CN106001544A - Method for purifying silver nanowires through settling separation - Google Patents
Method for purifying silver nanowires through settling separation Download PDFInfo
- Publication number
- CN106001544A CN106001544A CN201610538533.4A CN201610538533A CN106001544A CN 106001544 A CN106001544 A CN 106001544A CN 201610538533 A CN201610538533 A CN 201610538533A CN 106001544 A CN106001544 A CN 106001544A
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- CN
- China
- Prior art keywords
- nano silver
- silver wire
- ethyl acetate
- polyvinylpyrrolidone
- silver nanowires
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for purifying silver nanowires through settling separation. The method is characterized by comprising the following steps of uniformly scattering a silver nanowire mother liquid synthetized by adopting a polyhydric alcohol method in a polyvinylpyrrolidone alcoholic solution, feeding ethyl acetate, standing, gathering the silver nanowires and precipitating the silver nanowires, and removing a supernatant liquid; and precipitating repeatedly to obtain the purified silver nanowires. Silver nanoparticles in the silver nanowire mother liquid are removed with ethyl acetate, the silver nanowires are purified, operation is simple, the production cost is low, the purifying effect is good, and the haze of a transparent conductive thin film prepared from the purified silver nanowires is remarkably reduced.
Description
Technical field
The present invention relates to the method for purification of a kind of nano silver wire.
Background technology
Nano silver wire nesa coating is considered as the new function material being hopeful most to substitute TIO thin film, its good transparency
It is made to can be used for various flat pannel display, touch screen, thin-film solar cells, Organic Light Emitting Diode (OLED), sensor and resist
The fields such as electrostatic coatings.
It is mainly polyxol method, due to the problem of preparation principle, in its products therefrom mother solution for preparing the method for nano silver wire
Certainly exist the situation that silver nano-grain and nano silver wire are blended, it is therefore desirable to purify.Purify centrifugal point of general employing at present
From method or sieve method.Wherein, centrifugal separation is time-consuming, power consumption, reduces productivity, and separating effect is poor；And sieve method is often
Easily cause thinner nano silver wire and be deposited on mesh surface obstruction sieve aperture, reduce separation efficiency, simultaneously because thinner silver nanoparticle
Line can " be bored a hole ", will also result in the loss of nano silver wire.
Patent CN201510690210.2 discloses the method for purification of a kind of nano silver wire, and the method goes desilver to receive by water and acetone
Rice grain, it is achieved purify purpose.It is known that acetone is a kind of colourless transparent liquid, have special acrid odors, inflammable,
Volatile.What is more important, human central nervous system is impacted by acetone acute poisoning and chronic poisoning, thus results in
Harm the biggest.And the large usage quantity of acetone in the method disclosed in this patent, in process of production to operating environment requirements relatively
Height is the highest to the liquid waste processing also cost after using.
Summary of the invention
The present invention is for avoiding the weak point existing for above-mentioned prior art, it is provided that the side of a kind of settlement separate purification nano silver wire
Method, it is intended to simplify purification step, improve reduction pollution while product purity.
To achieve these goals, the present invention adopts the following technical scheme that
The present invention is by the method for settlement separate purification nano silver wire, and its feature is, comprises the steps:
The first step, the nano silver wire mother solution using polyxol method synthesis is dispersed in the alcoholic solution of polyvinylpyrrolidone
In, obtain nano silver wire mother solution dispersion liquid；It is subsequently adding ethyl acetate, stands, make nano silver wire reunite and precipitate, in removal
Layer liquid, remains bottom precipitation；
Second step, bottom precipitation is dispersed in the alcoholic solution of polyvinylpyrrolidone, adds ethyl acetate, stand,
Make nano silver wire reunite and precipitate, removing supernatant liquid, again remain bottom precipitation；
3rd step, repetition second step 3～5 times, nano silver wire after being purified；
4th step, nano silver wire after described purification is dispersed in ethanol, then adds ethyl acetate, stand, make silver
Nanowire cluster coalescence precipitates, and removes supernatant liquid, it is thus achieved that nano silver wire after again purifying；
5th step, by described again purify after nano silver wire dispersed in deionized water, obtain the aqueous solution of nano silver wire,
Complete the purification of nano silver wire.
