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Large-scale preparation and purification method for superfine silver nanowires

A purification method and nanowire technology, which is applied in the field of large-scale preparation and purification of ultra-fine silver nanowires, can solve the problems of high surface tension of aqueous dispersions, inability to alleviate blocking problems, and affect film-forming performance.

Active Publication Date: 2021-05-18
珠海纳金科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, positive pressure filtration will lead to agglomeration of silver nanowires, making it difficult to disperse again, which will affect its film-forming effect and performance after film-forming
The invention patent (publication number CN201610538533.4) discloses a separation method in which ethyl acetate is added to the ethanol dispersion of silver nanowires with a diameter of 20nm to make the silver nanowires agglomerate, and then settle down. This method also needs to repeat the sedimentation many times To purify, it needs to consume a lot of ethanol, ethyl acetate and time
In this method, the aqueous dispersion of silver nanowires has a high surface tension, and its filter membrane is particularly prone to clogging, resulting in low purification efficiency.
Validation experiments show that paddles do not alleviate clogging problems

Method used

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  • Large-scale preparation and purification method for superfine silver nanowires
  • Large-scale preparation and purification method for superfine silver nanowires
  • Large-scale preparation and purification method for superfine silver nanowires

Examples

Experimental program
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Effect test

Embodiment 1

[0050] A method for large-scale preparation and purification of ultrafine silver nanowires, comprising the following steps:

[0051] Step 1. Mix 285mL of ethylene glycol and 150mL of diethylene glycol, add 15g of polyvinylpyrrolidone with an average molecular weight of 1300000, stir at 1200r / min for 60min to dissolve, then add 2.8g of silver nitrate, stir at 1200r / min for 60min to dissolve the silver nitrate, Then add 50mL of 1.17mM tetrabutylammonium chloride, 100mL of 1.17mM tetrabutylammonium bromide, continue stirring at 1200r / min for 45min, add 1.5mL of 0.017M ferric trichloride hexahydrate to obtain a reaction solution, and the reaction solution Pour into the polytetrafluoroethylene liner, put the polytetrafluoroethylene liner into the reaction kettle, heat to 160 ° C for 180 minutes of reaction, and naturally cool to room temperature after the reaction to obtain the ultrafine silver nanowire mother liquor;

[0052] Step 2, diluting the ultrafine silver nanowire mother s...

Embodiment 2

[0063] A method for preparing ultrafine silver nanowires, comprising the following steps:

[0064]Step 1. Mix 285mL of ethylene glycol and 150mL of diethylene glycol, add 15g of polyvinylpyrrolidone with an average molecular weight of 1300000, stir at 1200r / min for 60min to dissolve, then add 2.8g of silver nitrate, stir at 1200r / min for 60min to dissolve the silver nitrate, Then add 40mL of 1.17mM tetrabutylammonium chloride and 80mL of 1.17mM tetrabutylammonium bromide, continue to stir at 1200r / min for 45min, add 1.5mL of 0.017M ferric trichloride hexahydrate to obtain a reaction solution, and the reaction solution Pour into the polytetrafluoroethylene liner, put the polytetrafluoroethylene liner into the reaction kettle, heat to 160 ° C for 180 minutes of reaction, and naturally cool to room temperature after the reaction to obtain the ultrafine silver nanowire mother liquor;

[0065] Step 2, diluting the ultrafine silver nanowire mother solution to 1 time to obtain a dilu...

Embodiment 3

[0076] A method for preparing ultrafine silver nanowires, comprising the following steps:

[0077] Step 1. Mix 285mL of ethylene glycol and 150mL of diethylene glycol, add 15g of polyvinylpyrrolidone with an average molecular weight of 1300000, stir at 1200r / min for 60min to dissolve, then add 2.8g of silver nitrate, stir at 1200r / min for 60min to dissolve the silver nitrate, Then add 40mL of 1.17mM tetrabutylammonium chloride and 80mL of 1.17mM tetrabutylammonium bromide, continue to stir at 1200r / min for 45min, then subject the mixture to ultrasonic treatment under pressure for 15min, and then add 1.5 mL0.017M ferric trichloride hexahydrate to obtain the reaction solution, pour the reaction solution into the polytetrafluoroethylene lining, put the polytetrafluoroethylene lining into the reaction kettle, heat to 160°C for 180min, after the reaction Naturally cool to room temperature to obtain ultra-fine silver nanowire mother liquor; pressurized ultrasonic treatment condition...

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Abstract

The invention discloses a large-scale preparation and purification method for superfine silver nanowires. The large-scale preparation and purification method comprises the following steps of mixing ethylene glycol with diethylene glycol, adding polyvinylpyrrolidone, carrying out stirring for dissolving, then adding silver nitrate, carrying out stirring for dissolving the silver nitrate, then adding an ethylene glycol solution of tetrabutylammonium chloride and tetrabutylammonium bromide, carrying out stirring, adding ferric trichloride hexahydrate, after carrying out heating for reaction, carrying out natural cooling to room temperature to obtain superfine silver nanowire mother liquor; and diluting the superfine silver nanowire mother liquor, adding the diluted superfine silver nanowire mother liquor into a filtering device, and carrying out separation and purification to obtain the extremely pure superfine silver nanowires. According to the preparation method for the superfine silver nanowires, the prepared silver nanowires are narrower in diameter range and large in length-diameter ratio; and the preparation method does not need inert gases, expensive reagents and toxic reagents, and is low in preparation cost, simple to operate, suitable for industrial production, simple in post-treatment and low in treatment cost.

Description

technical field [0001] The invention relates to the technical field of preparation of one-dimensional nanomaterials, in particular to a large-scale preparation and purification method of ultrafine silver nanowires. Background technique [0002] Indium tin oxide (ITO) transparent conductive electrodes are widely used in photovoltaic industry, touch screen display, surface-enhanced Raman spectroscopy, organic light-emitting diodes and other fields. In recent years, due to the strong market demand for flexible electronic devices, flexible transparent conductive electrodes have received more and more attention. ITO cannot be used in flexible devices due to its inherent brittleness. In addition, the scarcity of raw materials and complicated preparation process lead to high cost of ITO. Silver nanowires have high electrical conductivity, light transmittance, flexibility, good stability and low cost. At the same time, the production process is simple and the yield rate is high. ...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/00B82Y40/00B01D29/56B01D29/60B01D29/86
CPCB22F9/24B82Y40/00B01D29/56B01D29/603B01D29/86B22F1/147B22F1/145Y02P10/20
Inventor 陈百利丁轶雷震
Owner 珠海纳金科技有限公司
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