CN104772469A - Method for quickly preparing silver nanoparticles through microwave irradiation - Google Patents
Method for quickly preparing silver nanoparticles through microwave irradiation Download PDFInfo
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- CN104772469A CN104772469A CN201510014437.5A CN201510014437A CN104772469A CN 104772469 A CN104772469 A CN 104772469A CN 201510014437 A CN201510014437 A CN 201510014437A CN 104772469 A CN104772469 A CN 104772469A
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Abstract
The invention discloses a method for quickly preparing silver nanoparticles through microwave irradiation. The method is characterized in that silver nitrate is used as a precursor, L-cysteine is used as a protective agent, the microwave irradiation is carried out after the precursor and the protective agent are mixed, spherical or spherical-like silver nanoparticles are generated, the particle size of the silver nanoparticles is small, the distribution is uniform, and the dispersibility of the silver nanoparticles in water solution is good. The method for preparing the silver nanoparticles, disclosed by the invention, is simple, quick and efficient and is low in cost.
Description
Technical field:
The present invention relates to a kind of preparation method of nano material, be specifically related to the silver nano-grain and preparation method thereof of a kind of even particle size distribution, stability of characteristics, belong to field of nanometer material technology.
Background technology:
Nano-noble metal refers to the noble metal of diameter between 1-100nm (as nanometer gold, silver, platinum etc.), and be the pith of composition nano material, its existence form comprises particle, colloid and cluster etc.As wherein important representative---Nano silver grain, there is very wide application prospect because it has special performance in fields such as superconduction, antibacterial, catalysis, heavy metal analysis.
The preparation method of silver nano material is a lot, and new preparation method is also continuing to bring out.In recent years, microwave because of the order of reaction had in chemical kinetics be improved, homogeneous heating and the advantage such as speed is rapid and obtaining in the application of material science develop rapidly.Microwave method is utilized to prepare the bibliographical information of the Nano silver grain of different size and different-shape at present a lot.As document (Tsuji M, NishizawaY, MatsumotoK, et al.Rapid synthesis of silver nanostructures by using microwave-polyol rnethod with the assistance of Pt seeds and polyovinylpyrrolidone [J] .Colloids and Surfaces A:Physicochemical and Engineering Aspects, 2007, 293 (1-3): 185-194) with ethylene glycol (EG) for reducing agent and solvent, polyethylene adjoins pyrrolidone and makes protective agent, silver nitrate is presoma, microwave irradiation has prepared the silver nanoparticle of different-shape, document (Chen J, Wang J, Zhang X, et al.Microwave-assisted green synthesis of nanoparticles by carboxymethyl cellulose sodium and silver nitrate [J] .Materials Chemistry and Physics, 2008, 108 (2-3): 421-424) with shuttle sodium carboxymethylcellulose pyce for reducing agent and protective agent, by shuttle methylcellulose under microwave hydrolysate reduction Ag
+ion.But these methods also exist some weak point: Small molecular organic reducing agent (as EG) adds, under microwave action, Ag
+rate of reduction accelerate, but the protected effect of these Small molecular to silver particles is poor, and interparticle fierce collision thing cause microwave to cause impels Aggregation of silver particles to grow up, and even precipitates; And it is oversize to form the silver nanoparticle reaction time by the hydrolysis of shuttle methylcellulose; The average grain diameter comparatively large (12 ~ 30nm) of the silver particles obtained by said method in addition.
Summary of the invention:
The present invention is to overcome above-mentioned defect of the prior art, provides a kind of method preparing silver nano-grain rapidly simple to operate, effective.
To achieve these goals, the inventive method preparation process is as follows:
Step one, with silver nitrate and cysteine for raw material is dissolved in ultra-pure water respectively, the concentration range of silver nitrate and cysteine is respectively: 0.05-0.2mol/L, 0.005-0.02mol/L.
Step 2, by the mixing of two of step one kinds of solution, form cysteine-silver ion complex, the mol ratio of two kinds of solution controls between 1.4:1-1.6:1, and then mixing shakes up and is placed on microwave in 170W-1000W micro-wave oven, time is 30s-120s, obtained silver nano-grain.
Compared with prior art, the invention has the beneficial effects as follows: adopt microwave method to prepare silver nano-grain, there is simple to operate, reaction speed fast, even particle size distribution, the advantages such as particle dispersion is good.
Accompanying drawing illustrates:
Fig. 1 is the uv absorption spectra of silver nano-grain in the present invention;
Fig. 2 is the transmission electron microscope picture of silver nano-grain in the present invention;
Fig. 3 is silver nanoparticle XRD figure in the present invention;
Fig. 4 is the infrared figure of silver nanoparticle in the present invention;
Detailed description of the invention:
Below by embodiment, the present invention is further described.