Wherein, mass fraction≤5% of the alcoholic solution of described polyvinylpyrrolidone.
Preferably, in the first step, the solid content of described nano silver wire mother solution is 0.1～20mg/mL, described nano silver wire mother solution,
The alcoholic solution of described polyvinylpyrrolidone and the volume ratio of described ethyl acetate are 1:1:1～1.5.
Preferably, in second step, the volume of ethyl acetate is 0.5～1.5 times of the alcoholic solution volume of polyvinylpyrrolidone.
Preferably, in the 4th step volume is alcohol by volume 0.5～1.5 times of ethyl acetate.
Preferably, the time of described standing is 5～15min.
Preferably, in described nano silver wire mother solution, the average diameter of contained nano silver wire is 20～200nm, and average length is 20～100
μm。
The model of polyvinylpyrrolidone used can be the one in K15, K17, K30, K60, K90 or combination in any.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention utilizes ethyl acetate to remove the silver nano-grain in nano silver wire mother solution, purifies nano silver wire, operation
Simply, low production cost, refining effect is good, and the mist degree of the transparent conductive film prepared by nano silver wire after purification substantially drops
Low.
2, the raw materials used ethanol of the present invention, ethyl acetate are colourless transparent liquids, hypotoxicity, to the working environment in production process
Require low, minimum to the health effect of human body, and cost is the most relatively low in liquid waste processing and use
Accompanying drawing explanation
Fig. 1 is the metallurgical microscope figure purifying front nano silver wire in the embodiment of the present invention；
Fig. 2 be the embodiment of the present invention purifies after the metallurgical microscope figure of nano silver wire.
Detailed description of the invention
Embodiment 1
The present embodiment initially with Jian-Yang Lin article " Jian-Yang Lin, Yu-Lee Hsueh, Jung-Jie Huang,
Jia-Rung Wu Thin Solid Films 584 (2015) 243 247 " disclosed in polyxol method prepare nano silver wire mother solution；
The current solid content of gained nano silver wire is 2mg/mL.Fig. 1 is its metallurgical microscope figure, it can be seen that synthesized silver nanoparticle
Line average diameter is 20～100 μm in 20nm, average length, can be seen that in nano silver wire containing substantial amounts of silver nanoparticle simultaneously
Grain.
As follows above-mentioned nano silver wire is purified:
The first step: take 20mL nano silver wire mother solution and be dispersed in the ethanol of the polyvinylpyrrolidone that 20mL mass fraction is 2%
In solution, obtain nano silver wire dispersion liquid；It is subsequently adding 30mL ethyl acetate, stands 5min, make nano silver wire reunite also
Precipitation, removes supernatant liquid, remains bottom precipitation；
Second step: again add the alcoholic solution that 10mL mass fraction is 2% polyvinylpyrrolidone, make bottom precipitation again
After being uniformly dispersed, it is subsequently adding the ethyl acetate of 10mL, stands 5min, make nano silver wire reunite and precipitate, remove upper strata
Liquid, remains bottom precipitation again；
3rd step: repeat second step 3 times, nano silver wire after being purified；
4th step: be dispersed in 10mL ethanol by nano silver wire after purification, is subsequently adding 10mL ethyl acetate, stands
5min, makes nano silver wire reunite and precipitates, and removes supernatant liquid, it is thus achieved that nano silver wire after again purifying；
5th step: during nano silver wire is dispersed in 10mL deionized water after again purifying, obtains the aqueous solution of nano silver wire,
Complete the purification of nano silver wire.
