CN105081348B - A kind of normal pressure one kettle way prepares the method without particle high-purity silver nano wire - Google Patents
A kind of normal pressure one kettle way prepares the method without particle high-purity silver nano wire Download PDFInfo
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- CN105081348B CN105081348B CN201510645524.0A CN201510645524A CN105081348B CN 105081348 B CN105081348 B CN 105081348B CN 201510645524 A CN201510645524 A CN 201510645524A CN 105081348 B CN105081348 B CN 105081348B
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Abstract
The nano silver wire method without particle high-purity is prepared the invention provides a kind of normal pressure one kettle way.First silver nitrate is dissolved in polyhydric alcohol solutions, then by polyvinylpyrrolidone（PVP）It is dissolved in polyhydric alcohol solutions, finally both the above mixed solution is transferred in the three-necked flask of the circulating condensing pipe equipped with lower temperature medium, 150 DEG C are heated to after stirring, stir and be incubated, when having metallic luster on liquid level in three-necked flask, 0.2 ~ 0.5h is incubated, terminates experiment, the mixed solution containing nano silver wire is obtained.After three-necked flask natural cooling, the centrifuge washing again of the mixed solution containing nano silver wire is diluted with alcohol, no particle high-purity silver nano wire is finally obtained.Next pot of method of the method preparation without particle high-purity silver nano wire of normal pressure of the present invention is simple to operate, and equipment cost is cheap, and preparation time is short, and nano silver wire purity is high, and without particle.
Description
Technical field
The present invention relates to metal silver nano material, particularly a kind of next pot of method of normal pressure prepares the Yin Na without particle high-purity
The method of rice noodles.
Background technology
Nano silver wire has high surface area, electric conductivity, the good characteristic such as thermal conductivity and nanocomposite optical property, therefore mainly should
For transparent conductive film, solar cell, precise electronic, medical domain etc..At present, the preferable application prospect of nano silver wire it
One is flexible transparent conductive film, and the ideal material for substituting ITO is found as scientific circles.The performance master of flexible transparent conductive film
If being embodied in electric conductivity, the transparency and electric conductivity and transparent change after bending for several times, and the embodiment master of these performances
Will by nano silver wire draw ratio（Length and diameter）With the influence of Argent grain.In order to improve nano silver wire transparent conductive film
Performance, prepare high length-diameter ratio and agranular nano silver wire be particularly important.Although relevant report prepared by nano silver wire has
Many, but production operation is simple, it is less to be adapted to the process of the agranular nano silver wire of large-scale industrial production high-purity.
The content of the invention
It is inexpensive high-purity without particle with the quick preparation of one kettle way at ambient pressure it is an object of the present invention to provide one kind is simple to operate
The method of the nano silver wire of degree, raising prepares the stability of nano silver wire, is adapted to large-scale industrial production nano silver wire.
Technical scheme is as follows：
The method that the hot method of alcohol that the present invention is provided prepares nano silver wire at ambient pressure, comprises the following steps：
（1）Silver nitrate is dissolved in polyhydric alcohol solutions；
（2）Then by polyvinylpyrrolidone（PVP）It is dissolved in polyhydric alcohol solutions；
（3）Finally by above solution（1）With（2）It is transferred to three mouthfuls of burnings of the circulating condensing pipe of the medium equipped with lower temperature
In bottle, 150 DEG C are heated to after stirring, stirs and is incubated, when having metallic luster on liquid level, be incubated 0.2 ~ 0.5h, knot
Beam is tested, and obtains the mixed solution containing nano silver wire.After three-necked flask natural cooling, the mixing containing nano silver wire is diluted with alcohol
Solution centrifuge washing again, finally obtains the nano silver wire of no particle high-purity.
Compared with prior art, all reagents are added at room temperature, at a normal, is mixed to get reaction mother liquor, enhance work
The stability of skill, simple to operate, equipment cost is low, and improves the draw ratio of nano silver wire, it is adaptable to mass produce.
Brief description of the drawings
Fig. 1 is the SEM that the embodiment of the present invention 1 prepares nano silver wire（SEM）Photo.
Fig. 2 is the SEM that the embodiment of the present invention 3 prepares nano silver wire（SEM）Photo.
Embodiment
Embodiment 1
By 20ml, 0.08M silver nitrates/ethylene glycol solution, 80ml, 0.1M polyvinylpyrrolidones（PVP）/ ethylene glycol is molten
Liquid is transferred in the three-necked flask of the circulating condensing pipe equipped with 5 DEG C of alcoholic medias, 150 DEG C is heated to after stirring, stirring is simultaneously
When having metallic luster on insulation, liquid level, 0.5h is incubated, terminates experiment, the mixed solution containing nano silver wire is obtained.
The mixed solution of reacted nano silver wire is cooled to room temperature, alcohol dilution is added and centrifuges, then remove
Upper solution, adds alcohol dilution precipitation, then centrifuge washing, obtains nano silver wire, 30 ~ 50nm of diameter, long 10 ~ 30mm.Fig. 1
SEM of the high-purity without particle nano silver wire prepared for this implementation（SEM）Photo.
Embodiment 2
By 40ml, 0.15M silver nitrates/ethylene glycol solution, 160ml, 0.15M polyvinylpyrrolidones（PVP）/ ethylene glycol
Solution is transferred in the three-necked flask of the circulating condensing pipe equipped with 5 DEG C of alcoholic medias, and 150 DEG C, stirring are heated to after stirring
And be incubated, when having metallic luster on liquid level, 0.5h is incubated, terminates experiment, the mixed solution containing nano silver wire is obtained.
