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Organic silicon nano particle modified electrode, sensor piece and preparation method of electrode

A technology of nanoparticles and modified electrodes, which is applied in the fields of organosilicon nanoparticles modified electrodes and sensor devices and its preparation, can solve the problems of large nanoparticle size distribution and difficulty in obtaining organosilicon nanoparticles, etc., and achieve high functional group content, The preparation method is simple and the selectivity is good

Inactive Publication Date: 2013-08-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using MPTS as a single silicon source, using NH 4 OH catalyzed hydrolysis reaction to obtain pure silicone nanoparticles of 0.2-3 μm, but the size distribution of nanoparticles is relatively large, and it is difficult to obtain very fine silicone nanoparticles [J.Phys.Chem.C, 2007, 111(51) :18892, Langmuir, 2011, 27(7):3372]

Method used

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  • Organic silicon nano particle modified electrode, sensor piece and preparation method of electrode
  • Organic silicon nano particle modified electrode, sensor piece and preparation method of electrode
  • Organic silicon nano particle modified electrode, sensor piece and preparation method of electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Mix 40 μL ultrapure water with 32 μL 0.1mol / L hydrochloric acid, then slowly add 188 μL 3-mercaptopropyltrimethoxysilane to fully hydrolyze it, and finally add 3-mercaptopropyltrimethoxysilane with a volume ratio of 1:2.5 Dilute with ethanol, stir at room temperature for 30 minutes to form a uniform and transparent solution; weigh 0.0133g of hexadecyltrimethylammonium bromide (1:100 molar ratio to 3-mercaptopropyltrimethoxysilane) and dissolve in 1.00 mL of ethanol was then added to the above solution, and the stirring was continued for 30 min to obtain 3-mercaptopropyltrimethoxysilane sol.

[0057] At room temperature, the cleaned gold electrode was immersed in the freshly prepared sol, self-assembled for 1 hour, removed and stabilized for 10 minutes, rinsed with ethanol, and blown dry with nitrogen. That is, the organosilicon nano film modified electrode is obtained.

[0058] Take out and stabilize for 1min, rinse with ethanol and ultrapure water in turn, and blow dr...

Embodiment 2

[0061] Immerse the cleaned gold electrode into the functionalized silicone gel in Example 1 at room temperature, self-assemble for 6 hours, take it out and stabilize it for 10 minutes, rinse with ethanol, and blow dry with nitrogen. That is, the organosilicon nano film modified electrode is obtained.

[0062] Take out and stabilize for 3 minutes, rinse with ethanol and ultrapure water in turn, and dry with inert gas; then extract in a mixture of 0.2mol / L hydrochloric acid and 99.7% ethanol by mass fraction, and the volume ratio of hydrochloric acid and ethanol is 1:1 The surfactant was removed, the extraction time was 1 h, the water was rinsed, and the nitrogen gas was blown to dry, and the mercapto-functionalized organosilicon nanoparticle-modified gold electrode was prepared.

[0063] The above-mentioned modified electrode is used as the working electrode, the platinum wire is used as the auxiliary electrode, and Ag / AgCl is used as the reference electrode, and the compositio...

Embodiment 3

[0065] Mix 160 μL ultrapure water and 128 μL 0.1mol / L hydrochloric acid, then slowly add 212 μL 3-aminopropyltrimethoxysilane to fully hydrolyze it, and finally add 3-aminopropyltrimethoxysilane with a volume ratio of 1:5 Dilute with ethanol, stir at room temperature for 1h to form a uniform and transparent solution, weigh 0.0488g (1:50 molar ratio to 3-aminopropyltrimethoxysilane) sodium dodecylbenzenesulfonate and dissolve in 1.00mL ethanol , and then added to the above solution, and continued to stir for 1h to obtain 3-aminopropyltrimethoxysilane sol.

[0066] The surface-cleaned indium tin oxide electrode was immersed in the freshly prepared sol, self-assembled for 10 hours, taken out and left for 5 minutes, rinsed with ethanol, and blown dry with nitrogen. Then extract 30min in 0.05mol / L hydrochloric acid and 95% ethanol with a mass fraction of hydrochloric acid and ethanol in a volume ratio of 1:1, rinse with ultrapure water, and dry with nitrogen to obtain amino-functio...

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Abstract

The invention relates to an organic silicon nano particle modified electrode, a sensor piece and a preparation method of the electrode. The organic silicon nano particle modified electrode is an organic silicon nano particle electrode, wherein organic silicon nano particles are subjected to surface finish sulfydryl or amino functionalization. The organic silicon nano particle modified electrode is characterized in that a silane material containing an organo-functional group is utilized as a silicon source, and uniform superfine organic silicon nano particles are obtained with the existence of a surface active agent with a proper quantity under room temperature; and further, a uniform compact organic silicon nano particle film is formed on the surface of the electrode through using a normal position assembly or condensed method, and therefore, the organic silicon nano particle modified electrode with different functions is obtained. The invention also discloses the sensor piece assembled by adopting the modified electrode, and the sensor piece is used for detecting trace heavy metal. The organic silicon with the single function is adopted as the silicon source in the preparation, and therefore, the functional groups on a nano surface are rich; and as the nano particles are utilized as a sensing interface, the sensitivity response of analytes such as the trace heavy metal (Pb, Hg, Cu and the like) in the sensor is greatly improved.

Description

technical field [0001] The invention relates to an organosilicon nano particle modified electrode, a sensing device and a preparation method thereof. Background technique [0002] Chemically modified electrodes are the frontier research fields of electrochemistry and electroanalytical chemistry in recent years, and have been widely used in many fields such as biology, environment, energy, analysis and materials science. Due to the characteristics of high specific surface area, adjustable pore size (2-30nm) and easy surface functionalization, mesoporous silica has broad application prospects in the fields of catalysis, adsorption, and sensing. Most of the current research uses inorganic-organic hybrid dual-silicon sources to obtain functionalized ordered mesoporous membranes as electrochemical sensing layers, such as Walcarius et al. Mercaptopropyltrimethoxysilane (MPTS) blend prepared mesoporous mesoporous silicon oxide film-modified carbon paste electrode containing mercap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30
Inventor 刘建允吴中玮肖健林杨健茂张鑫周鑫
Owner DONGHUA UNIV
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