Fig. 2 be purify after the metallurgical microscope figure of nano silver wire, understand with Fig. 1 contrast, after purification, silver nano-grain can arrive very well
Removal, the purity of nano wire is significantly improved.
The aqueous solution of the nano silver wire obtained after being respectively adopted nano silver wire mother solution and purifying, by Meyerrod method at PET
Make uniform film on substrate, then use photoelectricity its mist degree of mist degree instrument test.
Experimental results shows, the PET mist degree after the coating of nano silver wire mother solution reaches 8%, and resistance test shows non-conductive；Carry
The mist degree of the PET of the aqueous solution coating of pure rear nano silver wire is only 1.3%, and resistance test is shown as 40～70 ohm, after showing to purify
Mist degree and resistance reduce substantially.
Last it is noted that obvious, above-described embodiment is only for clearly demonstrating example of the present invention, and the most right
The restriction of embodiment.For those of ordinary skill in the field, can also be made other on the basis of the above description
The change of multi-form or variation.Here without also cannot all of embodiment be given exhaustive.And thus amplified out aobvious
And the change being clear to or variation still in protection scope of the present invention among.
Claims (7)
1. the method by settlement separate purification nano silver wire, it is characterised in that comprise the steps:
The first step, the nano silver wire mother solution using polyxol method synthesis is dispersed in the alcoholic solution of polyvinylpyrrolidone
In, obtain nano silver wire mother solution dispersion liquid；It is subsequently adding ethyl acetate, stands, make nano silver wire reunite and precipitate, in removal
Layer liquid, remains bottom precipitation；
Second step, bottom precipitation is dispersed in the alcoholic solution of polyvinylpyrrolidone, adds ethyl acetate, stand,
Make nano silver wire reunite and precipitate, removing supernatant liquid, again remain bottom precipitation；
3rd step, repetition second step 3～5 times, nano silver wire after being purified；
4th step, nano silver wire after described purification is dispersed in ethanol, then adds ethyl acetate, stand, make silver
Nanowire cluster coalescence precipitates, and removes supernatant liquid, it is thus achieved that nano silver wire after again purifying；
5th step, by described again purify after nano silver wire dispersed in deionized water, obtain the aqueous solution of nano silver wire,
Complete the purification of nano silver wire.
Method the most according to claim 1, it is characterised in that: the quality of the alcoholic solution of described polyvinylpyrrolidone is divided
Number≤5%.
Method the most according to claim 1 and 2, it is characterised in that: in the first step, described consolidating of nano silver wire mother solution contains
Amount is 0.1～20mg/mL, described nano silver wire mother solution, the alcoholic solution of described polyvinylpyrrolidone and described ethyl acetate
Volume ratio is 1:1:1～1.5.
Method the most according to claim 1 and 2, it is characterised in that: in second step, the volume of ethyl acetate is polyethylene pyrrole
0.5～1.5 times of the alcoholic solution volume of pyrrolidone.
Method the most according to claim 1 and 2, it is characterised in that: in the 4th step, the volume of ethyl acetate is alcohol by volume
0.5～1.5 times.
Method the most according to claim 1, it is characterised in that: the time of described standing is 5～15min.
