CN107127333A - A kind of method by vibrating and settling purification nano silver wire - Google Patents
A kind of method by vibrating and settling purification nano silver wire Download PDFInfo
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- CN107127333A CN107127333A CN201710371668.0A CN201710371668A CN107127333A CN 107127333 A CN107127333 A CN 107127333A CN 201710371668 A CN201710371668 A CN 201710371668A CN 107127333 A CN107127333 A CN 107127333A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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Abstract
A kind of method by vibrating and settling purification nano silver wire, belongs to nano silver wire purification technique field.The invention solves the problems that there is the bad technical problems of impurity removal effect such as the big, particle of acetone consumption in existing purification nano silver wire method.The method of the present invention：First, acetone is added into the nano silver wire mother liquor prepared using polyol process, vibrated, remove upper solution；Two then add distilled water, vibration be completely dispersed to nano wire, add acetone, vibrate, remove upper solution；If the 3, upper solution is muddy, the operation of repeat step two removes upper solution, that is, completes the purification of nano silver wire to the complete clear of upper solution.The present invention will add acetone and oscillating phase is combined, and progressively the impurity such as particle in separation nanowire solution, greatly improves the purity of nano silver wire, acetone consumption is reduced, and without standing, shortens processing time, operating procedure is few, without complex device, with significant low-cost advantage.
Description
Technical field
The invention belongs to nano silver wire purification technique field；It is specifically related to a kind of to purify nano silver wire by vibrating and settling
Method.
Background technology
In recent years, flexible electronic device obtains extensive concern, and the electrode based on electrical-conductive nanometer material is high-performance flexible
One of most important part of electronic device.Nano silver wire is because of its high electric conductivity and pliability, preferable stability and relatively low
Cost turn into one of most promising flexible electrode material.
Polyol process is because product structure is controllable, yield is high, the low advantage of cost, as the master for preparing nano silver wire at present
Want method.The nucleus of nano wire can not be grown to due to forming some in building-up process, and some that may be remained are not complete
The silver halide particle of reaction, makes to certainly exist nanometer or submicron particles and irregular nanometer sheet, the nanometer of tubbiness in product
Rod etc..Traditional method of purification is multiple centrifugation steps cleaning, but this method is not good enough to the separating effect of the impurity such as particle.And adopt
Very low with the method efficiency of membrane filtration, condition is not easy to control.
Patent CN201510690210.2 disclose it is a kind of in the aqueous solution of nano silver wire plus acetone after stand make nanometer
A ball of string gathers, so that the method that particle is separated with nano wire.But the method needs to consume a large amount of acetone, and cost is higher, and need
Stand for a long time, such as in the patent Example, 20mg nano silver wires are dispersed in the water that 10mL contains polyvinylpyrrolidone (PVP)
, it is necessary to by 4 purifications, 160mL acetone be needed altogether, standing total time is 40min, is taken more in solution.Patent
CN201610538533.4, which discloses a kind of stood in the aqueous solution of nano silver wire after addition ethyl acetate, makes nano wire reunite
And the method purified, but the method step is more, and operation is relatively complicated, and reagent consumption is also more, for example the patent Example
In, to 20mL nano silver wire mother liquors, ethanol solution and 70mL acetic acid second of the 60mL containing PVP need to be needed altogether by 5 purification operations
Ester.Document (Mayousse C, Celle C, Moreau E, et al.Improvements in purification
ofsilver nanowires by decantation and fabrication offlexible transparent
electrodes.Application to capacitive touch sensors[J].Nanotechnology,2013,24
(21):215501.) by the way that nano silver wire mother liquor to be stood to the side for settling nano wire and separating impurity particle naturally reported in
Method, this method is simple to operate, with low cost, but time of repose is up to 2 days, significantly extends process cycle.
The content of the invention
It is an object of the invention to provide a kind of refining effect is good, reagent consumption less, process cycle it is short, and effectively reduce into
The method of this purification nano silver wire.
