CN105397107A - Preparation method of ultra-long silver nanowires - Google Patents
Preparation method of ultra-long silver nanowires Download PDFInfo
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- CN105397107A CN105397107A CN201510985639.4A CN201510985639A CN105397107A CN 105397107 A CN105397107 A CN 105397107A CN 201510985639 A CN201510985639 A CN 201510985639A CN 105397107 A CN105397107 A CN 105397107A
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- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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Abstract
The invention discloses a controllable preparation method of ultra-long silver nanowires. According to the method, mother solutions of the silver nanowires are obtained through reaction of silver compounds, high-concentration silver nanowire control agents and dispersing agents; the mother solutions are dispersed into ethanol solutions after being subjected to centrifugal separation and washing several times, and then the ultra-long silver nanowires with the diameter ranging from 20 nm to 40 nm and the length ranging from 300 um to 500 um can be obtained. The preparation method has the advantages that the process is simple, the repeatability is high, the stability is good, the production cost is low, the sizes of the silver nanowires are controllable, and mass production is easy to realize.
Description
Technical field
The present invention relates to metal nano material field, a kind of preparation method of ultra-long silver nanowire is provided especially.
Technical background
Metal Nano structure, due to electricity, light, magnetic, the hot property of its uniqueness, is widely used in microelectronics, photoelectronic device, sensor emerging technology areas; In various nano material, one dimension nano silver wire has higher conductive and heat-conductive ability and excellent chemical stability, makes it will play vital effect in manufacture nanoscale devices.Therefore, the research of preparations and applicatio rapidly and efficiently of one dimension nano silver wire causes the interest of numerous researcher.At present, preparing the topmost method of nano silver wire is polyol process.Chinese patent CN101934378A, under inert gas shielding, adopts the silver-colored source compound of high concentration and ethylene glycol and copper chloride as reactive material, obtains nano silver wire; Chinese patent CN103167920A is obtained by reacting nano silver wire by the agent of nano silver wire growth control and silver compound that are polymerized the polymer obtained containing the polymerizable monomer of N-replacement (methyl) acrylamide under dark conditions in polyalcohol at 25 ~ 180 DEG C; Chinese patent CN104313687A is in stainless steel high pressure water heating kettle, is tied up to the interaction generation nano silver wire of seed-solution and derivant under uniform temperature by the aqueous liquid of template compound, reducing agent and silver-colored source compound.In the past traditional polyol process is prepared in the method for nano silver wire; it is little that the amount of nano silver wire controlling agent needs; need the external world to provide as conditions such as inert gas shielding, shading, high pressure, this certainly will add the complexity of technique, for large-scale production brings inconvenience.Therefore industry needs the nano silver wire that a kind of preparation method is simpler, quality is more excellent, draw ratio is higher.
Summary of the invention
In order to overcome the deficiency of background technology, the object of this invention is to provide a kind of simple, efficient, quick method preparing ultra-long silver nanowire, ultra-long silver nanowire diameter 20 ~ 40nm, the length 300 ~ 500um of synthesis, this method repeatability is high, good stability, production cost are low, nano silver wire size is controlled.
For achieving the above object, the present invention adopts following technical scheme, and a kind of preparation method of ultra-long silver nanowire, is characterized in that, comprises following basic step:
A polyalcohol as end liquid, is incubated 5 ~ 40min, is designated as A liquid by () under 120 DEG C ~ 200 DEG C oil bath temperatures;
B silver nitrate is dissolved in polyhydric alcohol solutions by (), obtain silver nitrate alcoholic solution after ultrasonic disperse, is designated as B liquid;
C silver nanowire growth controlling agent, dispersant are dissolved in polyhydric alcohol solutions by (), ultrasonic disperse postscript is C liquid, and in C liquid, the substance withdrawl syndrome of silver nanowire growth controlling agent is 0.006molL
-1~ 0.06molL
-1;
D () is under the state stirred, above-mentioned B liquid, C liquid are successively slowly at the uniform velocity added drop-wise in A liquid respectively by separatory funnel, and continue reaction, thus obtain nano silver wire mother liquor, in described nano silver wire mother liquor, the substance withdrawl syndrome of silver nanowire growth controlling agent, dispersant, silver nitrate is than being (0.4 ~ 4): (4 ~ 40): (1 ~ 10); The volume of described A liquid accounts for 1/6 ~ 1/3 of cumulative volume;
After e nano silver wire mother liquor reagent wash that step (d) obtains by (), centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire;
Described polyalcohol is the one in ethylene glycol, propane diols or glycerine.