Method the most according to claim 1, it is characterised in that: in described nano silver wire mother solution, contained nano silver wire is average
A diameter of 20～200nm, average length is 20～100 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610538533.4A CN106001544A (en) | 2016-07-08 | 2016-07-08 | Method for purifying silver nanowires through settling separation |
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| CN201610538533.4A CN106001544A (en) | 2016-07-08 | 2016-07-08 | Method for purifying silver nanowires through settling separation |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107127333A (en) * | 2017-05-22 | 2017-09-05 | 哈尔滨工业大学 | A kind of method by vibrating and settling purification nano silver wire |
| CN107598152A (en) * | 2017-08-30 | 2018-01-19 | 浙江科创新材料科技有限公司 | A kind of method of purification of nano silver wire |
| CN110402276A (en) * | 2017-03-14 | 2019-11-01 | 同和电子科技有限公司 | The manufacturing method of the good silver nanowires dispersion liquid of line property detached from each other |
| CN110814361A (en) * | 2019-11-08 | 2020-02-21 | 惠州达祺光电科技有限公司 | Silver nanowire purification method |
| CN113084155A (en) * | 2021-03-30 | 2021-07-09 | 重庆烯宇新材料科技有限公司 | Green, mild and efficient purification method of nano silver wires |
| JP2022528106A (en) * | 2019-04-03 | 2022-06-08 | カンブリオス フィルム ソリューションズ コーポレーション | Purification of metal nanostructures |
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| CN102575117A (en) * | 2009-08-24 | 2012-07-11 | 凯博瑞奥斯技术公司 | Purification of metal nanostructures for improved haze in transparent conductors made from the same |
| CN103785842A (en) * | 2014-01-16 | 2014-05-14 | 复旦大学 | Nanocrystalline metal elementary substance separation method |
| WO2015157741A2 (en) * | 2014-04-11 | 2015-10-15 | Cambrios Technologies Corporation | Methods of controlling nanowire morphology |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through hydrocyclone |
| CN105345022A (en) * | 2015-10-22 | 2016-02-24 | 东华大学 | Purification method for silver nanowire |
| CN105537622A (en) * | 2016-01-07 | 2016-05-04 | 嘉兴禾浦光电科技有限公司 | Method for preparing silver nanowires |
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Patent Citations (6)
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| CN102575117A (en) * | 2009-08-24 | 2012-07-11 | 凯博瑞奥斯技术公司 | Purification of metal nanostructures for improved haze in transparent conductors made from the same |
| CN103785842A (en) * | 2014-01-16 | 2014-05-14 | 复旦大学 | Nanocrystalline metal elementary substance separation method |
| WO2015157741A2 (en) * | 2014-04-11 | 2015-10-15 | Cambrios Technologies Corporation | Methods of controlling nanowire morphology |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through hydrocyclone |
| CN105345022A (en) * | 2015-10-22 | 2016-02-24 | 东华大学 | Purification method for silver nanowire |
| CN105537622A (en) * | 2016-01-07 | 2016-05-04 | 嘉兴禾浦光电科技有限公司 | Method for preparing silver nanowires |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110402276A (en) * | 2017-03-14 | 2019-11-01 | 同和电子科技有限公司 | The manufacturing method of the good silver nanowires dispersion liquid of line property detached from each other |
| CN107127333A (en) * | 2017-05-22 | 2017-09-05 | 哈尔滨工业大学 | A kind of method by vibrating and settling purification nano silver wire |
| CN107127333B (en) * | 2017-05-22 | 2019-04-02 | 哈尔滨工业大学 | A method of by vibrating and settling purification silver nanowires |
| CN107598152A (en) * | 2017-08-30 | 2018-01-19 | 浙江科创新材料科技有限公司 | A kind of method of purification of nano silver wire |
| JP2022528106A (en) * | 2019-04-03 | 2022-06-08 | カンブリオス フィルム ソリューションズ コーポレーション | Purification of metal nanostructures |
| CN110814361A (en) * | 2019-11-08 | 2020-02-21 | 惠州达祺光电科技有限公司 | Silver nanowire purification method |
| CN113084155A (en) * | 2021-03-30 | 2021-07-09 | 重庆烯宇新材料科技有限公司 | Green, mild and efficient purification method of nano silver wires |
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Effective date of registration: 20170615 Address after: 230088 A118, 602 Mount Huangshan Road, hi tech Zone, Anhui, Hefei Applicant after: HEFEI SILVER TECHNOLOGY CO., LTD. Address before: 230088 Anhui high tech Zone, Mount Huangshan, No. 602 Hefei Road, A105 Applicant before: Hefei Vigon Material Technologies Co., Ltd. |
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Application publication date: 20161012 |