CN104014805A - Preparing method for silver nanometer wire - Google Patents
Preparing method for silver nanometer wire Download PDFInfo
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- CN104014805A CN104014805A CN201410212897.4A CN201410212897A CN104014805A CN 104014805 A CN104014805 A CN 104014805A CN 201410212897 A CN201410212897 A CN 201410212897A CN 104014805 A CN104014805 A CN 104014805A
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Abstract
The invention discloses a preparing method for a silver nanometer wire. The method comprises the following steps that organic polyhydric alcohol, water and N-methyl pyrrolidone are mixed in sequence to obtain a mixed solution A; a weak reducing agent is added to the mixed solution A, stirred or dissolved through ultrasounds to obtain a reducing solution B; silver nitrate is added to the mixed solution A, stirred and dissolved fully to obtain a reaction solution C; the reducing solution B and the reaction solution C are pumped into two glass sprayers respectively, then the reducing solution B and the reaction solution C are sprayed into a tubular closed heating reactor in the opposite directions, after spraying is finished, the constant temperature is kept to obtain a grayish yellow silver nanometer wire stock solution; the silver nanometer wire stock solution is taken out and placed in a beaker for standing and layering, clear liquid of the upper layer is poured out, and pure water is added to the stock solution for washing to obtain the clean silver nanometer wire concentrated solution; the silver nanometer wire concentrated solution is dried to obtain silver nanometer wire powder products. The preparing method has the advantages that equipment is simple, the reaction cycle is short and energy consumption is low.
Description
Technical field
The present invention relates to a kind of preparation method of nano silver wire.
Background technology
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 in recent years.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, develops new substitution material and just seems very necessary.Silver nano material especially nano silver wire has unique optics, electromagnetism, mechanics, catalytic performance, makes it in various fields, have extremely important effect as the aspects such as electric slurry, electrically-conducting paint, electrically conductive ink, conductive rubber, conductive plastics and electromagnetic screen coating 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 synthetic silver nano material mainly contains template and wet chemistry synthetic method.Template is mainly divided into hard template and two kinds of approach of soft template.It is template that hard template be take Woelm Alumina, CNT, aeroge etc. conventionally, by modes such as electro-deposition, chemical depositions, prepares silver nano material; Soft template rule is to take high molecular surfactant as template, again with all kinds of silver nano materials of chemical preparation, adopting the advantage of template is strictly to control the pattern of silver nano material, but its size, pattern are controlled by again pattern, size that template itself has, this has just proposed higher requirement to synthetic template, simultaneously these class methods exist toward contact the complex process that template is removed, and are difficult to efficient, easy, synthetic silver nano material in large quantities.
Wet chemistry synthetic method is the current main method for the preparation of silver nano material.As (Chemistry of Materials such as Xia, 2002,14 (11): 4736-4745., US7585349) take Pt or Ag as crystal seed, by silver nitrate and polyvinylpyrrolidone mixed dissolution are prepared to nano silver wire by heat reduction in ethylene glycol; 201010281704.2 of Chinese patent application prepare nano silver wire having under the condition of inert gas shielding by adding copper chloride to make controlling agent mixture of heat reduction silver nitrate and polyvinylpyrrolidone in ethylene glycol; Chinese patent application 201210190066.2 is dissolved in silver nitrate and polyvinylpyrrolidone in the mixture of glycerine and water and obtains nano silver wire by heat reduction; 20121201644.8 of Chinese patent application provide several mode of heatings to prepare nano silver wire.
The existing shortcoming of preparing nano silver wire: (1) existing patent substantially all adopts seeded growth method, inefficiency, 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 conventionally, 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, thereby 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 1: 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: weak reductant is joined in step 1 gained mixed solvent A, and wherein the concentration of weak reductant is 0.01-5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: silver nitrate is joined in another part of mixed solvent A of step 1 gained, 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 are pumped into respectively in two glass sprayers for 1:10-10:1 by volume, then the spray velocity of pressing 0.1-100 ml/min sprays reducing solution B and reaction solution C simultaneously to subtend in a tube type closed reactor heating, heating-up temperature is 25-80 ° of C, after injection completes, under 25-80 ° of C constant temperature, keep 5-60 minute, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 30-240 minute, subsequently supernatant liquor is toppled over, and add pure water to wash it, and wash after standing 2-10 time, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product.