Further, described silver nanowire growth controlling agent is FeCl
36H
2o, NaCl, NiCl
26H
2o, MnCl
24H
2o or CoCl
26H
2one in O.
Further, described dispersant can be the one in PVP K30, polyvinylpyrrolidone K32, polyvinylpyrrolidone K45.
Further, in step (b), (c), ultrasonic power is 80W ~ 200W, and ultrasonic time is 10 ~ 40min.
Further, in step (d), separatory funnel rate of addition controls at 1minmL
-1~ 5minmL
-1.
Further, in step (d), the continuation reaction time is 0.5h ~ 10h.
Further, in step (e), the centrifugal rotational speed of centrifugation is 2000rpm ~ 8000rpm, and centrifugation time is 10min ~ 40min; Described reagent is deionized water, absolute ethyl alcohol or acetone, and washing times is 6 ~ 10 times.
Beneficial effect: adopt the present invention can prepare the ultra-long silver nanowire of diameter 20 ~ 40nm, length 300 ~ 500um, and this method technique is simple, repeatability is high, good stability, production cost are low, nano silver wire size is controlled, easily realize large-scale production.
Accompanying drawing explanation
Fig. 1 is ESEM (SEM) picture of the ultra-long silver nanowire length of the 2-in-1 one-tenth of reflection embodiment;
Fig. 2 is ESEM (SEM) picture of the ultra-long silver nanowire diameter of the 2-in-1 one-tenth of reflection embodiment.
Detailed description of the invention
embodiment 1
The ethylene glycol of 25mL is placed in there-necked flask as end liquid, under 120 DEG C ~ 200 DEG C oil bath temperatures, is incubated 5 ~ 40min, is designated as A liquid; 0.1274g silver nitrate is dissolved in the ethylene glycol solution of 50mL, is ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, obtains silver nitrate alcoholic solution, be designated as B liquid; 0.0527gNaCl, 0.6669gPVP-K32 are dissolved in the ethylene glycol of 50mL simultaneously, are ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, are designated as C liquid; Stir state under, successively by B liquid, C liquid respectively by separatory funnel with 2minmL
-1speed be added drop-wise in A liquid, and continue reaction 0.5h, thus obtain nano silver wire mother liquor; By nano silver wire mother liquor successively with after deionized water, absolute ethanol washing 6 times, centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire.After testing, gained nano silver wire diameter 20 ~ 40nm, length 300 ~ 500um.
embodiment 2
The ethylene glycol of 50mL is placed in there-necked flask as end liquid, under 120 DEG C ~ 200 DEG C oil bath temperatures, is incubated 5 ~ 40min, is designated as A liquid; 0.5096g silver nitrate is dissolved in the ethylene glycol solution of 50mL, is ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, obtains silver nitrate alcoholic solution, be designated as B liquid; Simultaneously by 0.41gFeCl
36H
2o, 1gPVP-K30 are dissolved in the ethylene glycol of 50mL, be ultrasonic 30min in the ultrasonic wave of 100W, be designated as C liquid in ultrasonic power; Stir state under, successively by B liquid, C liquid respectively by separatory funnel with 2minmL
-1speed be added drop-wise in A liquid, and continue reaction 2h, thus obtain nano silver wire mother liquor; By nano silver wire mother liquor successively with after deionized water, absolute ethanol washing 6 times, centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire.Through ESEM (SEM) detect, gained nano silver wire diameter be 20 ~ 40nm as shown in Figure 2, length be 300 ~ 500um as shown in Figure 1.
