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Method for preparing amino functional multiporous silica-based composite material for ion detection

An amino-functionalized, porous silicon-based technology, applied in the analysis of materials, material analysis by electromagnetic means, and measurement devices, can solve the problems of complex pretreatment, high operating costs, and expensive costs, and achieve high sensitivity and selectivity. , Efficient surface modification, high surface activity effect

Inactive Publication Date: 2012-06-27
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The instruments required by these methods are usually expensive, high operating costs, skilled operating experience and sufficient work space are required, and it is time-consuming and laborious to achieve large-scale detection; and some methods require complex pre-processing during measurement. Need to extract, concentrate and enrich or suppress interference; some cannot perform multi-component or multi-element analysis; some cannot be determined due to interference of elements, spectra, etc.

Method used

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  • Method for preparing amino functional multiporous silica-based composite material for ion detection
  • Method for preparing amino functional multiporous silica-based composite material for ion detection

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A. The P-type silicon wafers with a resistivity of 0.01~0.09Ω·cm were ultrasonically cleaned with absolute ethanol and deionized water for 5 minutes, and then immersed in hydrofluoric acid with a mass concentration of 10% for 10 minutes, and then placed the silicon wafers Put the volume ratio of deionized water: absolute ethanol: 50% hydrofluoric acid with a mass concentration of 1:1:1 into the etching solution, and use the double cell or single cell electrochemical etching method to use the silicon wafer as the anode. Platinum sheet is used as the negative electrode, applying 40mA / cm 2 The corrosion current is 30 minutes, that is, the silicon wafer is corroded to obtain porous silicon with a nanometer pore size;

[0029] B. The porous silicon obtained in step A was ultrasonically cleaned with absolute ethanol and deionized water for 10 minutes, and then the surface of the porous silicon was thermally oxidized at 100°C for 1 hour to introduce silicon hydroxyl bonds (Si-OH...

Embodiment 2

[0032] A. The P-type silicon wafers with a resistivity of 0.01~0.09Ω·cm were ultrasonically cleaned with absolute ethanol and deionized water for 20 minutes, and then soaked in hydrofluoric acid with a mass concentration of 5% for 5 minutes, and then the silicon wafers were placed Put the volume ratio of deionized water: absolute ethanol: mass concentration of 5% hydrofluoric acid = 0.5: 5: 0.5 in the etching solution, using double cell or single cell electrochemical etching method to use silicon wafer as anode, Platinum sheet is used as the negative electrode, applying 5mA / cm 2 The corrosion current is 80 minutes, that is, the silicon wafer is corroded to obtain porous silicon with a nanometer pore size;

[0033] B. The porous silicon obtained in step A was ultrasonically cleaned with absolute ethanol and deionized water for 1 minute in turn, and then thermally oxidized at 50°C for 3 hours to introduce silicon hydroxyl bonds (Si-OH) on the surface, and then press The solid-to-...

Embodiment 3

[0036] A. The N-type silicon wafers with a resistivity of 0.01Ω·cm were ultrasonically cleaned with absolute ethanol and deionized water for 1 minute, then immersed in hydrofluoric acid with a mass concentration of 40% for 1 minute, and then put the silicon wafers into the volume The ratio is deionized water: absolute ethanol: 60% hydrofluoric acid with a mass concentration of 2:10:5 in an etching solution, using double cell or single cell electrochemical etching method to use silicon wafer as anode, platinum wafer As the negative electrode, apply 100mA / cm 2 The corrosion current is 5 minutes, that is, the silicon wafer is corroded to obtain porous silicon with a pore size of the order of microns;

[0037] B. The porous silicon obtained in step A was ultrasonically cleaned with absolute ethanol and deionized water for 30 minutes, and then the surface of the porous silicon was thermally oxidized at 200°C for 0.5h to introduce silicon hydroxyl bonds (Si-OH) on the surface, and the...

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Abstract

The invention provides a method for preparing an amino functional multiporous silica-based composite material for ion detection. The method comprises the following steps of: pretreating an N-type or P-type silicon slice, putting the silicon slice into an erosion solution, taking the silicon slice as a positive electrode and a platinum slice as a negative electrode by using a double-electrolytic-bath or single-electrolytic-bath electrochemical erosion method, and applying erosion current, namely eroding the silicon slice to obtain multiporous silicon; and then washing, performing thermal oxidization treatment on the surface of the multiporous silicon to introduce a silicon hydroxyl bond into the surface of the multiporous silicon, putting the multiporous silicon into a substance containing an amino ligand, stirring and performing amino functional treatment, and thus obtaining the amino functional multiporous silica-based composite material. The material has relatively high sensitivity and selectivity to trace silver ions and copper ions, and has extremely large specific surface area and high surface activity, so that the material is subjected to simple and high-efficiency surface modification. The method is simple, and is easy to operate; and the amino functional multiporous silica-based composite material can be obtained quickly.

Description

Technical field [0001] The invention relates to a preparation method of an amino-functionalized porous silicon-based composite material for ion detection, which uses an amino-modified porous silicon selective electrode to achieve selective detection of metal ions. Background technique [0002] At present, the methods used for the detection of trace heavy metals mainly include atomic absorption, atomic fluorescence, inductively coupled plasma and other spectral analysis methods, inductively coupled plasma mass spectrometry, and ultraviolet-visible light spectrophotometry. The instruments required for these methods are usually expensive and expensive to operate. They require skilled operation experience and sufficient working space. It is time-consuming and laborious to achieve large-scale detection; and some methods of measurement require complicated pre-processing. Need to extract, concentrate or suppress interference; some cannot perform multi-component or multi-element analysis...

Claims

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Application Information

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IPC IPC(8): G01N27/333
Inventor 马文会李绍元周阳魏奎先谢克强龙萍王飞伍继君徐宝强刘大春杨斌戴永年
Owner KUNMING UNIV OF SCI & TECH
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