CN109954887A - A kind of preparation method of silver nanowires - Google Patents
A kind of preparation method of silver nanowires Download PDFInfo
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- CN109954887A CN109954887A CN201910221198.9A CN201910221198A CN109954887A CN 109954887 A CN109954887 A CN 109954887A CN 201910221198 A CN201910221198 A CN 201910221198A CN 109954887 A CN109954887 A CN 109954887A
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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
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
Abstract
The invention discloses a kind of preparation methods of silver nanowires.The method uses hydro-thermal reaction method, and using gallic acid as reducing agent, the silver chlorate generated by reaction, the silver ion for dissociateing low concentration carrys out the reaction speed of effective control system, is successfully prepared the higher silver nanowires of yield.Preparation method simple process of the invention, step is few, mild condition, easy to operate, and composition is controllable, and the conductive film based on the preparation of silver nanowires made from the method for the present invention shows good electric conductivity, and square resistance is up to 0.05 ± 10% Ω/sq.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, are related to a kind of preparation method of silver nanowires.
Background technique
Metal nanometer line becomes the research of nano material because of its potential application on electronics, optical device and sensor
Hot spot.Wherein one-dimensional metal silver nanowires is due to its unique physical and chemical performance, polarizing device, photonic crystal, catalysis with
And the fields such as biological and chemical sensor have potential application foreground.
Currently, microwave, ultrasonic wave assisted Reduction method, laser radiation method, electrochemical deposition method and hydro-thermal method etc. can succeed
Synthesis of silver nano-wire.United States Patent (USP) US7585349 is disclosed using Pt or Ag as crystal seed, by by silver nitrate and polyvinylpyrrolidine
Silver nanowires is prepared in ethylene glycol, by heating reduction in ketone mixed dissolution, however, the boiling point due to ethylene glycol is lower
(being lower than 200 DEG C), it is unfavorable for the generation of galactic nucleus, causes nano-silver thread yield too low.Contain in nano-silver thread made of the above method
There are by-product nano-Ag particles, separation is complex, causes entire production efficiency to decline, increases production cost pressure.At present
Synthesis high yield, the silver nanowires of high conduction performance are still a problem, hence it is imperative that developing a kind of environmentally protective side
Method can efficiently prepare the nano-silver thread of size uniformity, good conductivity.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of nano-silver thread easy to operate, controllability is strong, this method
The nano-silver thread size uniformity that is prepared and there is good mechanical performance and electric conductivity.
Technical scheme is as follows:
A kind of preparation method of silver nanowires, the specific steps are as follows:
It is 1:4.5~9:3~4:2~6 by the molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid,
First silver nitrate solution and polyvinylpyrrolidonesolution solution are uniformly mixed, then sodium chloride solution is added dropwise, is uniformly mixed
Afterwards, gallic acid is added, uniformly mixed be placed at 120~180 DEG C carries out hydro-thermal reaction, after reaction, water-soluble with ethyl alcohol
Liquid dilution, centrifuge washing, purification obtain silver nanowires.
Preferably, the concentration of the silver nitrate solution is 0.02mol/L.
Preferably, the concentration of the polyvinylpyrrolidonesolution solution is 0.15~0.3mol/L, polyvinylpyrrolidone
Average molecular weight be 58000.
Preferably, the concentration of the sodium chloride solution is 0.06~0.08mol/L, drop rate 5mL/h.
Preferably, the hydro-thermal reaction time is 12~18h.
Preferably, the centrifugation time is 20~30min, and centrifugal rotational speed is 2000~5000r/min.
Compared with prior art, the invention has the following advantages that
The present invention uses simple hydrothermal method, and using gallic acid as reducing agent, the silver chlorate generated by reaction is dissociateed
The silver ion of low concentration carrys out the reaction speed of effective control system, is successfully prepared the higher silver nanowires of yield.The present invention
Simple process, mild condition is easy to operate, and composition is controllable.Gallic acid is widely present in one is plant polyphenol kind compound
The plants such as rheum officinale, eucalyptus, Fructus Corni have a wide range of applications in Green Chemistry field.Yin Na based on the method for the present invention preparation
The conductive film of rice noodles has good electric conductivity, and wherein square resistance is up to 0.05 ± 10% Ω/sq.
Detailed description of the invention
Fig. 1 is silver nanowires SEM figure prepared by embodiment 1.
Fig. 2 is silver nanowires SEM figure prepared by embodiment 2.
Fig. 3 is silver nanowires SEM figure prepared by embodiment 3.
Fig. 4 is silver nanowires SEM figure prepared by embodiment 4.
Fig. 5 is silver nanowires SEM figure prepared by embodiment 5.
Fig. 6 is silver nanowires SEM figure prepared by comparative example 1.
Fig. 7 is silver nanowires SEM figure prepared by comparative example 2.
Fig. 8 is silver nanowires SEM figure prepared by comparative example 3.
Fig. 9 is the silver nanowires XRD diagram prepared based on embodiment 1.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.06mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added
(silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid molar ratio be 1:4.5:3:4), be uniformly mixed be placed on 180
Hydro-thermal reaction 12h at DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains silver nanowires.
Embodiment 2
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.08mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:4.5:4:4), is uniformly mixed
It is placed on hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains Yin Na
Rice noodles.
Embodiment 3
5mL 0.02mol/L silver nitrate solution and 30mL 0.30mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.06mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:9:3:4), after mixing
It is placed in hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains silver nanoparticle
Line.
Embodiment 4
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.08mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:4.5:4:6), is uniformly mixed
It is placed on hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains Yin Na
Rice noodles.
Embodiment 5
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.06mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added,
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:4.5:3:2), is uniformly mixed
It is placed on hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains Yin Na
Rice noodles.