embodiment 3
The ethylene glycol of 50mL is placed in there-necked flask as end liquid, under 120 DEG C ~ 200 DEG C oil bath temperatures, is incubated 5 ~ 40min, is designated as A liquid; 1.274g silver nitrate is dissolved in the ethylene glycol solution of 50mL, is ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, obtains silver nitrate alcoholic solution, be designated as B liquid; Simultaneously by 0.7254gNiCl
26H
2o, 3.3334gPVP-K45 are dissolved in the ethylene glycol of 50mL, be ultrasonic 30min in the ultrasonic wave of 100W, be designated as C liquid in ultrasonic power; Stir state under, successively by B liquid, C liquid respectively by separatory funnel with 2minmL
-1speed be added drop-wise in A liquid, and continue reaction 2h, thus obtain nano silver wire mother liquor; By nano silver wire mother liquor successively with after deionized water, absolute ethanol washing 6 times, centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire.After testing, gained nano silver wire diameter 20 ~ 40nm, length 300 ~ 500um.
embodiment 4
The ethylene glycol of 50mL is placed in there-necked flask as end liquid, under 120 DEG C ~ 200 DEG C oil bath temperatures, is incubated 5 ~ 40min, is designated as A liquid; 0.2548g silver nitrate is dissolved in the ethylene glycol solution of 50mL, is ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, obtains silver nitrate alcoholic solution, be designated as B liquid; Simultaneously by 0.9005gFeCl
36H
2o, 1gPVP-K30 are dissolved in the ethylene glycol of 50mL, be ultrasonic 30min in the ultrasonic wave of 100W, be designated as C liquid in ultrasonic power; Stir state under, successively by B liquid, C liquid respectively by separatory funnel with 2minmL
-1speed be added drop-wise in A liquid, and continue reaction 6h, thus obtain nano silver wire mother liquor; By nano silver wire mother liquor successively with after deionized water, absolute ethanol washing 6 times, centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire.After testing, gained nano silver wire diameter 20 ~ 40nm, length 300 ~ 500um.
embodiment 5
The ethylene glycol of 50mL is placed in there-necked flask as end liquid, under 120 DEG C ~ 200 DEG C oil bath temperatures, is incubated 5 ~ 40min, is designated as A liquid; 0.5096g silver nitrate is dissolved in the ethylene glycol solution of 50mL, is ultrasonic 30min in the ultrasonic wave of 100W in ultrasonic power, obtains silver nitrate alcoholic solution, be designated as B liquid; Simultaneously by 0.2706gCoCl
26H
2o, 1gPVP-K30 are dissolved in the ethylene glycol of 50mL, be ultrasonic 30min in the ultrasonic wave of 100W, be designated as C liquid in ultrasonic power; Stir state under, successively by B liquid, C liquid respectively by separatory funnel with 2minmL
-1speed be added drop-wise in A liquid, and continue reaction 10h, thus obtain nano silver wire mother liquor; By nano silver wire mother liquor successively with after deionized water, absolute ethanol washing 6 times, centrifugation, be scattered in ethanolic solution, obtain ultra-long silver nanowire.After testing, gained nano silver wire diameter 20 ~ 40nm, length 300 ~ 500um.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (7)
1. a preparation method for ultra-long silver nanowire, is characterized in that, comprises following basic step:
A polyalcohol as end liquid, is incubated 5 ~ 40min, is designated as A liquid by () under 120 DEG C ~ 200 DEG C oil bath temperatures;
B silver nitrate is dissolved in polyhydric alcohol solutions by (), obtain silver nitrate alcoholic solution after ultrasonic disperse, is designated as B liquid;
C silver nanowire growth controlling agent, dispersant are dissolved in polyhydric alcohol solutions by (), ultrasonic disperse postscript is C liquid, and in C liquid, the substance withdrawl syndrome of silver nanowire growth controlling agent is 0.006molL
-1~ 0.06molL
-1;
D above-mentioned B liquid, C liquid, under the state stirred, are successively slowly at the uniform velocity added drop-wise in A liquid respectively by separatory funnel, and continue reaction, thus obtain nano silver wire mother liquor by (); In described nano silver wire mother liquor, the substance withdrawl syndrome of silver nanowire growth controlling agent, dispersant, silver nitrate is than being (0.4 ~ 4): (4 ~ 40): (1 ~ 10), and the volume of described A liquid accounts for 1/6 ~ 1/3 of cumulative volume;
After e nano silver wire mother liquor reagent wash that step (d) obtains by (), centrifugation, be scattered in ethanolic solution, obtain the ultra-long silver nanowire that length is 300 ~ 500um;
Described polyalcohol is the one in ethylene glycol, propane diols or glycerine.
2. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, described silver nanowire growth controlling agent is FeCl
36H
2o, NaCl, NiCl
26H
2o, MnCl
24H
2o or CoCl
26H
2one in O.
3. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, described dispersant can be the one in PVP K30, polyvinylpyrrolidone K32, polyvinylpyrrolidone K45.
4. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, in step (b), (c), ultrasonic power is 80W ~ 200W, and ultrasonic time is 10 ~ 40min.
5. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, in step (d), separatory funnel rate of addition controls at 1minmL
-1~ 5minmL
-1.
6. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, in step (d), the continuation reaction time is 0.5h ~ 10h.
7. the preparation method of a kind of ultra-long silver nanowire according to claim 1, is characterized in that, in step (e), the centrifugal rotational speed of centrifugation is 2000rpm ~ 8000rpm, and centrifugation time is 10min ~ 40min; Described reagent is deionized water, absolute ethyl alcohol or acetone, and washing times is 6 ~ 10 times.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511596A (en) * | 2013-09-30 | 2015-04-15 | 中科院广州化学有限公司 | Continuous preparation method and device for nano-silver wire |
| CN106825610A (en) * | 2017-03-24 | 2017-06-13 | 苏州范曼新材料科技有限公司 | A kind of magnanimity preparation method of the ultra-fine nano silver wire of overlength |
| CN108157387A (en) * | 2017-11-27 | 2018-06-15 | 东南大学 | A kind of nano silver wire antibacterial aeroge and its preparation method and application |
| CN108262487A (en) * | 2018-01-20 | 2018-07-10 | 浙江大学 | The method that minor diameter nano silver wire is prepared using mixed alcohol |
| CN108436105A (en) * | 2018-06-07 | 2018-08-24 | 乐凯华光印刷科技有限公司 | A kind of overlength nano-silver thread dispersion liquid and preparation method thereof |
| CN108441949A (en) * | 2018-04-28 | 2018-08-24 | 无锡英特派金属制品有限公司 | A kind of preparation method of nano-silver thread |
| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
| CN108687358A (en) * | 2018-05-24 | 2018-10-23 | 首都师范大学 | A method of preparing compound silver nano wire |
| CN108971510A (en) * | 2018-07-26 | 2018-12-11 | 深圳清华大学研究院 | Silver nanowires and preparation method thereof, silver nanowires film and laminated film |
| CN109797470A (en) * | 2019-01-22 | 2019-05-24 | 常州天宇宏图电子有限公司 | A kind of preparation method of compliant conductive yarn |
| CN110010876A (en) * | 2019-04-15 | 2019-07-12 | 深圳市高能达电池有限公司 | A kind of controllable method for preparing of lithium sulphur one-shot battery nano anode material |
| CN110170644A (en) * | 2019-05-31 | 2019-08-27 | 陕西科技大学 | A method of by being centrifuged and settling purification silver nanowires |
| CN110586928A (en) * | 2019-09-20 | 2019-12-20 | 华南理工大学 | High-length-diameter-ratio silver nanowire based on one-pot polyol method and preparation method and application thereof |
| CN111036930A (en) * | 2019-12-25 | 2020-04-21 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of silver nanowire block for SERS detection |
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| CN102423808A (en) * | 2011-12-14 | 2012-04-25 | 天津工业大学 | Quick high concentration synthesizing method of silver nanometer line |
