CN104028775A - Preparation method for monodisperse uniform-particle-size silver nanoparticles - Google Patents
Preparation method for monodisperse uniform-particle-size silver nanoparticles Download PDFInfo
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- CN104028775A CN104028775A CN201410275855.5A CN201410275855A CN104028775A CN 104028775 A CN104028775 A CN 104028775A CN 201410275855 A CN201410275855 A CN 201410275855A CN 104028775 A CN104028775 A CN 104028775A
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Abstract
The invention relates to the field of precious metal nano materials, in particular to a preparation method for monodisperse uniform-particle-size silver nanoparticles. Equipment such as microwave and ultrasound is not required for assistance, and the needed silver nanoparticles can be obtained only by simple one-step quick chemical reaction. Expensive preparation equipment is omitted, the method is simple and controllable in process and technique, friendly in reaction solvent environment and mild in reaction conditions, and a new technique which is low in cost, short in period and capable of being implemented industrially is provided for the silver nanoparticles.
Description
Technical field
The present invention relates to noble metal nanometer material field, be specifically related to a kind of preparation method of the particle diameter silver nano-grain that is singly uniformly dispersed.
Background technology
Noble metal nano particles becomes the focus of Recent study because of its unique character and potential application.Wherein silver nano-grain is owing to having unique optics, electricity and catalytic property, in the numerous areas such as electronics, chemical industry, biology, the military project value that has a wide range of applications.According to incompletely statistics, exceed 600 tons (argentiferous 30% left and right) for the every annual requirement of electromagnetic screen coating of weaponry; And exceed 200 tons (argentiferous 50% left and right) for the every annual requirement of high-performance slurry of electronic printing; Because silver nano-grain has surface plasmon resonance effect, in photovoltaic cell, LED illumination, biomedical detection, also there is tempting application prospect again.
About the preparation method of silver nano-grain, be mainly divided at present Physical, chemical method, bioanalysis etc.Wherein, the advantages such as simple to operate owing to having, easy to control, the applicable production in enormous quantities of chemical method, are most widely used a kind of preparation means.Specifically can be divided into again chemical reduction method, photoreduction met hod, Microwave-assisted Reduction method, electrochemical process, sonochemistry method, microemulsion method etc. (M.Rycenga, C.M.Cobley, J.Zeng, W.Y.Li, C.H.Moran, Q.Zhang, D.Qin, and Y.N.Xia, " Controlling the Synthesis and Assembly of Silver Nanostructures for Plasmonic Applications ", Chem.Rev., 2011,111:3669-3712).For the silver nano-grain that makes preparation has excellent performance and good reliability, there are several key technologies urgently to be resolved hurrily, be wherein topmostly to keep grain diameter homogeneity, dispersion stabilization.Especially for small size silver nano-grain, owing to thering is higher specific area and chemism, utilize simple chemical reduction method to be difficult to solve the agglomeration traits between particle.
In order to obtain the silver nano-grain of uniform grading, polymolecularity, researchers have taked the multiple chemical preparating process of realizing approach improvement particle, as introduce multistep chemical reaction, relax reaction rate and adopt ultrasonic or microwave equipment (the H.S.Li such as to assist, H.B.Xia, D.Y.Wang, and X.T.Tao, " Simple synthesis of monodisperse; quasi-spherical; citrate-stabilized silver nanocrystals in water ", Langmuir, 2013,29:5074-5079).But not only having increased manufacturing cycle and cost greatly, said method also increases the uncontrollability of technique simultaneously.Therefore,, if can be by a simple step chemical reaction, the particle diameter silver nano-grain that is singly uniformly dispersed, can significantly improve the mass production ability of silver nano-grain undoubtedly, and its industrial applications is played to important impetus.
Summary of the invention
In order to solve the problem existing in existing silver nano-grain preparation technology, the invention provides a kind of preparation method of the particle diameter silver nano-grain that is singly uniformly dispersed of simple and fast.
Singly the be uniformly dispersed preparation method of particle diameter silver nano-grain, its preparation process is:
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) in 100ml there-necked flask, 4-8g polyvinylpyrrolidone is dissolved in 25ml ethylene glycol solution, rapid stirring, is heated to 120 DEG C by solution;
3) in flask, inject the above-mentioned liquor argenti nitratis ophthalmicus of 5ml with the speed of 5ml/ second, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
Utilize silver nano-grain tool prepared by the inventive method to have the following advantages:
1. can prepare quickly and easily the silver nano-grain of the particle diameter that is singly uniformly dispersed, only need a step chemical reaction to realize.
2. do not need complicated auxiliary Preparation equipment, with low cost.
3. the silver-colored particle colloidal sols good stability of preparation, can long-term storage, repeatedly use.
