CN103464778B - The synthetic method of different-grain diameter Nanometer Copper under microwave or ultraviolet irradiation - Google Patents
The synthetic method of different-grain diameter Nanometer Copper under microwave or ultraviolet irradiation Download PDFInfo
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Abstract
The present invention relates under microwave, ultraviolet irradiation different-grain diameter Nanometer Copper synthetic method, belong to nano-functional material field.The method is carried out as steps described below：Under microwave, ultraviolet irradiation, in the 100 ml three-neck flasks that the copper nitrate of 0.1 0.5 mol/L is added to, motor stirrer adds the organic modifier of 5 wt% 20 wt% after stirring 10 min, after solution rises to reaction temperature, dropwise Deca reducing agent sodium borohydride 0.2 2.5 mol/L, react 30 120 min, be prepared for various sizes of nano copper particle.The mean diameter of nano copper particle is 3 80 nm, distribution of sizes is 2 108 nm.The Nanometer Copper prepared with the method, grain diameter is little, even size distribution, good dispersion, and the method reaction condition is easily controllable, inexpensive, the advantage of processing technology and simple flow.
Description
Technical field
The present invention relates under microwave, ultraviolet irradiation different-grain diameter Nanometer Copper synthetic method, refer in particular in microwave, ultraviolet irradiation
Under, add and refer in particular to Sorbitol, double (p- sulfonyl-phenyl) the Phenylphosphine di-potassium of two hydrations containing polyhydric organic compound,
The method being prepared for different size Nanometer Copper under the conditions of differential responses, belongs to nano-functional material field.
Background technology
Nano metal has the thing different from reguline metal material at aspects such as catalysis, photochemistry, magnetic, conduction, biologies
Physical chemistry characteristic, the pattern of nano-metal particle directly influences these properties.Morphology control synthesis and the application of nano metal
Research belongs to the important directions in investigation of materials field, participates in chemosynthesis using surfactant, carries out particle size and pattern
The preparation of nano metal controlling and applied research have far-reaching theory and using value.With the slaine of copper as parent,
In aqueous solution or organic solution, using the organic modifier with different functional groups（As many carboxyls, polyhydroxy Organic substance etc.）,
Different preparation conditions, carries out the study on the synthesis of the Nanometer Copper of particle size and morphology control.The synthesis of Nanometer Copper morphology control is ground
Study carefully the relation of the formation disclosing nano metal crystal face and preparation condition, the morphology control synthesis to nano metal has guidance meaning
Justice.
Many methods are applied to prepare the nano copper particle of different-grain diameter, pattern, such as：Hydrothermal synthesis method, microemulsion method,
Thermal decomposition method, photochemical method and electrochemical deposition method.In these methods, " hard " template and " soft " template are widely used in control
The size of nano-particle, pattern, inductive formation different size, the nano copper particle of pattern.At present, using microwave, ultraviolet spoke
According to penetrance, selection heating property be heat source for reaction, select suitable organic modifier to carry out the high concentration of pattern, size Control
The synthesis of nano metal is just becoming the new direction of nano material synthesis.
Under the conditions of low-temp reaction, using microwave, ultraviolet irradiation, we have prepared mean diameter is 3-80 nm, size
It is distributed as the good nano copper particle of 2-108 nm, dispersive property.The method reaction condition is easily controllable, low cost, processing technology
Advantage with simple flow.
Content of the invention
The present invention propose a kind of by add the organic modifier containing different functional groups be used as control Nanometer Copper size
Template, under different exposure times, by change reaction condition parameter, the method preparing different-grain diameter Nanometer Copper.
Its preparation method is as follows：
Under microwave, ultraviolet irradiation, (microwave power is 500 w；Ultraviolet wavelength is 254 nm, and power for 500 w), will
In the 100 ml three-neck flasks that 0.1-0.5 mol/L copper nitrate is added to, after motor stirrer stirring 10min, add 5wt%-
20wt% organic modifier, dropwise Deca 0.2-2.5 mol/L sodium borohydride, reacts 30-120 min, obtains various sizes of
Nano copper particle.
The wherein above-mentioned organic modifier containing different functional groups refers to Sorbitol, double (p- sulfonyl-phenyl) benzene of two hydrations
Base phosphine di-potassium.
The addition of wherein organic modifier is：Add 0.05-1.0 g organic modifier according to every 40 ml copper nitrates.
The addition of wherein sodium borohydride is：Mol ratio according to sodium borohydride and copper nitrate is 2 ~ 5:1 ratio adds,
The concentration range of sodium borohydride is 0.2-2.5 mol/L.
The Nanometer Copper prepared with the method, grain diameter is little, even size distribution, good dispersion, and the method reaction
Condition is easily controllable, inexpensive, the advantage of processing technology and simple flow.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
Measure the 0.3 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The Sorbitol of 0.15 g is added after 10min.Under microwave exposure, the dropwise 0.6 mol/L sodium borohydride of Deca 40 ml, reaction
60 min.Reaction terminate after, obtain average diameter be 10 nm, distribution of sizes be 7 19 nm nano copper particle.
