CN104999089B - The preparation method of nano silver wire in a kind of hydrophobic phase - Google Patents
The preparation method of nano silver wire in a kind of hydrophobic phase Download PDFInfo
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- CN104999089B CN104999089B CN201510414352.6A CN201510414352A CN104999089B CN 104999089 B CN104999089 B CN 104999089B CN 201510414352 A CN201510414352 A CN 201510414352A CN 104999089 B CN104999089 B CN 104999089B
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Abstract
The present invention discloses a kind of preparation method of nano silver wire in hydrophobic phase, and step is：At room temperature, silver bromide, mantoquita and solvent are mixed, mixed liquor is fully dissolved to obtain in stirring, mixed liquor is warming up to 100~267 DEG C of 1~24h of reaction, be subsequently cooled to room temperature and obtain reaction solution, reaction solution washing is filtered, dries, obtain nano silver wire.Preparation method of the present invention, technique is simple, it is only necessary to three kinds of raw material mixing, heating response, without operating methods such as concussion, ultrasounds.The nano silver wire surface prepared has hydrophobic grouping, can be effectively dispersed in hydrophobic solvent and material, expands the application field of nano silver wire.
Description
Technical field
The invention belongs to nano silver wire field of material technology, it is related to a kind of preparation method of nano silver wire in hydrophobic phase.
Background technology
Nano silver wire is a kind of new 1-dimention nano precious metal material, compared to the nano material of shape of particle, Yin Na
Rice noodles have that specific surface area is big, surface-active is high, electric conductivity is excellent, the characteristic such as catalytic performance is excellent, also with unique table
Face plasma resonance effect.At present, this material is widely used to transparent conductive electrode, and flexible display screen, surface enhanced is drawn
The field such as graceful technology, biomarker, imaging and Measurement for Biotechnique, function nano device, by extensive in worldwide
Concern.
The technology of preparing of current nano silver wire mainly includes template, crystal seed method, polyol reduction method, hydro-thermal method etc..Mould
Plate method is usually using the material not reacted with silver（For example, alundum (Al2O3) etc.）The shape of silver nano material is controlled as masterplate
Shape.These methods are prepared in hydrophily system, and the nano silver wire prepared, which exists, uniformly to be divided in hydrophobic phase
Scattered shortcoming, limits the use of nano silver wire.
The content of the invention
For above shortcomings in the prior art, the invention provides a kind of preparation side of nano silver wire in hydrophobic phase
Method, is prepared by the method for the present invention obtained nano silver wire, effectively overcomes nano silver wire and is not can be uniformly dispersed in hydrophobic phase
Shortcoming.
To achieve these goals, technical solution of the present invention is：
The preparation method of nano silver wire in a kind of hydrophobic phase, it is characterised in that：At room temperature, by silver bromide, mantoquita and solvent
Mixed liquor is fully dissolved to obtain in mixing, stirring, and mixed liquor is warming up into 100~267 DEG C of 1~24h of reaction, room temperature is subsequently cooled to and obtains
Reaction solution, reaction solution washing, is filtered, and is dried, is obtained nano silver wire.
Described mantoquita is copper chloride, copper sulphate, copper nitrate, cupric oxide, basic copper carbonate or basic copper sulfate, preferably chlorine
Change copper.
Described solvent is oleyl amine, oleic acid, octadecylene or cetylamine, preferably oleyl amine.
The mass ratio of described silver bromide and mantoquita, solvent is 1:（0.001~1）:（10~1000）, preferably 1:（0.005
~0.1）:（50~200）, most preferably 1:0.01:100.
During above-mentioned reaction solution washing, detergent is organic solvent, preferably hexamethylene.
Preferably 160 DEG C of above-mentioned reaction temperature.
Preferably 6 h of above-mentioned reaction time.
The preparation method of nano silver wire is a kind of brand-new preparation method in the hydrophobic phase that the present invention is provided, with silver before
The hydrophily system that the preparation of nano wire is used is compared, although be all that silver salt is reduced using reducing agent, but the present invention is adopted
Hydrophobic solvent, in preparation process, hydrophobic grouping, which can be wrapped in nano silver wire surface, to be played a part of scattered and modifies,
So that the nano silver wire prepared is when in use, preferably it can be dispersed in hydrophobic solvent.
The preparation method of nano silver wire, has the beneficial effect that compared with prior art in hydrophobic phase of the present invention：Realize first
The preparation of nano silver wire in hydrophobic phase, technique is simple, it is only necessary to three kinds of raw material mixing, heating response, without concussion, ultrasound
Etc. operating method.The nano silver wire surface prepared has hydrophobic grouping, can be effectively in hydrophobic solvent and material
It is even scattered, expand the application field of nano silver wire.