A kind of method by vibrating and settling purification nano silver wire is completed in the steps below in the present invention：
Step 1: adding acetone into the nano silver wire mother liquor prepared using polyol process, vibrate, remove upper solution；
Step 2: then adding distilled water, vibration is completely dispersed to nano wire, adds acetone, is vibrated, and removes upper strata molten
Liquid；
Step 3: if upper solution is muddy, the operation of repeat step two removes upper strata to the complete clear of upper solution
Solution, that is, complete the purification of nano silver wire；Nano silver wire after step 3 is handled is dispersed in absolute ethyl alcohol and preserved.
Further limit, the solid content in nano silver wire mother liquor described in step one is 1-10mg/mL, by acetone and silver nanoparticle
The volume ratio of line mother liquor is (3-4):1 proportioning adds acetone；The volume of mother liquor in distilled water and the first step that step 2 is added
Than for (1-2):3, the acetone of addition and the volume ratio of distilled water are (2.5-4):1.
The duration of oscillation added described in step one and step 2 after acetone is 15-25s, preferably 20s.
Distilled water described in step 3 is identical with the consumption of step 2 with acetone consumption or consumption of than step 2 is few.
The use blending instrument of step one or step 2 carries out oscillating operation, and its oscillation rate is higher than 500 revs/min；Also may be used
With using manual operations.
The average diameter of nano silver wire is 20-200nm in nano silver wire mother liquor described in step one, and average length is 10-100
μm。
The present invention, which is added after acetone, to be vibrated, it is therefore an objective to nano silver wire is reunited immediately and is settled, the impurity such as particle is persisted
In upper solution, the purpose that upper solution reaches purification is removed.Step 1: it is to make nanometer that the purpose vibrated after acetone is added in two
Line is reunited and settled as early as possible, is thus reduced acetone consumption and is avoided time of repose, if sedimentation is not thorough, by influence impurity separation
Effect, and the loss of nano wire is caused during upper solution is removed, therefore in this two step, after vibration after nano wire sedimentation
Remove upper solution.
It is that the nano silver wire for making sedimentation disperses again that step 2 of the present invention, which adds vibration purpose after distilled water, adds third
Ketone, vibration, makes nano wire reunite again and settle, reaches the purpose further purified.Part after distilled water is added in step 2
Nano wire is still in aggregating state, and the impurity such as particle may be mixed in the nano wire of precipitation, will influence refining effect, added and steamed
Vibrated after distilled water, just it is to add acetone after nano wire is well dispersed in water, otherwise will influence refining effect.
The present invention, which adds acetone and vibrated, makes nano silver wire reunite and selective precipitation, so that nano wire and particle etc. are miscellaneous
Matter is separated, and refining effect is good, simple to operate.
The present invention can be such that nano silver wire settles immediately using the method for adding acetone and vibrating, without standing, so that progressively
The impurity such as the particle contained in separation of Silver nanowire solution, compared with the natural subsidence method described in existing patent, are substantially reduced
The consumption of acetone, decrement is up to 80%, and shortens the purification time, with significant cost advantage.
Brief description of the drawings
Fig. 1 is the stereoscan photograph before nano silver wire purification in the embodiment of the present invention 1；
Fig. 2 is the stereoscan photograph after nano silver wire purification in the embodiment of the present invention 1；
Fig. 3 is the stereoscan photograph before nano silver wire purification in the embodiment of the present invention 2；
Fig. 4 is the stereoscan photograph after nano silver wire purification in the embodiment of the present invention 2.
Embodiment
With reference to specific embodiment, the present invention is further elaborated.It should be noted that following embodiment is only
Implementation for illustrating the present invention, rather than operation of the present invention and parameter area are limited, thus amplify out
Change, still in the protection domain of the claims in the present invention.
