of the measured substance in the solution and certain electrical parameters (such as resistance, conductance, potential, There is a certain relationship between current, electricity, etc.), which has the characteristics of simple operation, low cost, fast detection speed, easy miniaturization and automation
However, there is no report on a photoelectrochemical electrode that can be used for both permanganate detection and dopamine detection.
In addition, there are some disadvantages and deficiencies in the photoelectrochemical sensors reported in the literature, for example, the photoelectrochemical sensors containing enzymes are usually less stable, and the photoelectrochemical sensors prepared by the coating method are prone to agglomeration of active substances, difficult to control the dosage, poor conductivity, etc. question

Method used

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  • A preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode
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  • A preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Ultrasonic cleaning of the Ti sheet (10 mm×20 mm×0.3 mm) with ethanol and distilled water to remove oil stains on the surface of the Ti sheet. Use 0.15g ammonium fluoride, 5g distilled water and 45g ethylene glycol to prepare a mixed solution, insert 10mm of the lower end of the Ti sheet into the mixed solution, the Ti sheet is the anode, and the Pt sheet is used as the cathode. Anodized for 3 hours under the conditions, a titanium dioxide nanotube array film (marked as TNTA) was formed on the surface of the metal titanium sheet; after the reaction, the sample was washed with distilled water and dried.

[0035] (2) A 0.03M silver nitrate solution containing 0.05M nitric acid and 0.05M ethanolamine was prepared. The TNTA was first soaked in 10ml silver nitrate solution for 10min, then the excess solution on the surface of the sample was washed with distilled water, and then soaked in 10ml 0.1M NaOH solution for 10min, and finally the sample was soaked in distilled wa...

Embodiment 2

[0045] (1) An electrolyte was prepared with 0.1 g of ammonium fluoride, 7.5 g of distilled water and 42.5 g of ethylene glycol. The process steps were the same as those in Example 1 (1), and anodic oxidation was carried out at 35° C. and 45 V for 2 hours to prepare TNTA.

[0046] (2) Prepare a 0.05M silver nitrate solution containing 0.1M nitric acid and 0.1M ethanolamine, the process steps are the same as those in Example 1(2), and Ag-TNTA is prepared by co-deposition twice.

[0047] (3) A copper-silver ion mixed solution containing 0.01M nitric acid, 0.01M ethanolamine, 0.005M silver nitrate and 0.045M copper nitrate was prepared.

[0048] Add 0.5 g of hydrazine hydrate to 100 ml of 0.5 M NaOH solution, stir to dissolve, and prepare a reducing solution. The Ag-Cu / Ag-TNTA electrode can be obtained by performing the hydrothermal reduction reaction according to the process conditions of Example 1(3).

Embodiment 3

[0050] (1) An electrolyte was prepared with 0.2 g of ammonium fluoride, 2.5 g of distilled water and 47.5 g of ethylene glycol. The process steps were the same as those in Example 1 (1), and anodic oxidation was carried out at 45° C. and 35 V for 4 hours to prepare TNTA.

[0051] (2) Prepare a 0.01M silver nitrate solution containing 0.01M nitric acid and 0.01M ethanolamine, the process steps are the same as those in Example 1(2), and Ag-TNTA is prepared by co-deposition 9 times.

[0052] (3) Prepare a copper-silver ion mixed solution containing 0.1M nitric acid, 0.1M ethanolamine, 0.09M silver nitrate and 0.01M copper nitrate.

[0053] Add 0.1 g of formaldehyde to 100 ml of 0.1 M NaOH solution, stir to dissolve, and prepare a reducing solution. The Ag-Cu / Ag-TNTA electrode can be obtained by performing the hydrothermal reduction reaction according to the process conditions of Example 1(3).

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Abstract

The invention relates to a method for preparing a titanium oxide nanotube array-based photoelectrochemical detection electrode. In this method, Ag-TNTA is first prepared by modifying TNTA with Ag, and then metal silver and copper are deposited into Ag-TNTA by chemical co-deposition and hydrothermal reduction to prepare electrodes. The photoelectrochemical detection electrode prepared by the invention can be used not only for the detection of permanganate, but also for the detection of dopamine, and the testing process is simple, fast and pollution-free.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and particularly relates to a preparation method of a photoelectrochemical detection electrode. Background technique [0002] Due to the wide application of heavy metal elements in many fields, a large number of heavy metal ions enter the water body, causing heavy metal ion pollution, which will cause serious harm to human health, animals and plants. For example, dopamine, a catecholamine neurotransmitter, is a transmitter of information in the brain, a chemical used to help cells transmit impulses and regulate various physiological functions of the central nervous system. This brain secretion is related to human lust and feeling, and it conveys the information of excitement and happiness. In addition, dopamine is also associated with various addictive behaviors. When manganese poisoning occurs, levodopa decarboxylase is inhibited, the decarboxylation of levodopa into dopamine an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30C25D11/26C23C18/12C23C18/44B82Y40/00B82Y15/00
CPCG01N27/305C25D11/26C23C18/1204C23C18/1295C23C18/1245C23C18/44B82Y40/00B82Y15/00
Inventor 赵建玲吴志刚王西新刘东鑫朱淼
Owner HEBEI UNIV OF TECH
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