Preparation method of ultra-pure and ultrafine silver nanowire

A nanowire and ultra-fine silver technology, applied in the field of nanowire materials, can solve the problems that cannot meet the requirements of the display screen for transparent conductive films, the transparent conductive film has a large haze, and the purification effect is not good, so as to achieve the reduction of hydroxide radicals The effect of plasma concentration, low cost, and simple method

Inactive Publication Date: 2019-04-16
SHAANXI COAL & CHEM TECH INST +1
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Problems solved by technology

The diameter of ultrafine silver nanowires reported in the literature can reach about 20nm, but the common disadvantage is that the prepared silver nanowires contain a large number of particles, and the mass fraction of silver nanowires is only about 50%, resulting in the preparation of silver nanowires transparent The haze of the conductive film is very large, which cannot meet the requirements of the display screen for the transparent conductive film
Silver nanowires can be separated from the prepared product through purification techniques, but currently known purification techniques either involve toxic chemicals, or the process is complicated, or the purification effect is not good

Method used

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  • Preparation method of ultra-pure and ultrafine silver nanowire
  • Preparation method of ultra-pure and ultrafine silver nanowire

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preparation example Construction

[0026] The method for preparing ultra-pure and ultra-fine silver nanowires of the present invention removes moisture in ethylene glycol by heating, regulates the size of the initial crystal nucleus, and after 30min-180min of heat preservation, nanowires with a diameter of 15nm-25nm can be obtained. Ultra-pure and ultra-fine silver nanowires with a mass percentage of 75%-95%.

[0027] Specifically include the following steps:

[0028] (1) Preparation of sodium bromide in ethylene glycol solution: Weigh a certain amount of sodium bromide and dissolve it in ethylene glycol, stir and dissolve on a heating plate at 100°C-150°C for 1min-180min, and the concentration is 1mM- 1000mM;

[0029] (2) Preparation of ethylene glycol solution of sodium chloride: Weigh a certain amount of sodium chloride and dissolve it in ethylene glycol, stir and dissolve on a heating plate at 100°C-150°C for 1min-180min, and the concentration is 1mM- 1000mM;

[0030] (3) Preparation of PVP ethylene glyc...

Embodiment 1

[0034] (1) Preparation of sodium bromide in ethylene glycol solution: weigh 0.4572g of sodium bromide and dissolve in 20mL of ethylene glycol, stir and dissolve on a heating plate at 130°C for 2h;

[0035] (2) Preparation of ethylene glycol solution of sodium chloride: Weigh 0.2466g of sodium chloride and dissolve in 20mL of ethylene glycol, stir and dissolve on a heating plate at 130°C for 2 hours;

[0036] (3) Preparation of PVP ethylene glycol solution: weigh 1.68g of PVP with a molecular weight of 360,000, dissolve it in 30mL of ethylene glycol, and stir and dissolve it on a heating plate at 130°C for 5 minutes;

[0037] (4) Preparation of ethylene glycol solution of silver nitrate: Weigh 15mL of ethylene glycol, stir on a heating plate at 130°C for 2 hours, cool to room temperature in a drying oven, weigh 0.6765g of silver nitrate, dissolve it in In the above-mentioned ethylene glycol, sonicate for 5 minutes in an ice-water bath at a temperature of 5°C in an ultrasonic in...

Embodiment 2

[0040] On the basis of Example 1, just change step (5) to take 116mL of ethylene glycol and pour it into a 250mL round bottom flask, stir and heat at 130°C in an oil bath for 120min, then add step (1)- (4) For the prepared solution, the molar ratio of silver nitrate, sodium bromide, sodium chloride and PVP is 10:1:1:10, the temperature is raised to 180°C, and the temperature is lowered to 160°C after the temperature stabilizes , and keep it warm for 60 minutes to obtain ultra-pure and ultra-fine silver nanowires with a diameter of 24 nm and a mass percentage of 89%.

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Abstract

The invention provides a preparation method of an ultra-pure and ultrafine silver nanowire. The preparation method comprises the following steps: step 1, an ethylene glycol solution with sodium bromide, an ethylene glycol solution with sodium chloride, an ethylene glycol solution with PVP and an ethylene glycol solution with silver nitrate are prepared, and in the preparation process, moisture inethylene glycol is removed through heating; and step 2, the ethylene glycol is taken, heating is conducted to remove the moisture, the ethylene glycol solution with sodium bromide, the ethylene glycolsolution with sodium chloride, the ethylene glycol solution with PVP and the ethylene glycol solution with silver nitrate which are prepared in the step 1 are added, the temperature is increased to form a nucleus, temperature increasing is reduced, and the ultra-pure and ultrafine silver nanowire is prepared. According to the preparation method, the adsorbed moisture in the ethylene glycol is removed through heating, thus the concentration of hydroxyl plasma in a reaction solution is effectively decreased, seed crystal damage caused by ion etching is reduced, the dynamic process of nucleus forming is adjusted and controlled, the probability that the crystal nucleus grows into the nanowire is increased significantly, and the ultra-pure and ultrafine silver nanowire can be obtained withoutthe need of the subsequent purification process.

Description

technical field [0001] The invention belongs to the technical field of nanowire materials, and relates to a preparation method of ultrapure and ultrafine silver nanowires. Background technique [0002] With the rapid development of smart phones and flat panel display fields, the demand for flexible and bendable display screens is increasing, which puts forward higher requirements for transparent conductive film materials. Due to the poor bending resistance of indium tin oxide (ITO) transparent conductive films, silver nanowire transparent conductive films have become a hot material in the industry. At present, in order to meet the requirement of low haze, the diameter of silver nanowires is limited to less than 40nm. The diameter of ultrafine silver nanowires reported in the literature can reach about 20nm, but the common disadvantage is that the prepared silver nanowires contain a large number of particles, and the mass fraction of silver nanowires is only about 50%, resul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00B82Y40/00
CPCB82Y40/00B22F9/24B22F1/0547
Inventor 魏葳叶长辉张晓东黄林泉陈桂南雷国伟赵炎王贵欣陈微微闫国栋
Owner SHAANXI COAL & CHEM TECH INST
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