The mixed solution of reacted nano silver wire is cooled to room temperature, alcohol dilution is added and centrifuges, then remove
Upper solution, adds alcohol dilution precipitation, then centrifuge washing, obtains nano silver wire, 30 ~ 50nm of diameter, long 10 ~ 30mm.
Embodiment 3
By 20ml, 0.08M silver nitrates/glycerin solution, 80ml, 0.1M polyvinylpyrrolidones（PVP）/ glycerine is molten
Liquid is transferred in the three-necked flask of the circulating condensing pipe equipped with 5 DEG C of alcoholic medias, 150 DEG C is heated to after stirring, stirring is simultaneously
When having metallic luster on insulation, liquid level, 0.5h is incubated, terminates experiment, the mixed solution containing nano silver wire is obtained.Due to third
Triol is heated to after more than 100 DEG C to generate after yellow polymer, glycerine generation polymer in atmosphere, as reducing agent and
The amount of solvent is just reduced, so there is Argent grain in last testing result nano silver wire, thus glycerine as reducing agent not
It is easy to heat preparation high-purity in atmosphere without particle nano silver wire.
The mixed solution of reacted nano silver wire is cooled to room temperature, alcohol dilution is added and centrifuges, then remove
Upper solution, adds alcohol dilution precipitation, then centrifuge washing, obtains nano silver wire, 30 ~ 50nm of diameter, long 10 ~ 30mm.Fig. 2
The SEM of the nano silver wire prepared for this implementation（SEM）Photo.
Claims (2)
1. a kind of method that normal pressure one kettle way prepares the nano silver wire without particle high-purity, it is characterised in that methods described includes
Following specific steps：
（1）Silver nitrate is dissolved in ethylene glycol solution；
（2）Then by polyvinylpyrrolidone（PVP）It is dissolved in ethylene glycol solution；
（3）Finally by above solution（1）With（2）It is transferred to the circulating condensing pipe as circulating condensing liquid medium equipped with 5 DEG C of alcohol
Three-necked flask in, 150 DEG C are heated to after stirring, stirs and is incubated, when having metallic luster on liquid level, insulation 0.2 ~
0.5h, obtains the mixed solution containing nano silver wire；After three-necked flask natural cooling, the mixing containing nano silver wire is diluted with alcohol molten
Liquid centrifuge washing again, then removes upper solution, adds alcohol dilution precipitation, then centrifuge washing, finally obtains no particle high
The nano silver wire of purity.
2. preparing the method for the nano silver wire without particle high-purity according to a kind of normal pressure one kettle way described in claim 1, it is special
Levy and be：Whole experiment process keeps normal pressure and stirring.
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| CN105081348B true CN105081348B (en) | 2017-08-08 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105081351B (en) * | 2015-10-09 | 2017-09-26 | 重庆文理学院 | A kind of preparation method of uniform high length-diameter ratio nano silver wire |
| CN105537615B (en) * | 2015-12-24 | 2018-10-30 | 河南大学 | The method that one kettle way prepares different-diameter nano silver wire |
| CN105810364A (en) * | 2016-05-12 | 2016-07-27 | 南京工业大学 | Processing method for silver nanowire conductive thin film |
| CN106226376B (en) * | 2016-10-09 | 2019-07-05 | 南京膜材料产业技术研究院有限公司 | A kind of preparation method of the nano pulp for electrode print |
| CN107999742B (en) * | 2017-11-23 | 2019-10-18 | 华南理工大学 | A kind of preparation method of silver nanowires micro-patterning |
| CN112605380A (en) * | 2020-11-30 | 2021-04-06 | 哈尔滨工业大学 | Filtering and purifying method of silver nanowires |
| CN115555574B (en) * | 2022-03-07 | 2023-10-31 | 盐城工学院 | Method for preparing silver nanowire with high length-diameter ratio at low temperature |
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| CN103762011A (en) * | 2014-01-16 | 2014-04-30 | 中国科学院青岛生物能源与过程研究所 | Transparent conducting thin film based on sodium alga acid and preparation method of transparent conducting thin film |
| CN104785794A (en) * | 2015-05-12 | 2015-07-22 | 重庆文理学院 | Making method for silver nanowire even in length-diameter ratio |
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| KR20110071526A (en) * | 2009-12-21 | 2011-06-29 | (주)켐스 | Silver nanowire and method of preparing same and transparent conductors using same |
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| CN101550260A (en) * | 2009-05-15 | 2009-10-07 | 吉林大学 | High-dielectric composite material containing silver nanowire and preparing method thereof |
| CN102423808A (en) * | 2011-12-14 | 2012-04-25 | 天津工业大学 | Quick high concentration synthesizing method of silver nanometer line |
| CN103111628A (en) * | 2013-03-17 | 2013-05-22 | 青岛科技大学 | Method for preparing bendable Ag nanowire |
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Inventor after: Liu Bitao Inventor after: Jin Rong Inventor after: Chen Shanyong Inventor after: Li Junjun Inventor after: Li Lu Inventor before: Liu Bitao Inventor before: Li Lu Inventor before: Xiang Chengdan Inventor before: Chen Shanyong Inventor before: Jin Rong Inventor before: Li Junjun |
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Effective date of registration: 20211227 Address after: 402760 5th floor, building 52, enterprise Tiandi, Bishan District, Chongqing Patentee after: Chongqing Dingwang Technology Co.,Ltd. Address before: 402168 Chongqing College of Arts and Sciences, Shuangzhu Town, Yongchuan District, Chongqing Patentee before: CHONGQING University OF ARTS AND SCIENCES |