CN1843670A - Method for reduction preparation of silver nanowire by composite solvent - Google Patents
Method for reduction preparation of silver nanowire by composite solvent Download PDFInfo
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- CN1843670A CN1843670A CN 200610010847 CN200610010847A CN1843670A CN 1843670 A CN1843670 A CN 1843670A CN 200610010847 CN200610010847 CN 200610010847 CN 200610010847 A CN200610010847 A CN 200610010847A CN 1843670 A CN1843670 A CN 1843670A
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Abstract
The invention relates to a method for using compound solvent reduction method to prepae silver nanometer wire, belonging to the technique of metallic powder preparation, with lower cost, environment protection and the application for industrial production. The method comprises: dissolving polyvinyl pyrrolidon in compound solvent whose volume ration is 1:0.1-1:1 between glycerin, and water, ethanol, isopropanol, glycol, or acetylacetone, to be heated; adding silver nitrate into the solution of glycerin and ion-exchange water whose volume is 1:2, to attain the Ag+ solution in 0.5-2.0M; using said solution to spray compound solvent and react 1/4-4 hours in 90-160Deg. C; collecting products; the mol percentage between the polyvinyl pyrrolidon and the Ag+ is 0.5-10; and the Ag+ solution sprays the regurgitated compound solvent in the speed of 3g/m2.s-10g/m2.s while the reaction time is 1-4 hours and the reaction temperature is 120-160Deg. C. The shape and size of particles are controlled by the ration of react matters and react condition, and said invention can attain the silver nanometer wires whose length is 5 mum-200 mum, diameter is 70-90nm, and reduced silver rate is 99%.
Description
Affiliated technical field
The present invention relates to the metal powder material preparation method.
Background technology
Nano silver wire produces conductive electric current under the applying electrical potential effect, have the electric conductivity of block silver, especially Du Te quantum transmission effects and receiving much concern in nano photoelectric designs and application facet.At present, to prepare nano silver wire be nano wire by CNT, silica template, molecular template absorption nano particle and by self-organizing growth mainly to template.Productive rate is low, product separates than problems such as difficulties with template but exist.For solving the problem that exists, " a kind of device for preparing the fine silver monocrystal nanowire ", CN1522951, provide and comprised dc source, substrate and precipitation silver ion conducting film thereon, metal anode and metallic cathode, wherein metal anode and metallic cathode are the silver metal film that is deposited in the substrate two ends.This device needs special installation and preparation." synthetic method of monocrystal silver nano line ", CN1424163 is to prepare nano silver wire under the butyl titanate media environment, has the residual or absorption problem of inorganic ions." a kind of synthetic method of nano silver wire ", CN1740405 proposes prefabricated silver-colored crystal seed, under 140-200 ℃ of temperature, the method of ethylene glycol medium two step synthesizing nano-silver line because simple ethylene glycol solvent has considerable restraint to the solubility of silver nitrate, can not obtain the reaction system of higher concentration.Therefore, this method is unwell to industrial-scale production.How preparation cost is cheap, and the no too much inorganic salts of stable performance pollute system, and method that can the suitability for industrialized production nano-silver thread is the target that does not reach as yet at present.
Summary of the invention
The purpose of this invention is to provide the method for preparing nano silver wire that cost is low, cost performance is high, suitability for industrialized is produced.
The present invention realizes by following approach:
(1) weighing polyvinylpyrrolidonepowder powder is dissolved in it in double solvents that volume ratio is 1: 0.1～1: 1 glycerine and water or ethanol or isopropyl alcohol or one of ethylene glycol or acetylacetone,2,4-pentanedione, adds hot reflux 15～40 minutes;
(2) silver nitrate being added volume ratio is 1: 2 glycerine and ion-exchange water mixed solution, forms the Ag of 0.5～2.0M
+Solution with this solution spraying double solvents (1), is collected product after reacting 1/4～4 hour between 90 ℃～160 ℃;
Wherein, polyvinylpyrrolidone monomer and Ag in the double solvents
+The molal weight ratio be 0.5～10.
Described Ag
+The double solvents that solution refluxes with vaporific spray, its speed is 3g/m
2.s～10g/m
2.s.
The described reaction time is preferable over 1-4 hour, and reaction temperature is preferable between 120 ℃～160 ℃.
The product of described reaction dilutes centrifuge washing final vacuum drying with acetone or deionized water.
Wherein, silver-colored solution adding mode, PVP concentration directly influence the size pattern of nano wire.Reaction temperature also influences the speed that nucleus generates except the size pattern that influences nano wire.As preferably, reaction temperature can not be too low, and temperature is too low, and reaction can not be carried out; Reaction temperature is too high, is easy to generate short line or other pattern.
