Method for fixing noble metal nano particles on single-crystal silicon surface polymer brush

A nanoparticle and polymer brush technology, which is applied in the field of micro-nano material preparation, can solve the problems of uneven grafting, low graft density, difficulty in obtaining thick polymer brushes, etc., and achieve the effect of controllable fixation

Inactive Publication Date: 2012-10-10
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former chemically reacts the reactive groups on the polymer chains with the groups on the macroscopic surface to fix the polymer chains on the surface of the substrate, but its disadvantages are low grafting density and uneven grafting, making it difficult to obtain a layer with controllable thickness. polymer brush

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Place the monocrystalline silicon wafer in a 10vol% hydrofluoric acid solution for 2 minutes to remove the silicon dioxide oxide layer on the surface of the monocrystalline silicon wafer to obtain a hydrogenated silicon wafer A;

[0024] 2) Adding 4-vinylbenzyl chloride dropwise on the surface of silicon wafer A, irradiating with ultraviolet light for 3 minutes, washing with acetone, and drying to obtain silicon wafer B containing atom transfer radical polymerization initiator groups on the surface;

[0025] 3) Add silicon wafer B to 15mL of acetone containing 50mmol of butyl acrylate, remove oxygen, add 0.01mmol of copper bromide, 0.5mmol of cuprous bromide and 1mmol of bipyridine, and carry out surface-induced atom transfer radical polymerization. for 50 o C, the reaction time is 12 hours, obtain the silicon chip C that the surface contains polybutylacrylate brush;

[0026] 4) Place silicon wafer C in a dichloromethane solution containing 10vol% trifluoroacetic ac...

Embodiment 2

[0029] 1) Same as step 1 in Example 1;

[0030] 2) Same as step 2 of Example 1;

[0031] 3) Add silicon chip B into 12mL of tetrahydrofuran containing 40mmol of butyl acrylate, remove oxygen, add 0.01mmol of copper bromide, 0.5mmol of cuprous bromide and 1mmol of pentamethyldiethylenetriamine to carry out surface-induced atom transfer Free radical polymerization, the reaction temperature is 60 o C, the reaction time is 24 hours, obtain the silicon chip C that the surface contains polybutylacrylate brush;

[0032] 4) Place silicon wafer C in a dichloromethane solution containing 10vol% trifluoroacetic acid, the molar ratio of trifluoroacetic acid to butyl acrylate is 4:1, stir at room temperature for 24 hours, and obtain polyacrylic acid on the surface of single crystal silicon The polymer brush, the thickness of the polymer brush is 18nm;

[0033] 5) Soak the polymer brush obtained in the previous step in 0.006mol / L nickel chloride solution for 1 hour, take it out and react...

Embodiment 3

[0035] 1) Same as step 1 in Example 1;

[0036] 2) Same as step 2 of Example 1;

[0037] 3) Add silicon wafer B to 14mL of acetone containing 45mmol of butyl methacrylate, remove oxygen, add 0.0096mmol of cupric chloride, 0.48mmol of cuprous chloride and 0.96mmol of pentamethyldiethylenetriamine, and perform surface Initiate atom transfer radical polymerization, the reaction temperature is 60 o C, the reaction time is 36 hours, obtain the silicon chip C that the surface contains polybutylmethacrylate brush;

[0038] 4) Place silicon wafer C in a dichloromethane solution containing 10vol% trifluoroacetic acid, the molar ratio of trifluoroacetic acid to butyl methacrylate is 4:1, stir at room temperature for 36 hours, and obtain A polymer brush of polymethacrylic acid, the thickness of the polymer brush is 21nm;

[0039] 5) Soak the polymer brush obtained in the previous step in 0.005mol / L silver nitrate solution for 1 hour, take it out and react in 0.1mol / L sodium borohydrid...

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Abstract

The invention relates to a method for fixing noble metal nano particles on a single-crystal silicon surface polymer brush, which comprises the following steps: soaking a single-crystal silicon wafer in a hydrofluoric acid solution to obtain a silicon wafer A; dropwisely adding 4-vinylbenzyl chloride onto the surface, radiating, rinsing with acetone, drying, and adding into a monomer-containing solvent; adding copper bromide or copper chloride, cuprous bromide or cuprous chloride and ligand into the solvent to carry out surface-initiated atom transfer and free radical polymerization, thus obtaining a silicon wafer C; putting the silicon wafer C in a dichloromethane solution of trifluoroacetic acid, and stirring to obtain a carboxyl-containing polymer brush; and sufficiently soaking the polymer brush in a solution containing noble metal ions, then taking out, and finally reacting in a sodium borohydride solution, thus fixing the noble metal nano particles on the single-crystal silicon surface polymer brush. The invention achieves the following technical effects: the activity is controllable in the polymerization process, the graft polymerization density is high; the polymer chain isprevented from falling off the substrate; and the controllable fixation of the noble metal nano particles is effectively implemented.

Description

technical field [0001] The invention relates to a method for fixing noble metal nanoparticles on a polymer brush on the surface of single crystal silicon, and belongs to the technical field of preparation of micro-nano materials. Background technique [0002] Metal nanoparticles have unique properties due to quantum effects and extremely large specific surface areas. They have attractive application prospects in optoelectronic devices, sensors, catalysis, and medicine. Therefore, the structure of metal nanoparticles has become one of the core research contents of nanoscience. The most common problem in the preparation and application of metal nanoparticles is that they are very easy to agglomerate due to the high surface energy of the nanoparticles. To reduce or prevent aggregation, metal nanoparticles must be stably dispersed in solutions, matrices, macroscopic surfaces or interfaces. The study found that the composite material of polymer / metal nanoparticles not only ret...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/51
Inventor 李亮赵旭刘仿军郑华明陈郁勃高大志
Owner WUHAN INSTITUTE OF TECHNOLOGY
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