Further, organic polyhydric alcohol described in step 1 is one or more mixtures in ethylene glycol, propane diols, butanediol, pentanediol, glycerine.
Preferably, in step 1, the volume ratio of the rear organic polyhydric alcohol of mixing 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, described in step 3, the concentration of silver nitrate 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, in step 5, by the washing of nano silver wire stoste, standing number of times, it is 3-8 time.
Further, in step 6, drying mode is freeze drying or constant temperature forced air drying, and be 30-300 minute drying time.
Due to the utilization of technique scheme, compared with prior art, the advantage having is in the present invention: 1, equipment is simple, reaction time is short, and easy, the easy row of method, heating-up temperature are low, and energy consumption is little; 2, the silver nanoparticle diameter that the method makes 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 reaction is carried out without 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, by condition, control that to obtain product purity high, draw ratio is large, without centrifugal treating, through short time sedimentation separation, can obtain.
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.
The specific embodiment
Below in conjunction with drawings and the specific embodiments, the present invention will be further described, and following examples are only for technical scheme of the present invention is more clearly described, and can not limit the scope of the invention with this.
Embodiment mono-:
As depicted in figs. 1 and 2: a kind of preparation method of nano silver wire, comprises the following steps:
Step 1: in order ethylene glycol, water, 1-METHYLPYRROLIDONE are mixed,, after mixing, the volume ratio of ethylene glycol and water is 1:10, the concentration of 1-METHYLPYRROLIDONE is 0.05 mol/L, and, obtain mixed solution A;
Step 2: weak reductant ascorbic acid is joined in step 1 gained mixed solvent A, and the concentration of weak reductant ascorbic acid is 0.5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: silver nitrate is joined in another part of mixed solvent A of step 1 gained, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 0.05 mol/L, obtains reaction solution C;
Step 4: by step 2 gained reducing solution B and step 3 gained reaction solution C by volume in 1:1 two the glass sprayers at two ends that pumped into reactor respectively, then by the spray velocity of 10 ml/min, reducing solution B and reaction solution C are sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 30 ° of C, after injection completes, under the constant temperature of 30 ℃, keep 10 minutes, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 30 minutes, subsequently supernatant liquor is toppled over, and add pure water to wash it, wash after standing 3 times, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product, and dry mode is freeze drying or constant temperature forced air drying, and be 30 minutes drying time, and the diameter of the nano silver wire of gained is 10 nanometers.
Embodiment bis-:
As shown in Figure 1, Figure 3 and Figure 4: a kind of preparation method of nano silver wire, comprises the following steps:
Step 1: 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: weak reductant potassium citrate is joined in step 1 gained mixed solvent A, and 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: silver nitrate is joined in another part of mixed solvent A of step 1 gained, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 1 mol/L, obtains reaction solution C;
Step 4: by step 2 gained reducing solution B and step 3 gained reaction solution C by volume in 2:1 two the glass sprayers at two ends that pumped into reactor respectively, then by the spray velocity of 20 ml/min, reducing solution B and reaction solution C are sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 40 ° of C, after injection completes, under the constant temperature of 40 ℃, keep 25 minutes, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 100 minutes, subsequently supernatant liquor is toppled over, and add pure water to wash it, wash after standing 4 times, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product, dry mode is freeze drying or constant temperature forced air drying, be 120 minutes drying time, and the diameter of the nano silver wire of gained is 70 nanometers, and the longer free from admixture of length.
Embodiment tri-:
As shown in Fig. 1, Fig. 5 and Fig. 6: a kind of preparation method of nano silver wire, comprises the following steps:
Step 1: 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: weak reductant citric acid is joined in step 1 gained mixed solvent A, and the concentration of weak reductant citric acid is 3 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: silver nitrate is joined in another part of mixed solvent A of step 1 gained, 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 are pumped into respectively in two glass sprayers at reactor two ends for 1:5 by volume, then by the spray velocity of 50 ml/min, reducing solution B and reaction solution C are sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 50 ° of C, after injection completes, under the constant temperature of 50 ℃, keep 35 minutes, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 170 minutes, subsequently supernatant liquor is toppled over, and add pure water to wash it, wash after standing 6 times, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product, dry mode is freeze drying or constant temperature forced air drying, be 210 minutes drying time, and the diameter of the nano silver wire of gained is 300 nanometers, and the longer free from admixture of length.