Polyvinylpyrrolidone, promptly PVP is polymerized by single N vinyl pyrrolidone, and the monomer molar quality is 112g.
The principle of the invention can be stated as: with PVP as polymer template, glycerine and water, or ethanol or isopropyl alcohol or the uniform double solvents of one of ethylene glycol or acetylacetone,2,4-pentanedione dissolving be as reaction medium, and cracking produced solvated electron after the hydroxyl of glycerine was heated and reaches uniform temperature.When using Ag
+Solution forms dropping liquid or vaporific when going to spray the double solvents of backflow, Ag
+Solution down precipitates under gravity and fluid pressure action, simultaneously, and solvated electron and Ag that glycerine produces
+Between gravitational interaction, obtain the energy solvated electron and leap to Ag by excitation state
+Less than being with Ag
+Reduction.Contain Ag organic dispersion medium and PVP and form silver nano-grain bunch by Fan Dehuali interaction polymerization, silver nano-grain is touched motion collision in the plate at the PVP polymer, and crystal grain shoots up and is the filiform of 1-dimention nano steric configuration.
The present invention has realized that polymer beads changes to the nanometer wire by nanometer is spherical, reaction product need not to clean sodium ion and acid-base reagent, can obtain length after the filtration is 5 μ m～200 μ m, diameter is the nano silver wire of 70～90nm well-crystallized shape, and the percent reduction of silver does not detect other inorganic ions up to 99% in end product.Therefore, the present invention is environmentally friendly, productive rate height, suitability for industrialized production.
Description of drawings
Fig. 1 is that the low power of nano silver wire sample of the present invention scans electric border photo.
Fig. 2 is that the high power of nano silver wire sample of the present invention scans electric border photo.
The specific embodiment
Embodiment 1:
In the polytetrafluoroethylene (PTFE) reactor, weighing template polyethylene of dispersing agent pyrrolidones 2.8g adds the 100ml glycerine, and in the 10ml water compounded solvents, the heating temperature of reaction kettle reaches 120 ℃, refluxes 20 minutes; Adding volume ratio with the silver nitrate of purity 99.5% is to heat a little in 1: 2 glycerine and the deionized water mixed solution, obtains the 1M liquor argenti nitratis ophthalmicus; With this solution 60ml gradation spray double solvents, the speed of spray can be at 3g/m
2.s～10g/m
2.s between, 120 ℃ were reacted 4 hours, separate, and acetone or deionization washing one time, vacuum drying, the gained powder carries out physics and chemistry and detects, and obtains nano silver wire 6.25g.In Fig. 1 as seen, the nano silver wire that a large amount of filiforms of tens microns of length are formed.
Embodiment 2:
Press method and the dosage of embodiment 1, the amount of PVP is added to 11.2g, and temperature of reaction kettle reaches 160 ℃, reacts 4 hours, obtains the Nano Silver nano wire, and product has 6.32g.
Embodiment 3:
Press the method for embodiment 1,100ml glycerine, 100ml water, PVP2.8g, spray 40ml1MAgNO
3Solution, 90 ℃ of temperature of reaction kettle reacted 4 hours, obtained the dark yellow silver sol of even nano silver wire, and visible ultraviolet maximum absorption band is near 420nm.
Embodiment 4:
Press the method for embodiment 1,100ml glycerine, 20ml acetylacetone,2,4-pentanedione, PVP2.8g, 10ml1MAgNO
3Solution, 120 ℃ of temperature of reaction kettle reacted 2 hours, obtained nano silver wire 6.19g.As seen, pattern is clear, the nano silver wire of homogeneous in Fig. 2.
Claims (4)
1, with the method for double solvents reduction preparation of silver nano wire, it is characterized in that:
(1) weighing polyvinylpyrrolidonepowder powder is dissolved in it in double solvents that volume ratio is 1: 0.1～1: 1 glycerine and water or ethanol or isopropyl alcohol or one of ethylene glycol or acetylacetone,2,4-pentanedione, adds hot reflux 15～40 minutes;
(2) silver nitrate being added volume ratio is 1: 2 glycerine and ion-exchange water mixed solution, forms the Ag of 0.5～2.0M
+Solution with this solution spraying double solvents (1), is collected product after reacting 1/4～4 hour between 90 ℃～160 ℃;
Wherein, polyvinylpyrrolidone monomer and Ag in the double solvents
+The molal weight ratio be 0.5～10.
2, the method with double solvents reduction preparation of silver nano wire according to claim 1 is characterized in that Ag
+The double solvents that solution refluxes with vaporific spray, its speed is 3g/m
2.s～10g/m
2.s.
3, the method with double solvents reduction preparation of silver nano wire according to claim 1 is characterized in that the reaction time is preferable over 1～4 hour, and reaction temperature is preferable between 120 ℃～160 ℃.
