CN108555310A - A kind of preparation method of nano silver wire suspension solution - Google Patents
A kind of preparation method of nano silver wire suspension solution Download PDFInfo
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- CN108555310A CN108555310A CN201810301344.4A CN201810301344A CN108555310A CN 108555310 A CN108555310 A CN 108555310A CN 201810301344 A CN201810301344 A CN 201810301344A CN 108555310 A CN108555310 A CN 108555310A
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- nano
- suspension solution
- wire suspension
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- silver
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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
- 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
- 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 method of nano silver wire suspension solution, nano silver wire suspension solution is mixed by nano-silver thread and lower alcohol, and the nano-silver thread is prepared by method comprising the following steps:S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;S20, at 20 35 DEG C, water soluble silver salt is gradually added dropwise in the mixed liquor;After being added dropwise, 30 60min of ultrasonic disperse is warming up to 120 150 DEG C of 20 50min of reaction, obtains mixture;S30, the mixture is collected by centrifugation to precipitation, the nano-silver thread is obtained after washing is dry.Nano-silver thread Production Time is short, and dimensional discrepancy is smaller, is suitble to large-scale production.Ductility of the nano silver wire suspension solution on basilar memebrane made from nano-silver thread and lower alcohol is good, convenient for coating.
Description
Technical field
The present invention relates to the preparation methods of the nano metal line for flexible transparent conductive film, more particularly, to one
The preparation method of kind nano silver wire suspension solution.
Background technology
Transparent conductive film is widely used in the light such as flat-panel monitor, solar cell, optical communication equipment, solid-state lighting
Electrical domain.Transparent conductive film most important application at present or on touch screen technology, the use of touch screen is in mobile phone, flat
In terms of plate, notebook, mobile terminal, current commercialized transparent conductive film is tin-doped indium oxide(ITO)Film, although ITO has
There are higher electric conductivity and translucency, but indium resource allowable exploitation is limited, the rise of indium price has driven the rise of ITO prices,
The ductility of ITO is insufficient simultaneously, cannot be satisfied the growth requirement of flexible electronic technology.The width of nano silver wire only has hairline
A ten thousandth, sufficiently fine benefit exactly can keep transparent on film, and graphene is the material of monatomic thickness, is in the world
Most thin two-dimensional material, they are all the preferable materials of conductive capability.It is nano silver wire graphene is compound and be transferred to flexible base
On bottom, so that it may with formed one it is transparent, conductive and have film flexible, it is this be based on nano silver wire/graphene composite transparent
Conductive film can be widely applied for the photoelectric fields such as flat-panel monitor, solar cell, optical communication equipment, solid-state lighting.
Nano-silver thread preparation process takes longer in nano silver wire suspension solution in the prior art, and dimensional discrepancy is larger,
Be not suitable for large-scale production.
Invention content
The present invention is directed to solve one of above-mentioned technical problem at least to a certain extent.For this purpose, the present invention provides one kind
The preparation method of nano silver wire suspension solution.
In order to solve the above technical problems, the present invention uses following technical scheme:
The preparation method of nano silver wire suspension solution according to the ... of the embodiment of the present invention, the nano silver wire suspension solution is by nano silver
Line and lower alcohol mix, and the nano-silver thread is prepared by method comprising the following steps:
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
At S20,20-35 DEG C, water soluble silver salt is gradually added dropwise in the mixed liquor;After being added dropwise, ultrasonic disperse 30-
60min is warming up to 120-150 DEG C of reaction 20-50min, obtains mixture;
S30, the mixture is collected by centrifugation to precipitation, the nano-silver thread is obtained after washing is dry.
Further, it is 1 that the water soluble silver salt and the metal ion halide, which obtain molar ratio,:1-100:1.
Further, in step S10, the content of the water soluble silver salt is 20-50wt%, the water-soluble polymer
Content is 0.5-5%, and the content of the surface-active is 0.001-1%.
Further, the molecular weight of the water-soluble polymer is 10,000-1,000,000.
Further, it is total to be selected from polyacrylic acid, polyvinylpyrrolidone, polyacrylamide machine for the water-soluble polymer
At least one of polymers.
Further, the surfactant is cationic surfactant.
Further, the water soluble silver salt is silver nitrate or silver acetate.
Further, the metal ion halide is selected from sodium chloride, sodium bromide, potassium bromide, potassium chloride, magnesium chloride, chlorine
Change at least one of zinc and copper chloride.
Further, the lower alcohol is selected from least one of methanol, ethyl alcohol, isopropanol or ethylene glycol.