4. the method agents useful for same environmentally safe, technological parameter is simple, can conveniently realize mass production.
The present invention has developed a kind of preparation technology of the particle diameter silver nano-grain that is singly uniformly dispersed.Auxiliary without microwave, the equipment such as ultrasonic, by a simple step fast chemical reaction, can obtain required silver nano-grain.The method is without expensive Preparation equipment, and process is simply controlled, reaction dissolvent environmental friendliness, reaction condition gentleness, for silver nano-grain material provide a kind of low cost, short period, can industrializing implementation new technology.
Brief description of the drawings
Fig. 1 is the TEM figure of silver nano-grain synthetic in comparative example 1;
Fig. 2 is the TEM figure of silver nano-grain synthetic in embodiment 1;
Fig. 3 is the TEM figure of silver nano-grain synthetic in comparative example 2;
Fig. 4 is the TEM figure of silver nano-grain synthetic in embodiment 2.
Detailed description of the invention
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) polyvinylpyrrolidone that is 10000 by 4g molecular weight in 100ml there-necked flask is dissolved in 25ml ethylene glycol solution, and solution is heated to 120 DEG C by rapid stirring.
3) in flask, inject fast the above-mentioned liquor argenti nitratis ophthalmicus of 5ml with the speed of 5ml/ second, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
Comparative example 1
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) polyvinylpyrrolidone that is 10000 by 4g molecular weight in 100ml there-necked flask is dissolved in 25ml ethylene glycol solution, rapid stirring.
3) in flask, slowly drip the above-mentioned liquor argenti nitratis ophthalmicus of 5ml, be heated to 120 DEG C with the heating rate of 1 DEG C/min, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
Fig. 1 is the TEM figure of silver nano-grain synthetic in comparative example 1.Can see prepared silver nano-grain pattern spherical in shape.The particle diameter of particle changes between 50 nanometers in 5 nanometers, and reunites between some particle.Fig. 2 is the TEM figure of silver nano-grain synthetic in embodiment 1.As we can see from the figure, prepared silver nano-grain pattern spherical in shape, size is distributed in 20 to 40 nanometers substantially.Compare and can find with the silver-colored particle in comparative example 1, in embodiment 1, the distribution of the particle diameter of the silver nano-grain of synthesized is more even, dispersiveness is better, and the reunion between particle is less.By means such as Spectral Extinctions, above-mentioned two kinds of silver nano-grains are characterized, its result has also confirmed this phenomenon.Utilize technique described in embodiment 1 why can obtain the particle diameter silver nano-grain that is singly uniformly dispersed, main attribution is: in hot reproducibility solvent, inject fast after silver salt solution, Ag ion is reduced to rapidly a large amount of silver atoms, produce a large amount of cores, the degree of supersaturation moment of Ag atom is increased, thereby can evenly grow up at growth phase.Compare with the electronation preparation technology described in traditional similar comparative example 1, such growth conditions more easily makes the growth conditions of crystal grain be consistent, thereby has improved the monodispersity of product and the uniformity of particle diameter.
Embodiment 2
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) polyvinylpyrrolidone that is 40000 by 8g molecular weight in 100ml there-necked flask is dissolved in 25ml ethylene glycol solution, and solution is heated to 120 DEG C by rapid stirring.
3) in flask, inject fast the above-mentioned liquor argenti nitratis ophthalmicus of 5ml with the speed of 5ml/ second, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
Comparative example 2
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) polyvinylpyrrolidone that is 40000 by 8g molecular weight in 100ml there-necked flask is dissolved in 25ml ethylene glycol solution, rapid stirring.
3) in flask, slowly drip the above-mentioned liquor argenti nitratis ophthalmicus of 5ml, be heated to 120 DEG C with the heating rate of 1 DEG C/min, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
Fig. 3 is the TEM figure of silver nano-grain synthetic in comparative example 2.Can see prepared silver nano-grain pattern spherical in shape.The particle diameter of particle changes between 60 nanometers in 20 nanometers, and reunites between some particle.Fig. 4 is the TEM figure of silver nano-grain synthetic in embodiment 2.As we can see from the figure, prepared silver nano-grain pattern spherical in shape, size is distributed in 20 to 30 nanometers substantially.Compare and can find with the silver-colored particle in comparative example 2, in embodiment 2 particle diameter of the silver nano-grain of synthesized distribute more evenly, dispersed better, between particle almost without reunion.By means such as Spectral Extinctions, above-mentioned two kinds of silver nano-grains are characterized, its result has also confirmed this phenomenon.It forms mechanism with described in embodiment 1.
