CN104625087A - Method for hydrothermally manufacturing silver nanowires - Google Patents
Method for hydrothermally manufacturing silver nanowires Download PDFInfo
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- CN104625087A CN104625087A CN201510090816.2A CN201510090816A CN104625087A CN 104625087 A CN104625087 A CN 104625087A CN 201510090816 A CN201510090816 A CN 201510090816A CN 104625087 A CN104625087 A CN 104625087A
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Abstract
The invention provides a method for hydrothermally manufacturing silver nanowires. The method is characterized by including: at room temperature, mixing inorganic silver salt, quaternary ammonium salt, reductant and water; stirring for sufficient dissolving to obtain mixed liquid; heating the mixed liquid in a hydrothermal kettle to be 80 DEG C-150 DEG C for 20min-10h; cooling the mixed liquid to be room temperature to obtain reaction liquid; using water to wash the reaction liquid to obtain the silver nanowires. Compared with the prior art, the method has the advantages that the method is simple in process, low in reaction temperature, short in time, high in product concentration and low in cost; the water is used as solvent, so that the method is safe, environment friendly and little in pollution; product aggregation is avoided after surfactant is added, so that the surfactant can be uniformly dispersed in the solvent to form stable dispersion liquid.
Description
Technical field
The invention belongs to nano silver wire field of material technology, relate to a kind of method that hydro-thermal prepares nano silver wire.
Background technology
Nano silver wire is a kind of novel 1-dimention nano precious metal material, compared to the nano material of shape of particle, nano silver wire has that specific area is large, surface-active is high, electric conductivity is excellent, the characteristics such as catalytic performance is excellent, also has unique surface plasma resonance effect.At present, this material is widely used in transparency conductive electrode, flexible display screen, and surface enhanced Raman technique, biomarker, imaging and the field such as Measurement for Biotechnique, function nano device, be subject to the extensive concern in worldwide.
The technology of preparing of current nano silver wire mainly comprises template, crystal seed method, polyol reduction method, hydro-thermal method etc.Template uses the material (such as, alundum (Al2O3) etc.) do not reacted with silver to control the shape of silver nano material as masterplate usually.Although this method can regulate and control the pattern of nano silver wire very well, but preparation terminates rear and the post-processing operation of carrying out (such as, remove template) more loaded down with trivial details, and the nano silver wire amount that masterplate method is produced is little, in the problem facing large-scale production, there is cost and technical dual restriction; Crystal seed method at room temperature successfully can prepare nano silver wire, but needs to introduce crystal seed, thus causes preparation process relatively loaded down with trivial details.Polyol reduction method is by high temperature utilizing the predecessor of polyol process silver to prepare nano silver wire material.This method may be used for suitability for industrialized production, but is the use of the much higher first alcohol of viscosity as solvent, and it is comparatively loaded down with trivial details that preparation terminates rear carried out post-processing operation (washing, centrifugal etc.), and waste liquid pollutes the environment.
In the hydro-thermal method reported, the seminar of professor Qian Yitai of China Science & Technology University leader employs the 180 DEG C of reactions 18 hours in water heating kettle of silver chlorate, glucose and water, obtain the nano silver wire of diameter 100 nm length up to 500 μm (
chem. Eur. J.2004,11,160-163).The weak point of this method is that reaction temperature is higher, and the time is longer, and lack surfactant, product be difficult to formed in a solvent dispersed.
Summary of the invention
In order to overcome the defect existed in above method, the invention provides a kind of method that hydro-thermal prepares nano silver wire.
The present invention is realized by following measures:
Under room temperature, inorganic silver salt, quaternary ammonium salt, reducing agent and water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 80 ~ 150 DEG C of reaction 20min ~ 10h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.
Described inorganic silver salt is one or more in trifluoroacetic acid silver, silver nitrate, silver acetate and silver chlorate, preferred silver nitrate.
Described quaternary ammonium salt is in one in hexadecyltrimethylammonium chloride, DTAC and OTAC etc. or several, preferred hexadecyltrimethylammonium chloride.
Described reducing agent is one or more of glucose, ascorbic acid and formaldehyde, preferred ascorbic acid.
Mol ratio >=the 1:1 of described quaternary ammonium salt and inorganic silver salt, preferred 3:1.