The preparation method of nano silver wire suspension solution according to the ... of the embodiment of the present invention, gained nano-silver thread Production Time is short,
Dimensional discrepancy is smaller, is suitble to large-scale production.Nano silver wire suspension solution is on basilar memebrane made from nano-silver thread and lower alcohol
Ductility it is good, convenient for coating.
Specific implementation mode
The embodiment of the present invention is described below in detail, in which the same or similar labels are throughly indicated same or like
Element or element with the same or similar functions.It is exemplary below with reference to the embodiment of embodiment description, purport
For explaining the present invention, and it is not considered as limiting the invention.
The preparation method of nano silver wire suspension solution according to the ... of the embodiment of the present invention, nano silver wire suspension solution is by nano silver
Line and lower alcohol mix, and nano-silver thread is prepared by method comprising the following steps:
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
At S20,20-35 DEG C, water soluble silver salt is gradually added dropwise in mixed liquor;After being added dropwise, ultrasonic disperse 30-60min,
It is warming up to 120-150 DEG C of reaction 20-50min, obtains mixture;
S30, mixture is collected by centrifugation to precipitation, nano-silver thread is obtained after washing is dry.
According to an optional embodiment of the invention, it is 1 that water soluble silver salt and metal ion halide, which obtain molar ratio,:1-
100:1。
In an optional realization method of the invention, in step S10, the content of water soluble silver salt is 20-50wt%, water
The content of soluble polymer is 0.5-5%, and the content of surface-active is 0.001-1%.
In another optional realization method of the invention, the molecular weight of water-soluble polymer is 10,000-1,000,
000。
In another optional realization method of the invention, water-soluble polymer is selected from polyacrylic acid, polyvinylpyrrolidine
At least one of ketone, polyacrylamide machine copolymer.
In another optional realization method of the invention, surfactant is cationic surfactant.Preferably, positive
Ionic surface active agent is selected from:Quaternary ammonium salt, pyridine derivate, betanin derivative, imidazoles with amide groups and ester group
At least one of derivative and quinoline.According to some comparative examples, in other steps and the identical feelings of agents useful for same
Under condition, anion surfactant is used only or amphoteric surfactant replaces cationic surfactant, can cause obtained
The dimensional discrepancy of nano-silver thread is larger, and quality is opposite poor using only cationic surfactant.
In an optional realization method of the invention, water soluble silver salt is silver nitrate or silver acetate.
In another optional realization method of the invention, metal ion halide is selected from sodium chloride, sodium bromide, bromination
At least one of potassium, potassium chloride, magnesium chloride, zinc chloride and copper chloride.
In an optional realization method of the invention, lower alcohol in methanol, ethyl alcohol, isopropanol or ethylene glycol extremely
Few one kind.
A diameter of 20-50nm of nano-silver thread obtained by the embodiment of the present invention, length 5-40nm, nano silver wire are suspended
A concentration of 8-20mg/mL of solution.Preferably, a diameter of 25-35nm of nano-silver thread, 10-20 μm of length, nano silver wire hangs
A concentration of 10mg/mL alcohol suspensions of turbid solution.
Technical solution of the present invention is further explained with reference to specific embodiment, it is to be understood that the present invention is simultaneously
It is not limited to following embodiment.
Embodiment 1
It is prepared by the following method nano-silver thread(Used raw material maximum weight is no more than 20g):
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
S20, at 25 DEG C, water soluble silver salt is gradually added dropwise in mixed liquor;After being added dropwise, ultrasonic disperse 35min is warming up to
130 DEG C of reaction 50min, obtain mixture;
S30, mixture is collected by centrifugation to precipitation, nano-silver thread is obtained after washing is dry.A diameter of 25nm of gained nano-silver thread,
The size uniformity degree of 15 μm of length, each nano-silver thread is good, and size difference is smaller.
Nano-silver thread obtained is put into ethyl alcohol and is stirred, nano silver wire suspension solution is obtained.
Embodiment 2
It is prepared by the following method nano-silver thread(Used raw material maximum weight is no more than 50g):
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
S20, at 25 DEG C, water soluble silver salt is gradually added dropwise in mixed liquor;After being added dropwise, ultrasonic disperse 50min is warming up to
130 DEG C of reaction 20min, obtain mixture;
S30, mixture is collected by centrifugation to precipitation, nano-silver thread is obtained after washing is dry.A diameter of 30nm of gained nano-silver thread,
The size uniformity degree of 18 μm of length, each nano-silver thread is good, and size difference is smaller.
Nano-silver thread obtained is put into ethyl alcohol and is stirred, nano silver wire suspension solution is obtained.