Embodiment 1：Nano silver wire is prepared according to polyol process, is operated as follows：Solution, including A (CuCl are prepared first2It is molten
In ethylene glycol (EG), Cl-Concentration is 1mM), B (190mg PVP are dissolved in 15mL EG, and wherein PVP molecular weight is 1,300,
000), C (240mgAgNO3It is dissolved in 15mL EG).3.17mL solution As are added in 46.8mL EG, 170 DEG C, addition are preheating to
15mL solution Bs, are heated to that 15mL solution Cs are uniformly added drop-wise in above-mentioned solution in 170 DEG C, 60min, and continue guarantor at 170 DEG C
Warm 20min, is cooled down in atmosphere, obtains nano silver wire mother liquor.Solid content about 1.9mg/mL in mother liquor.Fig. 1 is not purified
Nano wire stereoscan photograph, nanowire length is between 0-220 μm.In addition to nano wire, also comprising more in product
Nano particle.Purified in accordance with the following steps：
Step 1: taking 3mL mother liquors, 9mL acetone is added thereto, using blending instrument with 2000 revs/min of rate oscillation
20 seconds, nano silver wire was reunited and settled completely, removed upper suspension；
Step 2,2mL distilled water is added into the precipitum of step one, and vibration makes nano wire be well dispersed in distilled water
In, 6mL acetone is added, using blending instrument with 2000 revs/min of rate oscillation 20 seconds, nano silver wire is reunited and settled completely,
At this moment supernatant liquid has changed into clear, removes it；Complete purification operations；
3mL ethanol is added into the nano silver wire after purification, vibration makes nano wire fully dispersed in ethanol, obtains silver
Nanowire dispersion, is preserved.
Fig. 2 is the nano wire stereoscan photograph after purification, it is seen that most of granule foreigns all have been cleared by, nanometer
Line purity is improved significantly.
Embodiment 2：Nano silver wire is prepared according to polyol process, is operated as follows：Solution is prepared first, solvent is EG, wrap
Include A (KBr solution, concentration is 2mM), B (PVP solution, concentration is 300mM, and wherein PVP molecular weight is 1,300,000), C
(AgNO3Solution, concentration is 300mM).12.008mL EG, 2.116mL solution As, 3.526mL solution are sequentially added in flask
It is put into after B, 2.351mL solution C, stirring 30min in the oil bath of preheating and is heated to 150 DEG C, 3h is incubated under without stirring state,
Cooled down in air, obtain nano silver wire mother liquor.Solid content about 3.8mg/mL in mother liquor.Fig. 3 is that not purified nano wire is swept
Electromicroscopic photograph is retouched, nanowire length is between 0-80 μm.In addition to nano wire, the nanometer of more tubbiness is also included in product
Rod, sub-micron and micron particles.Purified as follows：
Step 1: taking 6mL mother liquors, 18mL acetone is added thereto, using blending instrument with 2000 revs/min of rate oscillation
20 seconds, nano silver wire was reunited and settled completely, removed upper suspension；
Step 2: adding 4mL distilled water into first step precipitum, vibration makes nano wire be well dispersed in distilled water,
10mL acetone is added, using blending instrument with 2000 revs/min of rate oscillation 20 seconds, nano wire is reunited and settled completely, removed
Upper suspension；
Step 3: the operation of repeat step two 1 time, at this moment supernatant liquid has changed into clear, removes it, remaining
Nano silver wire after purification, completes purification operations；
6mL ethanol is added into the nano silver wire after purification, vibration makes nano wire fully dispersed in ethanol, obtains silver
Nanowire dispersion, is preserved.
Fig. 4 is the nano wire stereoscan photograph after purification, it is seen that most of particles and nanometer rods impurity are all clear
Remove, nano wire purity is improved significantly.
In the embodiment of the above two, acetone volume integral used in Unit Weight nano silver wire Wei not patent CN201510690210.2
The 33% and 20% of acetone used in the disclosed embodiments, and time of repose is avoided, with significant cost advantage.