Embodiment tetra-:
As shown in Fig. 1, Fig. 7 and Fig. 8: a kind of preparation method of nano silver wire, comprises the following steps:
Step 1: 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: weak reductant ascorbic acid is joined in step 1 gained mixed solvent A, and the concentration of weak reductant ascorbic acid is 4 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: silver nitrate is joined in another part of mixed solvent A of step 1 gained, and carry out sufficient stirring and dissolving, obtaining silver nitrate concentration is 4 mol/L, obtains reaction solution C;
Step 4: by step 2 gained reducing solution B and step 3 gained reaction solution C by volume in 5:1 two the glass sprayers at two ends that pumped into reactor respectively, then by the spray velocity of 80 ml/min, reducing solution B and reaction solution C are sprayed to subtend in tubular sealed reactor heating as shown in Figure 1 simultaneously, heating-up temperature is 60 ° of C, after injection completes, under the constant temperature of 60 ℃, keep 50 minutes, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 240 minutes, subsequently supernatant liquor is toppled over, and add pure water to wash it, wash after standing 8 times, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product, dry mode is freeze drying or constant temperature forced air drying, be 300 minutes drying time, 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, easy, the easy row of method, heating-up temperature are low, and energy consumption is little; 2, the silver nanoparticle diameter that the method makes 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 reaction is carried out without 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, by condition, control that to obtain product purity high, draw ratio is large, without centrifugal treating, through short time sedimentation separation, can obtain.
Claims (9)
1. a preparation method for nano silver wire, is characterized in that: comprise the following steps:
Step 1: 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: weak reductant is joined in step 1 gained mixed solvent A, and wherein the concentration of weak reductant is 0.01-5 mol/L, through stirring or ultrasonic dissolution, obtains reducing solution B;
Step 3: silver nitrate is joined in another part of mixed solvent A of step 1 gained, 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 are pumped into respectively in two glass sprayers for 1:10-10:1 by volume, then the spray velocity of pressing 0.1-100 ml/min sprays reducing solution B and reaction solution C simultaneously to subtend in a tube type closed reactor heating, heating-up temperature is 25-80 ° of C, after injection completes, under 25-80 ° of C constant temperature, keep 5-60 minute, obtain being lark nano silver wire stoste;
Step 5: step 4 gained nano silver wire stoste is taken out and is placed in and carry out layering in beaker standing 30-240 minute, subsequently supernatant liquor is toppled over, and add pure water to wash it, and wash after standing 2-10 time, can obtain clean nano silver wire concentrate;
Step 6: step 5 gained nano silver wire concentrate is drying to obtain to nano silver wire powder product.
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 1 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: after mixing in step 1, 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. a kind of method of preparing nano 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. according to the preparation method of a kind of nano silver wire described in claim 1 or 4, it 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: described in step 3, the concentration of silver nitrate 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 ° of 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: in step 5, by the washing of nano silver wire stoste, standing number of times, be 3-8 time.
9. a kind of method of preparing nano-silver thread according to claim 1, is characterized in that: in step 6, drying mode is freeze drying or constant temperature forced air drying, and be 30-300 minute drying time.
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| CN113649558B (en) * | 2021-07-08 | 2023-03-10 | 山东建邦胶体材料有限公司 | Nano silver wire and preparation method thereof |
| CN113857487A (en) * | 2021-09-06 | 2021-12-31 | 中化学科学技术研究有限公司 | Silver nanowire and preparation method thereof |
| CN113857487B (en) * | 2021-09-06 | 2024-04-26 | 中化学科学技术研究有限公司 | Silver nanowire and preparation method thereof |
| CN115555574A (en) * | 2022-03-07 | 2023-01-03 | 盐城工学院 | Method for preparing silver nanowires with high length-diameter ratio at low temperature |
| CN115555574B (en) * | 2022-03-07 | 2023-10-31 | 盐城工学院 | Method for preparing silver nanowire with high length-diameter ratio at low temperature |
| CN115555575A (en) * | 2022-09-21 | 2023-01-03 | 安徽格派锂电循环科技有限公司 | Method for preparing nano cobalt particles by utilizing thermal spraying method |
| CN115555575B (en) * | 2022-09-21 | 2024-03-29 | 安徽格派锂电循环科技有限公司 | Method for preparing nano cobalt particles by using thermal spraying method |
| CN116072350A (en) * | 2023-04-07 | 2023-05-05 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
| CN116072350B (en) * | 2023-04-07 | 2023-08-15 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
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