Mol ratio >=the 2:1 of described reducing agent and inorganic silver salt, preferred 2:1.
Mass ratio >=the 140:1 of described water and inorganic silver salt, preferred 140:1.
Described reaction temperature preferably 130 DEG C; Preferred 2h of described reaction time.
Hydro-thermal of the present invention prepares the method for nano silver wire, and compared with prior art beneficial effect is:
(1) technique is simple, only needs, by three kinds of raw material mixing, to be placed in reactor and to react, without the need to reaction means such as stirring, shake, be ultrasonic;
(2) use water as solvent, safety and environmental protection, pollutes little;
(3) cost is low, and reaction temperature is low, and the reaction time is short, and production concentration is large, reduces production cost.
Accompanying drawing explanation
Fig. 1 is low power SEM (SEM) figure of embodiment 1 nano silver wire;
Fig. 2 is high power SEM (SEM) figure of embodiment 1 nano silver wire.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail, and following embodiment is only to explain the present invention, does not limit its content.
Embodiment 1
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 100nm, average length 30 μm.
Embodiment 2
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 20min, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 95nm, average length 30 μm.
Embodiment 3
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 10h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is centrifugal, and precipitate washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 110nm, average length 30 μm.
Embodiment 4
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 80 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 110nm, average length 40 μm.
Embodiment 5
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 150 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 90nm, average length 40 μm.
Embodiment 6
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g glucose and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, filtered by reactant liquor sand core funnel, filter cake washes with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 110nm, average length 30 μm.
Embodiment 7
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.08g formaldehyde and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 120nm, average length 35 μm.
Embodiment 8
Under room temperature, 0.21g silver chlorate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 110nm, average length 50 μm.
Embodiment 9
Under room temperature, by 0.33g trifluoroacetic acid silver, the mixing of 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 85nm, average length 50 μm.
Embodiment 10
Under room temperature, 0.25g silver nitrate, 1.5g DTAC, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 100nm, average length 35 μm.
Embodiment 11
Under room temperature, 0.25g silver nitrate, 2.1g OTAC, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 100nm, average length 40 μm.
Embodiment 12
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 2.0g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 90nm, average length 40 μm.
Embodiment 13
Under room temperature, 0.25g silver nitrate, 20.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 35g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 80nm, average length 50 μm.
Embodiment 14
Under room temperature, 0.25g silver nitrate, 2.0g hexadecyltrimethylammonium chloride, 0.5g ascorbic acid and 100g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 130 DEG C of reaction 2h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.The nano silver wire that the present embodiment is obtained, average diameter 100nm, average length 30 μm.
Comparative example
Under room temperature, 17mg silver nitrate, 5.8mg sodium chloride, 36mg glucose and 30g water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 180 DEG C of reaction 18h, is then cooled to room temperature, by precipitate washed with water, obtains nano silver wire.The nano silver wire that this comparative example is obtained, average diameter 100nm, average length 500 μm.
From embodiment and comparative example, the inventive method compared with prior art technique is simple, reaction temperature is low, time is short, 80 ~ 150 DEG C are reacted about 2h and all can reach good effect, production concentration is large, identical reactant liquor volume comparative example can only produce the nano silver wire of 10mg, and the present invention can produce the nano silver wire of 160mg, uses water as solvent, safety and environmental protection, pollute little, cost is low, containing surfactant in reactant liquor, product soilless sticking phenomenon, dispersedly can form stable dispersion liquid in a solvent.
Claims (10)
1. a hydro-thermal prepares the method for nano silver wire, it is characterized in that: under room temperature, inorganic silver salt, quaternary ammonium salt, reducing agent and water are mixed, stir and fully dissolve to obtain mixed liquor, mixed liquor is warming up in water heating kettle 80 ~ 150 DEG C of reaction 20min ~ 10h, then be cooled to room temperature and obtain reactant liquor, reactant liquor is washed with water, obtains nano silver wire.
2. hydro-thermal according to claim 1 prepares the method for nano silver wire, it is characterized in that: described inorganic silver salt is one or more in trifluoroacetic acid silver, silver nitrate, silver acetate and silver chlorate.