Claims (8)
1. it is a kind of by vibrating and settling the method for purifying nano silver wire, it is characterised in that the method for purification is in the steps below
Complete：
Step 1: adding acetone into the nano silver wire mother liquor prepared using polyol process, vibrate, remove upper solution；
Step 2: then adding distilled water, vibration is completely dispersed to nano wire, adds acetone, is vibrated, and removes upper solution；
Step 3: if upper solution is muddy, the operation of repeat step two removes upper strata molten to the complete clear of upper solution
Liquid, that is, complete the purification of nano silver wire.
2. according to the method described in claim 1, it is characterised in that the solid content in nano silver wire mother liquor described in step one is 1-
10mg/mL, is (3-4) by the volume ratio of acetone and nano silver wire mother liquor:1 proportioning adds acetone.
3. according to the method described in claim 1, it is characterised in that duration of oscillation described in step one is 15-25s.
4. method according to claim 2, it is characterised in that the body of mother liquor in distilled water and the first step that step 2 is added
Product is than being (1-2):3, the acetone of addition and the volume ratio of distilled water are (2.5-4):1.
5. according to the method described in claim 1, it is characterised in that the duration of oscillation added described in step 2 after acetone is 15-
25s。
6. according to the method described in claim 1, it is characterised in that distilled water described in step 3 and acetone consumption and step 2
Consumption it is identical or consumption of than step 2 is few.
7. according to the method described in claim 1, it is characterised in that：Vibration behaviour is carried out using blending instrument in step one or step 2
Make, its oscillation rate is higher than 500 revs/min；Or vibrated by hand in step one or step 2.
8. according to the method described in claim 1, it is characterised in that：Nano silver wire is flat in nano silver wire mother liquor described in step one
A diameter of 20-200nm, average length is 10-100 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710371668.0A CN107127333B (en) | 2017-05-22 | 2017-05-22 | A method of by vibrating and settling purification silver nanowires |
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| CN201710371668.0A CN107127333B (en) | 2017-05-22 | 2017-05-22 | A method of by vibrating and settling purification silver nanowires |
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| CN107127333B CN107127333B (en) | 2019-04-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482900A (en) * | 2018-12-14 | 2019-03-19 | 浙江加州国际纳米技术研究院台州分院 | A kind of method high-volume synthesis and efficiently purify ultra-fine silver nanowires |
| CN114289728A (en) * | 2020-09-21 | 2022-04-08 | 湖北大学 | Synthesis and simple purification method of silver nanowires |
| CN115194143A (en) * | 2022-06-22 | 2022-10-18 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinyl pyrrolidone coated nano particles |
| CN115283661A (en) * | 2022-08-09 | 2022-11-04 | 北京化工大学 | Method for purifying copper nanowire and copper nanowire prepared by same |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3098134B1 (en) * | 2019-07-02 | 2021-07-02 | Commissariat Energie Atomique | Process for the purification of metallic nanowires |
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| JP2009007593A (en) * | 2007-06-26 | 2009-01-15 | Furukawa Electric Co Ltd:The | Fine particle dispersion and method for producing fine particle dispersion |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482900A (en) * | 2018-12-14 | 2019-03-19 | 浙江加州国际纳米技术研究院台州分院 | A kind of method high-volume synthesis and efficiently purify ultra-fine silver nanowires |
| CN114289728A (en) * | 2020-09-21 | 2022-04-08 | 湖北大学 | Synthesis and simple purification method of silver nanowires |
| CN115194143A (en) * | 2022-06-22 | 2022-10-18 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinyl pyrrolidone coated nano particles |
| CN115194143B (en) * | 2022-06-22 | 2023-11-14 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinylpyrrolidone coated nano particles |
| CN115283661A (en) * | 2022-08-09 | 2022-11-04 | 北京化工大学 | Method for purifying copper nanowire and copper nanowire prepared by same |
| CN115283661B (en) * | 2022-08-09 | 2024-09-13 | 北京化工大学 | Method for purifying copper nanowire and copper nanowire manufactured by the method |
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