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| CN105081349A (en) * | 2015-10-09 | 2015-11-25 | 重庆文理学院 | Method for preparing silver nanowires with high length-diameter ratio |
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| CN101934377A (en) * | 2010-09-14 | 2011-01-05 | 浙江大学 | Quick and efficient synthesis method for silver nanowires |
| CN102423808A (en) * | 2011-12-14 | 2012-04-25 | 天津工业大学 | Quick high concentration synthesizing method of silver nanometer line |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511596A (en) * | 2013-09-30 | 2015-04-15 | 中科院广州化学有限公司 | Continuous preparation method and device for nano-silver wire |
| CN106825610A (en) * | 2017-03-24 | 2017-06-13 | 苏州范曼新材料科技有限公司 | A kind of magnanimity preparation method of the ultra-fine nano silver wire of overlength |
| CN108157387B (en) * | 2017-11-27 | 2021-01-05 | 东南大学 | Silver nanowire antibacterial aerogel and preparation method and application thereof |
| CN108157387A (en) * | 2017-11-27 | 2018-06-15 | 东南大学 | A kind of nano silver wire antibacterial aeroge and its preparation method and application |
| CN108262487A (en) * | 2018-01-20 | 2018-07-10 | 浙江大学 | The method that minor diameter nano silver wire is prepared using mixed alcohol |
| CN108441949A (en) * | 2018-04-28 | 2018-08-24 | 无锡英特派金属制品有限公司 | A kind of preparation method of nano-silver thread |
| CN108687358A (en) * | 2018-05-24 | 2018-10-23 | 首都师范大学 | A method of preparing compound silver nano wire |
| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
| CN108436105A (en) * | 2018-06-07 | 2018-08-24 | 乐凯华光印刷科技有限公司 | A kind of overlength nano-silver thread dispersion liquid and preparation method thereof |
| CN108436105B (en) * | 2018-06-07 | 2023-06-20 | 乐凯华光印刷科技有限公司 | Ultra-long nano silver wire dispersion liquid and preparation method thereof |
| CN108971510A (en) * | 2018-07-26 | 2018-12-11 | 深圳清华大学研究院 | Silver nanowires and preparation method thereof, silver nanowires film and laminated film |
| CN109797470A (en) * | 2019-01-22 | 2019-05-24 | 常州天宇宏图电子有限公司 | A kind of preparation method of compliant conductive yarn |
| CN110010876A (en) * | 2019-04-15 | 2019-07-12 | 深圳市高能达电池有限公司 | A kind of controllable method for preparing of lithium sulphur one-shot battery nano anode material |
| CN110170644A (en) * | 2019-05-31 | 2019-08-27 | 陕西科技大学 | A method of by being centrifuged and settling purification silver nanowires |
| CN110170644B (en) * | 2019-05-31 | 2021-08-13 | 陕西科技大学 | Method for purifying silver nanowires through centrifugation and sedimentation |
| CN110586928A (en) * | 2019-09-20 | 2019-12-20 | 华南理工大学 | High-length-diameter-ratio silver nanowire based on one-pot polyol method and preparation method and application thereof |
| CN111036930A (en) * | 2019-12-25 | 2020-04-21 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of silver nanowire block for SERS detection |
| CN111036930B (en) * | 2019-12-25 | 2022-06-24 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of silver nanowire block for SERS detection |
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Application publication date: 20160316 |