4, the method with double solvents reduction preparation of silver nano wire according to claim 1 is characterized in that the product that reacts dilutes centrifuge washing final vacuum drying with acetone or deionized water.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220506B (en) * | 2007-09-27 | 2011-05-04 | 复旦大学 | Method for high concentration mass-synthesis of silver nano-wire |
| CN102085574B (en) * | 2009-12-04 | 2012-12-12 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| CN103170645A (en) * | 2013-03-27 | 2013-06-26 | 中国科学院深圳先进技术研究院 | Preparation method of silver nanowires |
| CN103370455A (en) * | 2011-02-15 | 2013-10-23 | 卡尔斯特里姆保健公司 | Nanowire preparation methods, compositions, and articles |
| CN104014805A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparing method for silver nanometer wire |
| CN104028775A (en) * | 2014-06-19 | 2014-09-10 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for monodisperse uniform-particle-size silver nanoparticles |
| CN104551011A (en) * | 2015-01-29 | 2015-04-29 | 三明学院 | Production method of sliver nano-rods |
| 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 |
| US9073122B2 (en) | 2011-12-19 | 2015-07-07 | Industrial Technology Research Institute | Method for preparing silver nanowire |
| US9080255B2 (en) | 2011-03-31 | 2015-07-14 | The Hong Kong University Of Science And Technology | Method of producing silver nanowires in large quantities |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through hydrocyclone |
| CN105414561A (en) * | 2015-12-28 | 2016-03-23 | 中国科学技术大学 | Silver nanowire assembly and preparation method and flexible conductor thereof |
| JP2018532048A (en) * | 2015-10-09 | 2018-11-01 | 重▲慶▼文理学院 | Method for producing silver nanowire with uniform aspect ratio |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN109261983A (en) * | 2018-11-22 | 2019-01-25 | 韩金玲 | A kind of preparation method of ultra-fine high length-diameter ratio silver nanowires |
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| US6692715B2 (en) * | 2001-08-30 | 2004-02-17 | Mine Jeffrey Inc. | Silica nanofibers and method for preparing them |
| CN1203949C (en) * | 2002-12-31 | 2005-06-01 | 中国科学院上海光学精密机械研究所 | Method for synthesizing single crystal silver nano-wire |
| JP2005125282A (en) * | 2003-10-27 | 2005-05-19 | Denso Corp | Catalyst particle and method for manufacturing the same |
| CN1709791A (en) * | 2005-07-05 | 2005-12-21 | 华东理工大学 | Method for preparing silver nano line |
| CN100342064C (en) * | 2005-09-23 | 2007-10-10 | 浙江大学 | Silver nanometer wire synthesizing process |
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2006
- 2006-04-26 CN CNB2006100108473A patent/CN100379511C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220506B (en) * | 2007-09-27 | 2011-05-04 | 复旦大学 | Method for high concentration mass-synthesis of silver nano-wire |
| CN102085574B (en) * | 2009-12-04 | 2012-12-12 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| CN103370455A (en) * | 2011-02-15 | 2013-10-23 | 卡尔斯特里姆保健公司 | Nanowire preparation methods, compositions, and articles |
| US9080255B2 (en) | 2011-03-31 | 2015-07-14 | The Hong Kong University Of Science And Technology | Method of producing silver nanowires in large quantities |
| US9073122B2 (en) | 2011-12-19 | 2015-07-07 | Industrial Technology Research Institute | Method for preparing silver nanowire |
| CN103170645A (en) * | 2013-03-27 | 2013-06-26 | 中国科学院深圳先进技术研究院 | Preparation method of silver nanowires |
| CN104014805A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparing method for silver nanometer wire |
| CN104028775A (en) * | 2014-06-19 | 2014-09-10 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for monodisperse uniform-particle-size silver nanoparticles |
| CN104551011A (en) * | 2015-01-29 | 2015-04-29 | 三明学院 | Production method of sliver nano-rods |
| 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 |
| CN104998746A (en) * | 2015-07-31 | 2015-10-28 | 合肥微晶材料科技有限公司 | Method for separating silver nanowire through hydrocyclone |
| JP2018532048A (en) * | 2015-10-09 | 2018-11-01 | 重▲慶▼文理学院 | Method for producing silver nanowire with uniform aspect ratio |
| CN105414561A (en) * | 2015-12-28 | 2016-03-23 | 中国科学技术大学 | Silver nanowire assembly and preparation method and flexible conductor thereof |
| CN105414561B (en) * | 2015-12-28 | 2018-04-10 | 中国科学技术大学 | A kind of nano silver wire assembly and preparation method thereof and fexible conductor |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN109261983A (en) * | 2018-11-22 | 2019-01-25 | 韩金玲 | A kind of preparation method of ultra-fine high length-diameter ratio silver nanowires |
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