Embodiment 2
Measure the 0.1 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The Sorbitol of 0.1 g is added after 10min.Under microwave exposure, the dropwise 0.2 mol/L sodium borohydride of Deca 40 ml, reaction
30 min.Reaction terminate after, obtain average diameter be 3 nm, distribution of sizes be 25 nm nano copper particle.
Embodiment 3
Measure the 0.5 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The two of 1.0 g are added to be hydrated double (p- sulfonyl-phenyl) Phenylphosphine di-potassiums after 10min.Under microwave exposure, dropwise Deca 40
The 1.0 mol/L sodium borohydrides of ml, react 90 min.After reaction terminates, obtaining mean diameter is that 35 nm, particle diameter distribution are
The ball shaped nano copper granule of 10-50 nm.
Embodiment 4
Measure the 0.1 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The two of 0.2 g is added to be hydrated double (p- sulfonyl-phenyl) Phenylphosphine di-potassiums after 10min.Under microwave exposure, dropwise Deca 40
The 0.5 mol/L sodium borohydride of ml, reacts 120 min.After reaction terminates, obtaining average diameter is that 80 nm, distribution of sizes are
The nano copper particle of 30-108 nm.
Embodiment 5
Measure the 0.5 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The two of 0.5 g is added to be hydrated double (p- sulfonyl-phenyl) Phenylphosphine di-potassiums after 10min.Under ultraviolet irradiation, dropwise Deca 40
The 1.5 mol/L sodium borohydrides of ml, react 30 min.Reaction terminate after, obtain average diameter be 19 nm, distribution of sizes be 6-
The nano copper particle of 40 nm.
Embodiment 6
Measure the 0.3 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The Sorbitol of 0.6 g is added after 10min.Under ultraviolet irradiation, the dropwise 1.2 mol/L sodium borohydrides of Deca 40 ml, reaction
120 min.Reaction terminate after, obtain average diameter be 72 nm, distribution of sizes be 50-96 nm nano copper particle.
Embodiment 7
Measure the 0.1 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The Sorbitol of 0.05 g is added after 10min.Under ultraviolet irradiation, the dropwise 0.3 mol/L sodium borohydride of Deca 40 ml, reaction
90 min.Reaction terminate after, obtain average diameter be 12 nm, distribution of sizes be 6-22 nm nano copper particle.
Embodiment 8
Measure the 0.5 mol/L Cu (NO of 40 ml3)2, add in the three-neck flask of 100 ml, motor stirrer stirs
The Sorbitol of 1.0 g is added after 10min.Under ultraviolet irradiation, the dropwise 2.5 mol/L sodium borohydrides of Deca 40 ml, reaction
60 min.Reaction terminate after, obtain average diameter be 28 nm, distribution of sizes be 5-49 nm nano copper particle.
Claims (1)
1. under microwave or ultraviolet irradiation the synthetic method of different-grain diameter Nanometer Copper it is characterised in that preparation method is as follows：
Under microwave, ultraviolet irradiation, wherein microwave power is 500 w；Ultraviolet wavelength is 254 nm, and power is 500 w, by 0.1-
In the three-neck flask that 0.5 mol/L copper nitrate is added to, after motor stirrer stirring 10min, 5wt%-20wt% is added to have machine maintenance
Decorations agent, dropwise Deca sodium borohydride, reacts 30-120 min, obtains various sizes of nano copper particle；
Described organic modifier refers to Sorbitol or double (p- sulfonyl-phenyl) the Phenylphosphine di-potassium of two hydrations；
The addition of wherein organic modifier is：Add 0.05-1.0 g organic modifier according to every 40 ml copper nitrates；
The addition of wherein sodium borohydride is：Mol ratio according to sodium borohydride and copper nitrate is 2 ~ 5:1 ratio adds, boron hydrogen
The concentration range changing sodium is 0.2-2.5 mol/L.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101214554A (en) * | 2008-01-16 | 2008-07-09 | 上海第二工业大学 | One-step method preparing nano copper colloid water solution under ultrasonic field |
| CN101319357A (en) * | 2008-06-20 | 2008-12-10 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100809982B1 (en) * | 2006-09-21 | 2008-03-06 | 삼성전기주식회사 | Method for manufacturing copper nanoparticles using microwave |
| JP2011089153A (en) * | 2009-10-20 | 2011-05-06 | Mitsubishi Gas Chemical Co Inc | Method for producing copper fine particle |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101214554A (en) * | 2008-01-16 | 2008-07-09 | 上海第二工业大学 | One-step method preparing nano copper colloid water solution under ultrasonic field |
| CN101319357A (en) * | 2008-06-20 | 2008-12-10 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
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Inventor after: Wang Aili Inventor after: Yin Hengbo Inventor after: Dai Qiaowu Inventor after: Feng Yonghai Inventor before: Wang Aili Inventor before: Yin Hengbo Inventor before: Feng Yonghai |
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Effective date of registration: 20161230 Address after: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301 Applicant after: Jiangsu Univ. Applicant after: Affiliated Hospital of Jiangsu University Address before: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301 Applicant before: Jiangsu Univ. |
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