Embodiment 3
It is prepared by the following method nano-silver thread(Used raw material minimum weight is not less than 20kg):
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
S20, at 2 DEG C, water soluble silver salt is gradually added dropwise in mixed liquor;After being added dropwise, ultrasonic disperse 35min is warming up to
130 DEG C of reaction 50min, obtain mixture;
S30, mixture is collected by centrifugation to precipitation, nano-silver thread is obtained after washing is dry.A diameter of 25nm of gained nano-silver thread,
The size uniformity degree of 15 μm of length, each nano-silver thread is good similar to Example 1, and size difference is smaller.
Nano-silver thread obtained is put into ethyl alcohol and is stirred, nano silver wire suspension solution is obtained.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiments or example in can be combined in any suitable manner.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case of can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (9)
1. a kind of preparation method of nano silver wire suspension solution, which is characterized in that the nano silver wire suspension solution is by nano silver
Line and lower alcohol mix, and the nano-silver thread is prepared by method comprising the following steps:
S10, metal ion halide, surfactant and water-soluble polymer are dissolved in water uniformly mixed, obtain mixed liquor;
At S20,20-35 DEG C, water soluble silver salt is gradually added dropwise in the mixed liquor;After being added dropwise, ultrasonic disperse 30-
60min is warming up to 120-150 DEG C of reaction 20-50min, obtains mixture;
S30, the mixture is collected by centrifugation to precipitation, the nano-silver thread is obtained after washing is dry.
2. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the water soluble silver salt
It is 1 to obtain molar ratio with the metal ion halide:1-100:1.
3. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that described in step S10
The content of water soluble silver salt is 20-50wt%, and the content of the water-soluble polymer is 0.5-5%, the content of the surface-active
For 0.001-1%.
4. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the water-soluble polymeric
The molecular weight of object is 10,000-1,000,000.
5. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the water-soluble polymeric
Object is selected from least one of polyacrylic acid, polyvinylpyrrolidone, polyacrylamide machine copolymer.
6. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the surfactant
For cationic surfactant.
7. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the water soluble silver salt
For silver nitrate or silver acetate.
8. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the metal ion halogen
Compound is selected from least one of sodium chloride, sodium bromide, potassium bromide, potassium chloride, magnesium chloride, zinc chloride and copper chloride.
9. the preparation method of nano silver wire suspension solution according to claim 1, which is characterized in that the lower alcohol is selected from
At least one of methanol, ethyl alcohol, isopropanol or ethylene glycol.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109261982A (en) * | 2018-11-07 | 2019-01-25 | 暨南大学 | A kind of method of simple and quick preparation silver nanowires |
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CN102328095A (en) * | 2011-10-14 | 2012-01-25 | 济南大学 | Preparation method of metal silver nanowires with adjustable length and diameter |
CN102728848A (en) * | 2011-03-31 | 2012-10-17 | 香港科技大学 | Method of producing silver nanowires in large quantities |
CN102744421A (en) * | 2012-07-16 | 2012-10-24 | 浙江师范大学 | Method for preparing large-scale Ag nanowires in aqueous solution |
CN103153844A (en) * | 2010-07-22 | 2013-06-12 | 公州大学校产学协力团 | Method for manufacturing silver nanowires |
CN103203468A (en) * | 2013-04-17 | 2013-07-17 | 苏州冷石纳米材料科技有限公司 | Method for manufacturing silver nanowires |
DE102015013238A1 (en) * | 2014-10-28 | 2016-04-28 | Dow Global Technologies Llc | Low oxygen concentration process for producing silver nanowires |
CN106131984A (en) * | 2016-09-12 | 2016-11-16 | 南京工业大学 | A kind of preparation method of nano silver wire graphene oxide composite conductive thin film heater |
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Patent Citations (7)
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CN103153844A (en) * | 2010-07-22 | 2013-06-12 | 公州大学校产学协力团 | Method for manufacturing silver nanowires |
CN102728848A (en) * | 2011-03-31 | 2012-10-17 | 香港科技大学 | Method of producing silver nanowires in large quantities |
CN102328095A (en) * | 2011-10-14 | 2012-01-25 | 济南大学 | Preparation method of metal silver nanowires with adjustable length and diameter |
CN102744421A (en) * | 2012-07-16 | 2012-10-24 | 浙江师范大学 | Method for preparing large-scale Ag nanowires in aqueous solution |
CN103203468A (en) * | 2013-04-17 | 2013-07-17 | 苏州冷石纳米材料科技有限公司 | Method for manufacturing silver nanowires |
DE102015013238A1 (en) * | 2014-10-28 | 2016-04-28 | Dow Global Technologies Llc | Low oxygen concentration process for producing silver nanowires |
CN106131984A (en) * | 2016-09-12 | 2016-11-16 | 南京工业大学 | A kind of preparation method of nano silver wire graphene oxide composite conductive thin film heater |
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Application publication date: 20180921 |