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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 difficult promotion, easy agglomeration of active substances, poor conductivity, etc., and achieve the effects of improving the uniformity of deposition and dispersion, the fineness of metal particles, and the reduction of interfacial tension.

Active Publication Date: 2020-08-28
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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  • Preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode
  • Preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode
  • Preparation method of titanium oxide nanotube array-based photoelectrochemical detection electrode

Examples

Experimental program
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Effect test

Embodiment 1

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

[0035] (2) Prepare a 0.03M silver nitrate solution containing 0.05M nitric acid and 0.05M ethanolamine. Soak TNTA in 10ml silver nitrate solution for 10min, then wash off the excess solution on the surface of the sample piece with distilled water, put it into 10ml 0.1M NaOH solution and soak it for 10min, and finally soak the sample piece in distilled water for 5...

Embodiment 2

[0045] (1) Prepare an electrolyte solution with 0.1 g of ammonium fluoride, 7.5 g of distilled water and 42.5 g of ethylene glycol. The process steps are the same as in Example 1 (1), and anodic oxidation is 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 in Example 1(2), and co-deposit twice to prepare Ag-TNTA.

[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, and the deposition process was the same as in Example 1 (3), and a total of 10 depositions were performed.

[0048] Add 0.5g of hydrazine hydrate into 100ml of 0.5M NaOH solution, stir to dissolve, and prepare a reducing solution. The Ag-Cu / Ag-TNTA electrode can be prepared by carrying out the hydrothermal reduction reaction according to the process conditions of E...

Embodiment 3

[0050] (1) Prepare an electrolyte solution with 0.2 g of ammonium fluoride, 2.5 g of distilled water and 47.5 g of ethylene glycol. The process steps are the same as in Example 1 (1), and anodized at 45° C. and 35 V for 4 hours to prepare TNTA.

[0051] (2) A 0.01M silver nitrate solution containing 0.01M nitric acid and 0.01M ethanolamine was prepared, the process steps were the same as in Example 1(2), and Ag-TNTA was prepared by co-depositing 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. The deposition process is the same as in Example 1 (3), and the total deposition is 2 times.

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

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Abstract

The invention relates to a preparation method of a titanium oxide nanotube array-based photoelectrochemical detection electrode. According to the method, Ag-TNTA is firstly used for modifying TNTA toprepare Ag-TNTA, and then metal silver and copper are deposited into Ag-TNTA through chemical co-deposition and hydrothermal reduction to prepare the electrode. The photoelectrochemical detection electrode prepared by the invention can be used for detecting permanganate and dopamine, and the test process is simple, rapid and pollution-free.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a preparation method of a photoelectrochemical detection electrode. Background technique [0002] Because heavy metal elements are widely used 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 messenger of information in the brain, a chemical substance used to help cells transmit impulses, and regulate various physiological functions of the central nervous system. This brain secretion is related to human desire and feeling, and it conveys information of excitement and happiness. Additionally, dopamine has also been linked to various addictive behaviors. In manganese poisoning, levodopa decarboxylase is inhibited, and the process of decarboxylation of levodopa into dop...

Claims

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Application Information

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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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