CN104014805B - A kind of preparation method of nano silver wire - Google Patents
A kind of preparation method of nano silver wire Download PDFInfo
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- CN104014805B CN104014805B CN201410212897.4A CN201410212897A CN104014805B CN 104014805 B CN104014805 B CN 104014805B CN 201410212897 A CN201410212897 A CN 201410212897A CN 104014805 B CN104014805 B CN 104014805B
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Abstract
The invention discloses a kind of preparation method of nano silver wire, comprise the following steps: in order organic polyhydric alcohol, water, 1-METHYLPYRROLIDONE are mixed, obtain mixed solution A; Weak reductant being joined in mixed solvent A, through stirring or ultrasonic dissolution, obtaining reducing solution B; Silver nitrate is joined in mixed solvent A, and carry out sufficient stirring and dissolving, obtain reaction solution C; Reducing solution B and reaction solution C is pumped into respectively in two glass sprayers, then reducing solution B and reaction solution C is sprayed to subtend in a tube type closed reactor heating simultaneously, after having sprayed, keep constant temperature to obtain in lark nano silver wire stoste; Nano silver wire stoste taken out and is placed in stratification in beaker, subsequently supernatant liquor being toppled over, and adding pure water it is washed, obtaining clean nano silver wire concentrate; Carry out doing and obtain nano silver wire powder product to nano silver wire concentrate.Advantage is: equipment is simple, reaction time is short, energy consumption is little.
Description
Technical field
The present invention relates to a kind of preparation method of nano silver wire.
Background technology
In recent years along with extensively popularizing of touch-control electronic product is more and more higher to the requirement of touch-screen, particularly touch-control product of new generation is had higher requirement to light transmittance, electric conductivity, pliability.Traditional tin indium oxide (ITO) cannot meet the requirement of touch technology of new generation, thin-film solar cells etc. owing to facing the problems such as shortage of resources, pliability is poor, processing procedure is complicated, energy consumption is high, develop new alternative materials and just seem very necessary.Silver nano material especially nano silver wire has unique optics, electromagnetism, mechanics, catalytic performance, makes it in various fields as having extremely important effect in electric slurry, electrically-conducting paint, electrically conductive ink, conductive rubber, conductive plastics and the electromagnetic screen coating etc. in chemical-biological sensing, micro-nano circuit, molecular device, opto-electronic device, flexible electronic device, solar cell and electronics industry.
At present, the method for synthesizing silver nano material mainly contains template and wet chemistry synthetic method.Template is mainly divided into hard template and soft template two kinds of approach.Hard template usually with Woelm Alumina, CNT, aeroge etc. for template, prepare silver nano material by the mode such as electro-deposition, chemical deposition; Soft template rule take high molecular surfactant as template, again with all kinds of silver nano material of chemical preparation, the advantage adopting template is the pattern that strictly can control silver nano material, but its size, pattern are controlled by again pattern, size that template itself has, this just proposes higher requirement to synthesis template, simultaneously these class methods often also also exist the complex process that template is removed, be difficult to efficient, easy, synthesize silver nano material in large quantities.
Wet chemistry synthetic method is at present for the preparation of the main method of silver nano material.As (ChemistryofMaterials such as Xia, 2002,14 (11): 4736-4745., US7585349) with Pt or Ag for crystal seed, by silver nitrate and polyvinylpyrrolidone mixed dissolution are prepared nano silver wire by heat reduction in ethylene glycol; Chinese patent application 201010281704.2 makes controlling agent heat reduction silver nitrate and polyvinylpyrrolidone in ethylene glycol under the condition having inert gas shielding mixture by adding copper chloride prepares nano silver wire; Silver nitrate and polyvinylpyrrolidone are dissolved in the mixture of glycerine and water and obtain nano silver wire by heat reduction by Chinese patent application 201210190066.2; Chinese patent application 20121201644.8 provides several mode of heating and prepares nano silver wire.
The existing shortcoming preparing nano silver wire: (1) existing patent substantially all adopts seeded growth method, inefficiency, and products obtained therefrom purity is low, and centrifugal treating process is loaded down with trivial details; (2) existing patent reaction dissolvent is generally polyalcohols solvent, and environment is friendly not; (3) existing patent has the introducing of halogen-containing salt usually, increases post processing cost, especially after industry is amplified, has comparatively loaded down with trivial details blowdown problem; (4) the organic polyhydric alcohol system that existing patent adopts makes silver-colored source limited solubility, cannot obtain the reaction system of higher concentration, thus affect industry's enlarging production efficiency.
