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Method for large-batch synthesizing and high-efficiency purifying of superfine silver nano wires

An ultra-fine silver, high-volume technology, applied in nanotechnology and other directions, can solve the problems of difficult to guarantee product quality, difficult process control, and many impurities in nanoparticles, and achieve the effect of stable preparation

Inactive Publication Date: 2019-03-19
TAIZHOU BRANCH ZHEJIANG-CALIFORNIA INT NANOSYSTEMS INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the following problems will occur in the synthesis process of ultrafine AgNWs (diameter ≤ 40nm), such as: 1) There are too many impurities in nanoparticles, and the diameter of nanoparticles is generally between 100-1000nm, which will cause great difficulties in the purification of AgNWs; 2) ) When a small amount of AgNWs is synthesized, the process is easy to control and the product quality is relatively stable, but once scaled up, since the synthesis of AgNWs is a complex thermodynamic and kinetic process, the process is difficult to control and the product quality is difficult to guarantee

Method used

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  • Method for large-batch synthesizing and high-efficiency purifying of superfine silver nano wires
  • Method for large-batch synthesizing and high-efficiency purifying of superfine silver nano wires

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for large-scale synthesis and efficient purification of ultrafine AgNWs, comprising the following steps:

[0030] (1) prepare the ethylene glycol (EG) solution of NaCl, NaBr, concentration is respectively 210mM ​​and 220mM;

[0031] (2) Add 3.6L (4.02kg) EG into the three-necked flask, and put in 24.0g PVP (molecular weight 1300000) and 16.2g AgNO 3 , after mixing and dissolving, add 72ml NaCl solution and 48ml NaBr solution, pass N 2 , after heating up to 165°C, stop stirring, N 2 Continue to react in the atmosphere for 1.0h, then cool naturally to room temperature, add deionized water to the reaction solution, reduce the viscosity of the reaction solution to 6cP;

[0032] (3) Transfer the reaction solution to a centrifuge bottle, and centrifuge at 800rpm for 20min. After removing the sediment, the supernatant continues to centrifuge at 800rpm for 20min, and remove the sediment again;

[0033] (4) After repeating step (3) 6 times, completely remove the larg...

Embodiment 2

[0037] A method for large-scale synthesis and efficient purification of ultrafine AgNWs, comprising the following steps:

[0038] (1) prepare the ethylene glycol (EG) solution of KCl, KBr, concentration is respectively 200mM and 200mM;

[0039] (2) Add 3.6L (4.02kg) EG to the three-necked flask, and put in 24.0g PVP (molecular weight 1300000) and 16.2g AgNO 3 , after mixing and dissolving, add 80ml NaCl solution and 36ml NaBr solution, pass N 2 , after heating up to 165°C, stop stirring, N 2 Continue to react in the atmosphere for 1.5h, then naturally cool to room temperature, add deionized water to the reaction solution, reduce the viscosity of the reaction solution to 10cP;

[0040] (3) Transfer the reaction solution to a centrifuge bottle, and centrifuge at 1200rpm for 15min. After removing the sediment, continue the centrifugation of the supernatant at 1200rpm for 20min, and remove the sediment again;

[0041] (4) After repeating step (3) 7 times, completely remove the ...

Embodiment 3

[0045] A method for large-scale synthesis and efficient purification of ultrafine AgNWs, comprising the following steps:

[0046] (1) Preparation of CaCl 2 , MgBr 2 The ethylene glycol (EG) solution of concentration is respectively 100mM and 300mM;

[0047] (2) Add 3.6L (4.02kg) EG to the three-necked flask, and put in 10.05g PVP (molecular weight 360000) and 10.05g AgNO 3 , after mixing and dissolving, add 180ml KCl solution and 20ml KBr solution, pass N 2 , after heating up to 160°C, stop stirring, N 2 Continue to react in the atmosphere for 3.0h, then cool naturally to room temperature, add deionized water to the reaction solution, reduce the viscosity of the reaction solution to 20cP;

[0048] (3) Transfer the reaction solution to a centrifuge bottle, and centrifuge at 1100rpm for 30min. After removing the sediment, the supernatant continues to centrifuge at 1200rpm for 30min, and remove the sediment again;

[0049] (4) After repeating step (3) 5 times, completely rem...

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Abstract

The invention relates to the field of nano material synthesizing and application and aims at providing a method for large-batch synthesizing and high-efficiency purifying of superfine silver nano wires. The method includes the steps that polyvinylpyrrolidone and AgNO3 are added into glycol under the stirring condition and are evenly mixed and dissolved; a chloridion halogeno salt-ethylene glycol solution and a bromide ion halogeno salt-ethylene glycol solution are added continuously, and a reaction is carried out in the N2 atmosphere; supernatant liquor is taken centrifugally, acetone is addedunder the stirring condition, and standing is conducted so that flocculent solids can be deposited; ionized water is used for dispersing, and a uniform dispersion solution is formed; and acetone is added under the stirring condition, and the adding action is stopped when flocculent solids occur again, the operation is repeated for 6 times to 10 times, and the high-purity superfine silver nano wires are obtained. By means of the method, the processes of Ag crystal nucleus forming, crystal growth and the like can be controlled, and large-batch and stable preparing of the superfine AgNWs is achieved. Large-particle-size nano particle impurities are removed completely, and small-particle-size nano particles are separated from the AgNWs; the prepared silver nano wires do not have silver nano particle impurities, and the purity is nearly 100%; and the diameter of the silver nano wires is smaller than or equal to 40.0 nm.

Description

technical field [0001] The invention relates to a method for large-scale synthesis and high-efficiency purification of ultrafine silver nanowires, which belongs to the field of synthesis and application of nanomaterials. Background technique [0002] The 21st century is an era of informatization and networking, and the "information superhighway" has penetrated into all aspects of social life. With the gradual advancement of information terminals from mainframes to wearable devices, from flat and curved to bendable and rollable, electronic devices are facing the challenge of flexibility. Flexible electronic devices, such as flexible displays, electronic skins, printed electronic labels, and flexible thin-film solar cells, have the characteristics of deformability, portability, light weight, and large-scale application, and have broad application prospects in information, energy, medical, national defense, and other fields. . The development of flexible electronics is insepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B82Y40/00
CPCB22F9/24B22F2009/245B82Y40/00
Inventor 汪海风白盛池陈天锐杨辉吴春春郭兴忠阙永生
Owner TAIZHOU BRANCH ZHEJIANG-CALIFORNIA INT NANOSYSTEMS INST
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