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 PDF

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Publication number
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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CN
China
Prior art keywords
nano
suspension solution
wire suspension
preparation
silver
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CN201810301344.4A
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Chinese (zh)
Inventor
许小勇
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Suzhou Yu Lin New Mstar Technology Ltd
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Suzhou Yu Lin New Mstar Technology Ltd
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Priority to CN201810301344.4A priority Critical patent/CN108555310A/en
Publication of CN108555310A publication Critical patent/CN108555310A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0547Nanofibres or nanotubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture 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

A kind of preparation method of nano silver wire suspension solution
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.
CN201810301344.4A 2018-04-04 2018-04-04 A kind of preparation method of nano silver wire suspension solution Pending CN108555310A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
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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Application publication date: 20180921