Claims (1)
1. be singly the uniformly dispersed preparation method of particle diameter silver nano-grain, is characterized in that the method comprises the steps:
1) silver nitrate is dissolved in ethylene glycol, is stirred well to completely and dissolves, obtain the silver nitrate settled solution of 0.03g/L;
2) in 100ml there-necked flask, 4-8g polyvinylpyrrolidone is dissolved in 25ml ethylene glycol solution, rapid stirring, is heated to 120 DEG C by solution;
3) in flask, inject the above-mentioned liquor argenti nitratis ophthalmicus of 5ml with the speed of 5ml/ second, after insulation 30min, use frozen water to be cooled to normal temperature;
4), with obtaining nano silver colloidal sol after acetone centrifuge washing, after being dried, can obtain nano-Ag particles.
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Cited By (9)
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| CN105710386A (en) * | 2016-02-25 | 2016-06-29 | 天津工业大学 | One-dimension silver chain nano-structure, self-assembly preparation method and SERS application |
| CN106541149A (en) * | 2016-12-07 | 2017-03-29 | 桂林电子科技大学 | A kind of accurate-size controls the preparation method of extra small nano-Ag particles |
| CN106610144A (en) * | 2016-12-07 | 2017-05-03 | 桂林电子科技大学 | Method for preparing photo-thermal steam by absorbing sunlight through localized surface plasmon resonance (LSPR) of nano material |
| CN107363268A (en) * | 2017-08-24 | 2017-11-21 | 深圳市格络光电有限公司 | A kind of continuous apparatus and method for preparing high solids content Nano Silver |
| CN107639238A (en) * | 2017-10-26 | 2018-01-30 | 北京科技大学 | A kind of controllable method for preparing of monodisperse silver powder |
| CN108436101A (en) * | 2018-04-27 | 2018-08-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres |
| CN110014168A (en) * | 2019-05-23 | 2019-07-16 | 深圳先进技术研究院 | A kind of nano-Ag particles and preparation method thereof |
| CN110982354A (en) * | 2019-12-25 | 2020-04-10 | 上海市建筑科学研究院有限公司 | Antibacterial and mildew-proof interior wall coating for building and preparation method and application thereof |
| CN111112639A (en) * | 2020-01-02 | 2020-05-08 | 西安工业大学 | Nanoscale spherical silver particles with room-temperature antifriction effect and preparation method thereof |
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Cited By (14)
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|---|---|---|---|---|
| CN105710386A (en) * | 2016-02-25 | 2016-06-29 | 天津工业大学 | One-dimension silver chain nano-structure, self-assembly preparation method and SERS application |
| CN105710386B (en) * | 2016-02-25 | 2018-04-03 | 天津工业大学 | One-dimensional silver-colored chain nanostructured, self-assembly preparation method thereof and SERS applications |
| CN106541149B (en) * | 2016-12-07 | 2019-04-19 | 桂林电子科技大学 | A kind of accurate-size controls the preparation method of extra small nano-Ag particles |
| CN106541149A (en) * | 2016-12-07 | 2017-03-29 | 桂林电子科技大学 | A kind of accurate-size controls the preparation method of extra small nano-Ag particles |
| CN106610144A (en) * | 2016-12-07 | 2017-05-03 | 桂林电子科技大学 | Method for preparing photo-thermal steam by absorbing sunlight through localized surface plasmon resonance (LSPR) of nano material |
| CN106610144B (en) * | 2016-12-07 | 2019-10-25 | 桂林电子科技大学 | A kind of method that local surface plasma resonance absorption sunlight prepares steam |
| CN107363268A (en) * | 2017-08-24 | 2017-11-21 | 深圳市格络光电有限公司 | A kind of continuous apparatus and method for preparing high solids content Nano Silver |
| CN107363268B (en) * | 2017-08-24 | 2023-04-18 | 深圳原驰三维技术有限公司 | Device and method for continuously preparing high-solid-content nano silver |
| CN107639238A (en) * | 2017-10-26 | 2018-01-30 | 北京科技大学 | A kind of controllable method for preparing of monodisperse silver powder |
| CN108436101A (en) * | 2018-04-27 | 2018-08-24 | 同济大学 | A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres |
| CN110014168A (en) * | 2019-05-23 | 2019-07-16 | 深圳先进技术研究院 | A kind of nano-Ag particles and preparation method thereof |
| CN110982354A (en) * | 2019-12-25 | 2020-04-10 | 上海市建筑科学研究院有限公司 | Antibacterial and mildew-proof interior wall coating for building and preparation method and application thereof |
| CN111112639A (en) * | 2020-01-02 | 2020-05-08 | 西安工业大学 | Nanoscale spherical silver particles with room-temperature antifriction effect and preparation method thereof |
| CN111112639B (en) * | 2020-01-02 | 2023-04-07 | 西安工业大学 | Nanoscale spherical silver particles with room-temperature antifriction effect and preparation method thereof |
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