3. hydro-thermal according to claim 2 prepares the method for nano silver wire, it is characterized in that: described inorganic silver salt is silver nitrate.
4. hydro-thermal according to claim 1 prepares the method for nano silver wire, it is characterized in that: described quaternary ammonium salt is in one in hexadecyltrimethylammonium chloride, DTAC and OTAC etc. or several.
5. hydro-thermal according to claim 4 prepares the method for nano silver wire, it is characterized in that: described quaternary ammonium salt is hexadecyltrimethylammonium chloride.
6. hydro-thermal according to claim 1 prepares the method for nano silver wire, it is characterized in that: described reducing agent is one or more of glucose, ascorbic acid and formaldehyde.
7. hydro-thermal according to claim 6 prepares the method for nano silver wire, it is characterized in that: described reducing agent is ascorbic acid.
8. hydro-thermal according to claim 1 prepares the method for nano silver wire, it is characterized in that: the mol ratio >=1:1 of described quaternary ammonium salt and inorganic silver salt, mol ratio >=the 2:1 of described reducing agent and inorganic silver salt, the mass ratio >=140:1 of described water and inorganic silver salt.
9. hydro-thermal according to claim 8 prepares the method for nano silver wire, it is characterized in that: the mol ratio of described quaternary ammonium salt and inorganic silver salt is 3:1, the mol ratio of described reducing agent and inorganic silver salt is 2:1, and the mass ratio of described water and inorganic silver salt is 140:1.
10. hydro-thermal according to claim 1 prepares the method for nano silver wire, it is characterized in that: described reaction temperature is 130 DEG C, and the described reaction time is 2h.
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Cited By (7)
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| CN104874813A (en) * | 2015-05-28 | 2015-09-02 | 东华大学 | Preparation method of ultrathin super-long silver nanowire |
| CN106041115A (en) * | 2016-05-26 | 2016-10-26 | 华南理工大学 | Sodium alga acid/silver nanowire sol and preparation method thereof |
| CN107584137A (en) * | 2017-09-14 | 2018-01-16 | 浙江大学 | A kind of method that solwution method prepares metallic cobalt |
| CN108994315A (en) * | 2018-09-18 | 2018-12-14 | 合肥学院 | A method of silver nanowires material is prepared by template and reducing agent of carragheen |
| CN109890541A (en) * | 2016-10-25 | 2019-06-14 | 同和电子科技有限公司 | The manufacturing method of silver nanowires |
| CN110369732A (en) * | 2018-04-12 | 2019-10-25 | 北京化工大学 | A kind of low temperature preparation method of silver nanowires |
| CN111299604A (en) * | 2020-03-02 | 2020-06-19 | 华南理工大学 | Room-temperature coated ultra-long silver nanowire for flexible substrate and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104874813A (en) * | 2015-05-28 | 2015-09-02 | 东华大学 | Preparation method of ultrathin super-long silver nanowire |
| CN106041115A (en) * | 2016-05-26 | 2016-10-26 | 华南理工大学 | Sodium alga acid/silver nanowire sol and preparation method thereof |
| CN106041115B (en) * | 2016-05-26 | 2019-01-18 | 华南理工大学 | A kind of sodium alginate/silver nanowires colloidal sol and preparation method thereof |
| CN109890541A (en) * | 2016-10-25 | 2019-06-14 | 同和电子科技有限公司 | The manufacturing method of silver nanowires |
| CN107584137A (en) * | 2017-09-14 | 2018-01-16 | 浙江大学 | A kind of method that solwution method prepares metallic cobalt |
| CN110369732A (en) * | 2018-04-12 | 2019-10-25 | 北京化工大学 | A kind of low temperature preparation method of silver nanowires |
| CN108994315A (en) * | 2018-09-18 | 2018-12-14 | 合肥学院 | A method of silver nanowires material is prepared by template and reducing agent of carragheen |
| CN108994315B (en) * | 2018-09-18 | 2021-11-09 | 合肥学院 | Method for preparing silver nanowire material by using carrageenan as template and reducing agent |
| CN111299604A (en) * | 2020-03-02 | 2020-06-19 | 华南理工大学 | Room-temperature coated ultra-long silver nanowire for flexible substrate and preparation method thereof |
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