Summary of the invention
The invention provides a kind of quick, easy, method that nano silver wire is prepared in scale.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of nano silver wire, comprises the following steps:
Step one: in order organic polyhydric alcohol, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of organic polyhydric alcohol and water is 0.1:10-10:0.1, and the concentration of 1-METHYLPYRROLIDONE is 0.01-5 mol/L, obtains mixed solution A;
Step 2: joined by weak reductant in step one gained mixed solvent A, wherein the concentration of weak reductant is 0.01-5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 0.01-5 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers for 1:10-10:1 by volume respectively, reducing solution B and reaction solution C sprays to subtend in a tube type closed reactor heating by the spray velocity then pressing 0.1-100 ml/min simultaneously, heating-up temperature is 25-80 ° of C, after injection completes, under 25-80 ° of C constant temperature, keep 5-60 minute, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in beaker to leave standstill and carry out layering in 30-240 minute, subsequently supernatant liquor is toppled over, and add pure water it is washed, washing can obtain clean nano silver wire concentrate after leaving standstill 2-10 time;
Step 6: nano silver wire powder product is drying to obtain to step 5 gained nano silver wire concentrate.
Further, organic polyhydric alcohol described in step one is one or more mixtures in ethylene glycol, propane diols, butanediol, pentanediol, glycerine.
Preferably, in step one, after mixing, the volume ratio of organic polyhydric alcohol and water is 0.5:5-5:0.5; The concentration of 1-METHYLPYRROLIDONE is 0.02-4 mol/L;
Preferably, the concentration of weak reductant described in step 2 is 0.02-4 mol/L.
Further, described weak reductant is one or more mixtures in citric acid, ascorbic acid, tannic acid, tartaric acid, potassium citrate, sodium ascorbate.
Preferably, the concentration of silver nitrate described in step 3 is 0.02-4 mol/L.
Preferably, in step 4, the volume ratio of reducing solution B and reaction solution C is 1:5-5:1; Jet velocity is 0.5-80 ml/min, and heating-up temperature is 30-60 ° of C, and the retention time is 10-50 minute.
Preferably, nano silver wire stoste being washed in step 5, leaving standstill number of times is 3-8 time.
Further, in step 6, drying mode is freeze drying or constant temperature forced air drying, and drying time is 30-300 minute.
Due to the utilization of technique scheme, compared with prior art, the advantage had is in the present invention: 1, equipment is simple, reaction time is short, and method is easy, easy, heating-up temperature is low, and energy consumption is little; 2, the silver nanoparticle diameter that the method is obtained can regulate and control on a large scale; 3, this preparation method's technique is simple, easy to operate, reproducible, and transparent conductive film prepared by products obtained therefrom has excellent properties and the ITO transparent conductive film performance all fours such as high transmission rate, low sheet resistance, low haze; 4, adopt water, organic polyhydric alcohol, nitrogenous organic solvent mixed solvent as reaction system, promote reaction versatility; 5, promote silver nitrate reactant concentration, be beneficial to industry and amplify; 6, do not re-use long-chain organic polymer as directed agents/template molecule, simplify aftertreatment technology; 7, environment-friendly type, gentle reducing agent are introduced, and react and carry out without the need to high temperature; 8, use atomization reactor as reactor, augmenting response contact area, Reaction time shorten, reduction reaction temperature, save energy consumption, improves reaction efficiency; 9, control to obtain product purity by condition high, draw ratio is large, without the need to centrifugal treating, can obtain through short time sedimentation separation.
Accompanying drawing explanation
Accompanying drawing 1 is processing simulation figure of the present invention.
Accompanying drawing 2 is transmission electron microscope (TEM) figure of the nano silver wire powder of preparation in the embodiment of the present invention 1.
Accompanying drawing 3 is SEM (SEM) figure of the nano silver wire powder of preparation in the embodiment of the present invention 2.
Accompanying drawing 4 is the light microscope figure of the nano silver wire powder of preparation in the embodiment of the present invention 2.
Accompanying drawing 5 is SEM (SEM) figure of the nano silver wire powder of preparation in the embodiment of the present invention 3.
Accompanying drawing 6 is the light microscope figure of the nano silver wire powder of preparation in the embodiment of the present invention 3.
Accompanying drawing 7 is SEM (SEM) figure of the nano silver wire powder of preparation in the embodiment of the present invention 4.