Comparative example 1
5mL 0.02mol/L silver nitrate solution and 30mL 0.45mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.06mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added,
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:13.5:3:4), mixing is equal
Even to be placed on hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains silver
Nano wire.
Comparative example 2
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, 5mL 0.10mol/L sodium chloride solution is added, after being uniformly mixed, gallic acid is added, (the wherein nitric acid
Silver, polyvinylpyrrolidone, sodium chloride, gallic acid molar ratio be 1:4.5:5:4), be uniformly mixed and be placed on 180 DEG C and be lauched
Thermal response 12h, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains silver nanowires.
Comparative example 3
5mL 0.02mol/L silver nitrate solution and 30mL 0.15mol/L polyvinylpyrrolidonesolution solution are stirred
It is even, then 5mL 0.06mol/L sodium chloride solution is slowly injected into 5mL/h flow velocity, after being uniformly mixed, gallic acid is added
(molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid described in wherein is 1:4.5:3:8), is uniformly mixed
It is placed on hydro-thermal reaction 12h at 180 DEG C, to after reaction, be diluted with ethanol water, centrifuge washing, purification obtains Yin Na
Rice noodles.
1 silver nanowires resistive performance test result of table
Fig. 1~5 are respectively the SEM figure of silver nanowires made from Examples 1 to 5, and Fig. 6~8 are respectively that comparative example 1~3 is made
The SEM figure of the silver nanowires obtained.Schemed from SEM as can be seen that controlling silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid
Molar ratio when being 1:4.5~9:3~4:2~6, silver nanowires size uniformity made from each embodiment, pattern is good and yield
Height, and as known from Table 1, the conductive film based on silver nanowires made from each embodiment has good electric conductivity, square resistance
For 0.05 ± 10% Ω/sq.And silver nanowires pattern made from comparative example 1~3 is inhomogenous, granular and line style have, and from
Table 1 is led it is found that the square resistance of the conductive film based on silver nanowires made from comparative example 1~3 is 0.13 Ω/sq or more
It is electrically poor.
Claims (9)
1. a kind of preparation method of silver nanowires, which is characterized in that specific step is as follows:
It is 1:4.5~9:3~4:2~6 by the molar ratio of silver nitrate, polyvinylpyrrolidone, sodium chloride, gallic acid, first will
Silver nitrate solution is uniformly mixed with polyvinylpyrrolidonesolution solution, then sodium chloride solution is added dropwise, and after being uniformly mixed, is added
Enter gallic acid, uniformly mixed be placed at 120~180 DEG C carries out hydro-thermal reaction, after reaction, dilute with ethanol water
It releases, centrifuge washing, purifies, obtain silver nanowires.
2. preparation method according to claim 1, which is characterized in that the concentration of the silver nitrate solution is 0.02mol/
L。
3. preparation method according to claim 1, which is characterized in that the concentration of the polyvinylpyrrolidonesolution solution is
0.15~0.3mol/L.
4. preparation method according to claim 3, which is characterized in that the average molecular weight of the polyvinylpyrrolidone
It is 58000.
5. preparation method according to claim 1, which is characterized in that the concentration of the sodium chloride solution be 0.06~
0.08mol/L。
6. preparation method according to claim 5, which is characterized in that the drop rate of the sodium chloride solution is 5mL/
h。
7. preparation method according to claim 1, which is characterized in that the hydro-thermal reaction time is 12~18h.
8. preparation method according to claim 1, which is characterized in that the centrifugation time is 20~30min.
9. preparation method according to claim 8, which is characterized in that centrifugal rotational speed is 2000~5000r/min.
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Cited By (5)
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| CN110576193A (en) * | 2019-10-29 | 2019-12-17 | 哈尔滨工业大学 | method for preparing superfine silver nanowires by using citrate as reducing agent |
| CN111673092A (en) * | 2020-06-28 | 2020-09-18 | 南京优写智能科技有限公司 | Design synthesis method of ultra-long nano silver wire with uniform diameter |
| CN111922357A (en) * | 2020-08-31 | 2020-11-13 | 华南理工大学 | Nano silver cage and preparation method and application thereof |
| CN113732300A (en) * | 2021-08-31 | 2021-12-03 | 中硕实业(上海)有限公司 | Silver nanowire containing polyphenol compound and preparation method and application thereof |
| CN114985756A (en) * | 2022-05-20 | 2022-09-02 | 苏州大学 | Method for preparing silver nanowires at room temperature based on micromolecular phenolic acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110576193A (en) * | 2019-10-29 | 2019-12-17 | 哈尔滨工业大学 | method for preparing superfine silver nanowires by using citrate as reducing agent |
| CN111673092A (en) * | 2020-06-28 | 2020-09-18 | 南京优写智能科技有限公司 | Design synthesis method of ultra-long nano silver wire with uniform diameter |
| CN111922357A (en) * | 2020-08-31 | 2020-11-13 | 华南理工大学 | Nano silver cage and preparation method and application thereof |
| CN111922357B (en) * | 2020-08-31 | 2022-02-15 | 华南理工大学 | Nano silver cage and preparation method and application thereof |
| CN113732300A (en) * | 2021-08-31 | 2021-12-03 | 中硕实业(上海)有限公司 | Silver nanowire containing polyphenol compound and preparation method and application thereof |
| CN113732300B (en) * | 2021-08-31 | 2023-10-17 | 中硕实业(上海)有限公司 | Silver nanowire containing polyphenol compound and preparation method and application thereof |
| CN114985756A (en) * | 2022-05-20 | 2022-09-02 | 苏州大学 | Method for preparing silver nanowires at room temperature based on micromolecular phenolic acid |
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Application publication date: 20190702 |