Brief description of the drawings
Fig. 1 is the SEM of the nano silver wire of embodiment 1（SEM）Figure；
Fig. 2 is the SEM of the nano silver wire of embodiment 2（SEM）Figure；
Fig. 3 is the SEM of the nano silver wire of embodiment 3（SEM）Figure；
Fig. 4 is the SEM of the nano silver wire of embodiment 4（SEM）Figure；
Fig. 5 is the SEM of the nano silver wire of embodiment 5（SEM）Figure；
Fig. 6 is the SEM of the nano silver wire of embodiment 6（SEM）Figure；
Fig. 7 is the SEM of the nano silver wire of embodiment 7（SEM）Figure；
Fig. 8 is the SEM of the nano silver wire of embodiment 8（SEM）Figure；
Fig. 9 is the SEM of the nano silver wire of embodiment 9（SEM）Figure；
Figure 10 is the nano silver wire SEM of embodiment 10（SEM）Figure；
Figure 11 is the nano silver wire SEM of embodiment 11（SEM）Figure；
Figure 12 is the nano silver wire SEM of embodiment 12（SEM）Figure.
Embodiment
With reference to specific embodiment, the present invention will be described in detail, and following embodiments are merely to explain this hair
It is bright, its content is not defined.
Embodiment 1
At room temperature, 300 mg silver bromides, 3 mg copper chlorides and 30 g oleyl amines are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 160 DEG C of reaction 6h, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 1）, the nm of average diameter 60,10 μm of average length.
Embodiment 2
At room temperature, 300 mg silver bromides, 3 mg copper sulphate and 30 g oleyl amines are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 160 DEG C of 6 h of reaction, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 2）, the nm of average diameter 55,15 μm of average length.
Embodiment 3
At room temperature, 300 mg silver bromides, 3 mg cupric oxide and 30 g oleyl amines are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 160 DEG C of 6 h of reaction, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 3）, the nm of average diameter 67,10 μm of average length.
Embodiment 4
At room temperature, 300 mg silver bromides, 3 mg copper chlorides and 30 g oleic acid are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 160 DEG C of 6 h of reaction, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 4）, the nm of average diameter 60,15 μm of average length.
Embodiment 5
At room temperature, 300mg silver bromides, 3mg copper chlorides and 30 g octadecylenes are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 130 DEG C of 4 h of reaction, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 5）, the nm of average diameter 60,14 μm of average length.
Embodiment 6
At room temperature, 300 mg silver bromides, 3 mg copper nitrates and 30 g cetylamines are mixed, stirring is fully dissolved and must mixed
Liquid, is warming up to 200 DEG C of 10 h of reaction by mixed liquor, is subsequently cooled to room temperature and obtains reaction solution, reaction solution is washed with hexamethylene, mistake
Filter, dries, obtains nano silver wire.Nano silver wire made from the present embodiment（See Fig. 6）, the nm of average diameter 62,20 μm of average length.
Embodiment 7
At room temperature, 300 mg silver bromides, 3 mg basic copper carbonates and 30 g oleyl amines are mixed, stirring is fully dissolved and must mixed
Liquid, is warming up to 160 DEG C of 20 h of reaction by mixed liquor, is subsequently cooled to room temperature and obtains reaction solution, reaction solution is washed with hexamethylene, mistake
Filter, dries, obtains nano silver wire.Nano silver wire made from the present embodiment（See Fig. 7）, the nm of average diameter 65,18 μm of average length.
Embodiment 8
At room temperature, 300 mg silver bromides, 3 mg basic copper sulfates and 30 g oleyl amines are mixed, stirring is fully dissolved and must mixed
Liquid, is warming up to 230 DEG C of 12 h of reaction by mixed liquor, is subsequently cooled to room temperature and obtains reaction solution, reaction solution is washed with hexamethylene, mistake
Filter, dries, obtains nano silver wire.Nano silver wire made from the present embodiment（See Fig. 8）, the nm of average diameter 54, the μ of average length 16
m。
Embodiment 9
At room temperature, 300 mg silver bromides, 0.3 mg copper chlorides and 3 g oleyl amines are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 267 DEG C of reaction 24h, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with hexamethylene, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Fig. 9）, the nm of average diameter 58,20 μm of average length.
Embodiment 10
At room temperature, 300 mg silver bromides, 300 mg copper chlorides and 300 g oleyl amines are mixed, stirring is fully dissolved and must mixed
Liquid, is warming up to 100 DEG C of 1 h of reaction by mixed liquor, is subsequently cooled to room temperature and obtains reaction solution, reaction solution is washed with hexamethylene, filter,
Dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Figure 10）, the nm of average diameter 60,20 μm of average length.