Accompanying drawing 8 is the light microscope figure of the nano silver wire powder of preparation in the embodiment of the present invention 4.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments, the present invention will be further described, and following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment one:
As depicted in figs. 1 and 2: a kind of preparation method of nano silver wire, comprises the following steps:
Step one: in order ethylene glycol, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of ethylene glycol and water is 1:10, and the concentration of 1-METHYLPYRROLIDONE is 0.05 mol/L, obtain mixed solution A;
Step 2: joined by weak reductant ascorbic acid in step one gained mixed solvent A, the concentration of weak reductant ascorbic acid is 0.5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 0.05 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers at reactor two ends for 1:1 by volume respectively, then by the spray velocity of 10 ml/min, reducing solution B and reaction solution C is sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 30 ° of C, after injection completes, keep 10 minutes under the constant temperature of 30 DEG C, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste taken out and be placed in beaker to leave standstill and carry out layering in 30 minutes, toppled over by supernatant liquor subsequently, and add pure water and wash it, washing can obtain clean nano silver wire concentrate after leaving standstill 3 times;
Step 6: be drying to obtain nano silver wire powder product to step 5 gained nano silver wire concentrate, dry mode is freeze drying or constant temperature forced air drying, and drying time is 30 minutes, and the diameter of the nano silver wire of gained is 10 nanometers.
Embodiment two:
As shown in Figure 1, Figure 3 and Figure 4: a kind of preparation method of nano silver wire, comprises the following steps:
Step one: in order glycerine, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of glycerine and water is 2:5, and the concentration of 1-METHYLPYRROLIDONE is 1 mol/L, obtain mixed solution A;
Step 2: joined by weak reductant potassium citrate in step one gained mixed solvent A, the concentration of the anti-potassium citrate of weak reductant is 1 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 1 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers at reactor two ends for 2:1 by volume respectively, then by the spray velocity of 20 ml/min, reducing solution B and reaction solution C is sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 40 ° of C, after injection completes, keep 25 minutes under the constant temperature of 40 DEG C, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste taken out and be placed in beaker to leave standstill and carry out layering in 100 minutes, toppled over by supernatant liquor subsequently, and add pure water and wash it, washing can obtain clean nano silver wire concentrate after leaving standstill 4 times;
Step 6: nano silver wire powder product is drying to obtain to step 5 gained nano silver wire concentrate, dry mode is freeze drying or constant temperature forced air drying, drying time is 120 minutes, and the diameter of the nano silver wire of gained is 70 nanometers, and the longer free from admixture of length.
Embodiment three:
As shown in Fig. 1, Fig. 5 and Fig. 6: a kind of preparation method of nano silver wire, comprises the following steps:
Step one: in order pentanediol, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of ethylene glycol and water is 1:3, and the concentration of 1-METHYLPYRROLIDONE is 2.5 mol/L, obtain mixed solution A;
Step 2: joined by weak reductant citric acid in step one gained mixed solvent A, the concentration of weak reductant citric acid is 3 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 3 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers at reactor two ends for 1:5 by volume respectively, then by the spray velocity of 50 ml/min, reducing solution B and reaction solution C is sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 50 ° of C, after injection completes, keep 35 minutes under the constant temperature of 50 DEG C, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste taken out and be placed in beaker to leave standstill and carry out layering in 170 minutes, toppled over by supernatant liquor subsequently, and add pure water and wash it, washing can obtain clean nano silver wire concentrate after leaving standstill 6 times;
Step 6: nano silver wire powder product is drying to obtain to step 5 gained nano silver wire concentrate, dry mode is freeze drying or constant temperature forced air drying, drying time is 210 minutes, and the diameter of the nano silver wire of gained is 300 nanometers, and the longer free from admixture of length.
Embodiment four:
As shown in Fig. 1, Fig. 7 and Fig. 8: a kind of preparation method of nano silver wire, comprises the following steps:
Step one: in order ethylene glycol, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of ethylene glycol and water is 1:5, and the concentration of 1-METHYLPYRROLIDONE is 4 mol/L, obtain mixed solution A;
Step 2: joined by weak reductant ascorbic acid in step one gained mixed solvent A, the concentration of weak reductant ascorbic acid is 4 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 4 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers at reactor two ends for 5:1 by volume respectively, then by the spray velocity of 80 ml/min, reducing solution B and reaction solution C is sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 60 ° of C, after injection completes, keep 50 minutes under the constant temperature of 60 DEG C, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste taken out and be placed in beaker to leave standstill and carry out layering in 240 minutes, toppled over by supernatant liquor subsequently, and add pure water and wash it, washing can obtain clean nano silver wire concentrate after leaving standstill 8 times;
Step 6: nano silver wire powder product is drying to obtain to step 5 gained nano silver wire concentrate, dry mode is freeze drying or constant temperature forced air drying, drying time is 300 minutes, and the diameter of the nano silver wire of gained is 500 nanometers, and the longer free from admixture of length.