Embodiment 1:
Compound concentration is the liquor argenti nitratis ophthalmicus of 0.05mol/L and the Cys solution of 0.005mol/L respectively, by both with mol ratio be 1.5:1 ratio mixing be placed on irradiation in micro-wave oven, microwave power is 1000W, microwave time 90s, obtained silver nano-grain colloidal sol;
Embodiment 2:
Compound concentration is the liquor argenti nitratis ophthalmicus of 0.05mol/L and the Cys solution of 0.005mol/L respectively, by both with mol ratio be 1.5:1 ratio mixing be placed on irradiation in micro-wave oven, microwave power is 850W, microwave time 60s, obtained silver nano-grain colloidal sol;
Embodiment 3:
First, compound concentration is the liquor argenti nitratis ophthalmicus of 0.1mol/L and the Cys solution of 0.01mol/L respectively, and be that the ratio mixing of 1:1 is placed on irradiation in micro-wave oven with mol ratio by both, microwave power is 1000W, microwave time 90s, obtained silver nano-grain colloidal sol;
Embodiment 4:
First, compound concentration is the liquor argenti nitratis ophthalmicus of 0.2mol/L and the Cys solution of 0.02mol/L respectively, and be that the ratio mixing of 1.25:1 is placed on irradiation in micro-wave oven with mol ratio by both, microwave power is 660W, microwave time 120s, obtained absinthe-green silver nano-grain;
Be only several specific embodiment of the present invention above, but the present invention is not limited thereto, the changes that any person skilled in the art can think of all should fall into protection scope of the present invention.
Claims (4)
1. microwave method prepares a method for silver nano-grain fast, it is characterized in that: its step is,
Step one, is dissolved in ultra-pure water by silver nitrate and cysteine respectively;
Step 2, two kinds of solution mixing of step one being joined shake up, obtained cysteine-silver ion complex;
Step 3, complex solution step 2 obtained, as precursor, carries out microwave radiation processing, obtains silver nano-grain.
2. microwave method according to claim 1 prepares the method for silver nano-grain fast, it is characterized in that: in described step one, the concentration range of silver nitrate and cysteine is respectively: 0.05-0.2mol/L, 0.005-0.02mol/L.
3. microwave method according to claim 1 prepares the method for silver nano-grain fast, it is characterized in that: in described step 2, the molar ratio range of silver nitrate and cysteine is between 1.4:1-1.6:1.
4. microwave method according to claim 1 prepares the method for silver nano-grain fast, it is characterized in that: in described step 3, microwave power is at 170W-1000W, and microwave irradiation time is 30s-120s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510014437.5A CN104772469A (en) | 2015-01-12 | 2015-01-12 | Method for quickly preparing silver nanoparticles through microwave irradiation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510014437.5A CN104772469A (en) | 2015-01-12 | 2015-01-12 | Method for quickly preparing silver nanoparticles through microwave irradiation |
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| CN104772469A true CN104772469A (en) | 2015-07-15 |
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| CN201510014437.5A Pending CN104772469A (en) | 2015-01-12 | 2015-01-12 | Method for quickly preparing silver nanoparticles through microwave irradiation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108372309A (en) * | 2018-03-13 | 2018-08-07 | 昆明理工大学 | A kind of preparation method of nano silver cubic block |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121203A (en) * | 2007-07-23 | 2008-02-13 | 淮阴工学院 | Microwave preparing method for nanometer silver or gold |
| CN101310899A (en) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | Method for preparing silver nano-wire in large batch |
| CN102059344A (en) * | 2010-11-11 | 2011-05-18 | 厦门大学 | Method for synthesizing fluorescent silver nano-particles under microwave by polymethylacrylic acid |
| CN102860325A (en) * | 2012-09-12 | 2013-01-09 | 江南大学 | Bactericidal nano-silver water gel and preparation method thereof |
-
2015
- 2015-01-12 CN CN201510014437.5A patent/CN104772469A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121203A (en) * | 2007-07-23 | 2008-02-13 | 淮阴工学院 | Microwave preparing method for nanometer silver or gold |
| CN101310899A (en) * | 2008-03-18 | 2008-11-26 | 江苏工业学院 | Method for preparing silver nano-wire in large batch |
| CN102059344A (en) * | 2010-11-11 | 2011-05-18 | 厦门大学 | Method for synthesizing fluorescent silver nano-particles under microwave by polymethylacrylic acid |
| CN102860325A (en) * | 2012-09-12 | 2013-01-09 | 江南大学 | Bactericidal nano-silver water gel and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| BABITA BARUWATI ET AL.: "Glutathione promoted expeditious green synthesis of silver nanoparticles in water using microwaves", 《GREEN CHEMISTRY》 * |
| 翁春璐等: "微波法制备纳米银研究", 《高校实验室工作研究》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108372309A (en) * | 2018-03-13 | 2018-08-07 | 昆明理工大学 | A kind of preparation method of nano silver cubic block |
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Application publication date: 20150715 |
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