Embodiment 11
At room temperature, 300 mg silver bromides, 1.5 mg copper chlorides and 15 g oleyl amines are mixed, stirring is fully dissolved and must mixed
Liquid, is warming up to 100 DEG C of 6 h of reaction by mixed liquor, is subsequently cooled to room temperature and obtains reaction solution, reaction solution is washed with ethanol, filter, do
It is dry, obtain nano silver wire.Nano silver wire made from the present embodiment（See Figure 11）, the nm of average diameter 60,25 μm of average length.
Embodiment 12
At room temperature, 300 mg silver bromides, 30 mg copper chlorides and 60 g oleyl amines are mixed, mixed liquor is fully dissolved to obtain in stirring,
Mixed liquor is warming up to 267 DEG C of 6 h of reaction, room temperature is subsequently cooled to and obtains reaction solution, reaction solution is washed with methanol, filter, dry,
Obtain nano silver wire.Nano silver wire made from the present embodiment（See Figure 12）, the nm of average diameter 62,18 μm of average length.
Claims (9)
1. the preparation method of nano silver wire in a kind of hydrophobic phase, it is characterised in that：At room temperature, silver bromide, mantoquita and solvent are mixed
Close, mixed liquor is fully dissolved to obtain in stirring, mixed liquor is warming up to 100~267 DEG C of 1~24 h of reaction, room temperature is subsequently cooled to and obtains
Reaction solution, reaction solution washing, is filtered, and is dried, is obtained nano silver wire；
Described solvent is oleyl amine, oleic acid, octadecylene or cetylamine.
2. preparation method according to claim 1, it is characterised in that：Described mantoquita is copper chloride, copper sulphate, nitric acid
Copper, cupric oxide, basic copper carbonate or basic copper sulfate.
3. preparation method according to claim 2, it is characterised in that：Described mantoquita is copper chloride.
4. preparation method according to claim 1, it is characterised in that：Described solvent is oleyl amine.
5. preparation method according to claim 1, it is characterised in that：Described silver bromide and mantoquita, the mass ratio of solvent
For 1:（0.001~1）:（10~1000）.
6. preparation method according to claim 5, it is characterised in that：Described silver bromide and mantoquita, the mass ratio of solvent
For 1:（0.005~0.1）:（50~200）.
7. preparation method according to claim 6, it is characterised in that：Described silver bromide and mantoquita, the mass ratio of solvent
For 1:0.01:100.
8. preparation method according to claim 1, it is characterised in that：During above-mentioned reaction solution washing, detergent is organic molten
Agent.
9. preparation method according to claim 1, it is characterised in that：Reaction temperature is 160 DEG C, and the reaction time is 6h.
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Citations (4)
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|---|---|---|---|---|
| CN102744421A (en) * | 2012-07-16 | 2012-10-24 | 浙江师范大学 | Method for preparing large-scale Ag nanowires in aqueous solution |
| CN103357889A (en) * | 2013-07-15 | 2013-10-23 | 中南大学 | Preparation method and application of silver nanowire with high length-width ratio |
| CN104607656A (en) * | 2015-03-06 | 2015-05-13 | 中国科学院上海硅酸盐研究所 | Super-long silver nanowire and preparation method thereof |
| CN104759634A (en) * | 2015-03-04 | 2015-07-08 | 江苏大学 | Preparation method for superfine silver nanowire |
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| US20140123808A1 (en) * | 2012-11-08 | 2014-05-08 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102744421A (en) * | 2012-07-16 | 2012-10-24 | 浙江师范大学 | Method for preparing large-scale Ag nanowires in aqueous solution |
| CN103357889A (en) * | 2013-07-15 | 2013-10-23 | 中南大学 | Preparation method and application of silver nanowire with high length-width ratio |
| CN104759634A (en) * | 2015-03-04 | 2015-07-08 | 江苏大学 | Preparation method for superfine silver nanowire |
| CN104607656A (en) * | 2015-03-06 | 2015-05-13 | 中国科学院上海硅酸盐研究所 | Super-long silver nanowire and preparation method thereof |
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Address after: 272000 A5 building, Chongwen road research and production base, Jining hi tech Industrial Development Zone, Shandong, China Patentee after: Shandong lett Nano Technology Co., Ltd. Address before: 272000 A5 building, Chongwen road research and production base, Jining hi tech Industrial Development Zone, Shandong, China Patentee before: Jining Leader Nano Technology Co., Ltd. |