In above-mentioned reaction: 1, equipment is simple, reaction time is short, method is easy, easy, heating-up temperature is low, and energy consumption is little; 2, the silver nanoparticle diameter that the method is obtained can regulate and control on a large scale; 3, this preparation method's technique is simple, easy to operate, reproducible, and transparent conductive film prepared by products obtained therefrom has excellent properties and the ITO transparent conductive film performance all fours such as high transmission rate, low sheet resistance, low haze; 4, adopt water, organic polyhydric alcohol, nitrogenous organic solvent mixed solvent as reaction system, promote reaction versatility; 5, promote silver nitrate reactant concentration, be beneficial to industry and amplify; 6, do not re-use long-chain organic polymer as directed agents/template molecule, simplify aftertreatment technology; 7, environment-friendly type, gentle reducing agent are introduced, and react and carry out without the need to high temperature; 8, use atomization reactor as reactor, augmenting response contact area, Reaction time shorten, reduction reaction temperature, save energy consumption, improves reaction efficiency; 9, control to obtain product purity by condition high, draw ratio is large, without the need to centrifugal treating, can obtain through short time sedimentation separation.
Claims (9)
1. a preparation method for nano silver wire, is characterized in that: comprise the following steps:
Step one: in order organic polyhydric alcohol, water, 1-METHYLPYRROLIDONE are mixed, after mixing, the volume ratio of organic polyhydric alcohol and water is 0.1:10-10:0.1, and the concentration of 1-METHYLPYRROLIDONE is 0.01-5 mol/L, obtains mixed solution A;
Step 2: joined by weak reductant in step one gained mixed solvent A, wherein the concentration of weak reductant is 0.01-5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: joined by silver nitrate in step one gained another part of mixed solvent A, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 0.01-5 mol/L, obtains reaction solution C;
Step 4: step 2 gained reducing solution B and step 3 gained reaction solution C is pumped in two glass sprayers for 1:10-10:1 by volume respectively, reducing solution B and reaction solution C sprays to subtend in a tube type closed reactor heating by the spray velocity then pressing 0.1-100 ml/min simultaneously, heating-up temperature is 25-80 DEG C, after injection completes, under 25-80 DEG C of constant temperature, keep 5-60 minute, obtain in lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in beaker to leave standstill and carry out layering in 30-240 minute, subsequently supernatant liquor is toppled over, and add pure water it is washed, washing can obtain clean nano silver wire concentrate after leaving standstill 2-10 time;
Step 6: nano silver wire powder product is drying to obtain to step 5 gained nano silver wire concentrate.
2. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: organic polyhydric alcohol described in step one is one or more mixtures in ethylene glycol, propane diols, butanediol, pentanediol, glycerine.
3. the preparation method of a kind of nano silver wire according to claim 1 and 2, is characterized in that: in step one, after mixing, the volume ratio of organic polyhydric alcohol and water is 0.5:5-5:0.5; The concentration of 1-METHYLPYRROLIDONE is 0.02-4 mol/L;
4. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: the concentration of weak reductant described in step 2 is 0.02-4 mol/L.
5. the preparation method of a kind of nano silver wire according to claim 1 or 4, is characterized in that: described weak reductant is one or more mixtures in citric acid, ascorbic acid, tannic acid, tartaric acid, potassium citrate, sodium ascorbate.
6. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: the concentration of silver nitrate described in step 3 is 0.02-4 mol/L.
7. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: in step 4, the volume ratio of reducing solution B and reaction solution C is 1:5-5:1; Jet velocity is 0.5-80 ml/min, and heating-up temperature is 30-60 DEG C, and the retention time is 10-50 minute.
8. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: nano silver wire stoste being washed in step 5, leaving standstill number of times is 3-8 time.
9. the preparation method of a kind of nano silver wire according to claim 1, is characterized in that: in step 6, drying mode is freeze drying or constant temperature forced air drying, and drying time is 30-300 minute.
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| CN110369732A (en) * | 2018-04-12 | 2019-10-25 | 北京化工大学 | A kind of low temperature preparation method of silver nanowires |
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| CN1187153C (en) * | 2002-12-16 | 2005-02-02 | 同济大学 | Method for making silver nano wire using aerogel as template |
| CN1709791A (en) * | 2005-07-05 | 2005-12-21 | 华东理工大学 | Method for preparing silver nano line |
| CN100379511C (en) * | 2006-04-26 | 2008-04-09 | 云南大学 | Method for reduction preparation of silver nanowire by composite solvent |
| JP5203769B2 (en) * | 2008-03-31 | 2013-06-05 | 富士フイルム株式会社 | Silver nanowire and method for producing the same, aqueous dispersion and transparent conductor |
| JP5467252B2 (en) * | 2009-05-11 | 2014-04-09 | 国立大学法人信州大学 | Silver nanowire manufacturing method and silver nanowire |
| CN103203467B (en) * | 2013-04-17 | 2015-02-11 | 苏州冷石纳米材料科技有限公司 | Method for preparing silver nanowires |
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