CN103464778A - Synthetic method of nanometer copper particles different in particle size under irradiation of microwave and ultraviolet - Google Patents
Synthetic method of nanometer copper particles different in particle size under irradiation of microwave and ultraviolet Download PDFInfo
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- CN103464778A CN103464778A CN2013103975920A CN201310397592A CN103464778A CN 103464778 A CN103464778 A CN 103464778A CN 2013103975920 A CN2013103975920 A CN 2013103975920A CN 201310397592 A CN201310397592 A CN 201310397592A CN 103464778 A CN103464778 A CN 103464778A
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Abstract
The invention relates to a synthetic method of nanometer copper particles different in particle size under the irradiation of microwave and ultraviolet and belongs to the field of nanometer functional materials. The synthetic method includes the steps: under the irradiation of the microwave and the ultraviolet, adding 0.1-0.5mol/L of copper nitrate into a 100ml three-necked flask, stirring for 10mins by a motor stirrer prior to adding, by weight, 5-20% of organic modifier, adding 0.2-2.5mol/L reducing agent sodium borohydride by drops after solution is raised to a reaction temperature, and reacting for 30-120mins to obtain the nanometer copper particles different in particle size. Average particle size of the nanometer copper particles is 3-80 nanometers with size distribution ranging from 2 nanometers to 108 nanometers. The synthetic method has the advantages that nanometer copper is small in particle size, uniform in size distribution, good in dispersion, easy to control in reaction conditions and low in cost, and has simple and convenient production technology and process.
Description
Technical field
The present invention relates to the synthetic method of different-grain diameter Nanometer Copper under microwave, ultraviolet irradiation, refer in particular under microwave, ultraviolet irradiation, add containing polyhydric organic compound and refer in particular to sorbierite, two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of two hydrations, prepare the method for different size Nanometer Copper under the differential responses condition, belonged to the nano-functional material field.
Background technology
Nano metal has at aspects such as catalysis, photochemistry, magnetic, conduction, biologies the physicochemical characteristics that is different from the reguline metal material, and the pattern of nano-metal particle directly has influence on these character.The pattern of nano metal is controlled and is synthesized the important directions that belongs to the investigation of materials field with application study, utilize surfactant to participate in chemical synthesis, preparation and the application study of carrying out the nano metal of particle size and pattern control have far-reaching theory and using value.The slaine of copper of take is parent, in the aqueous solution or organic solution, utilizes the organic modifier (as many carboxyls, polyhydroxy organic matter etc.) with different functional groups, at different preparation conditions, carries out the study on the synthesis of the Nanometer Copper that particle size and pattern control.The Nanometer Copper pattern is controlled study on the synthesis and has been disclosed the formation of nano metal crystal face and the relation of preparation condition, and the pattern of nano metal is controlled to the synthetic directive significance that has.
Many methods are applied to preparing the nano copper particle of different-grain diameter, pattern, as: hydrothermal synthesis method, microemulsion method, thermal decomposition method, photochemical method and electrochemical deposition method.In these methods, " firmly " template and " soft " template are widely used in size, the pattern of controlling nano particle, induce the nano copper particle that has generated different size, pattern.At present, utilizing the penetrability of microwave, ultraviolet irradiation, selection heating property is heat source for reaction, selects suitable organic modifier to carry out the synthetic synthetic new direction of nano material that just becoming of the highly concentrated nano metal of pattern, size Control.
Under the low-temp reaction condition, utilize microwave, ultraviolet irradiation, we have prepared average grain diameter is the nano copper particle that 3-80 nm, distribution of sizes are 2-108 nm, dispersive property is good.The method reaction condition is easy to control, low cost, the advantage of manufacture craft and simple flow.
Summary of the invention
The present invention proposes a kind of organic modifier that contains different functional groups by interpolation as the template of controlling the Nanometer Copper size, under different exposure times, by changing the reaction condition parameter, prepare the method for 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, power is 500 w), in the 100 ml three-neck flasks that 0.1-0.5 mol/L copper nitrate is joined, electric mixer adds the 5wt%-20wt% organic modifier after stirring 10min, dropwise drip 0.2-2.5 mol/L sodium borohydride, react 30-120 min, obtain the nano copper particle of different size.
Wherein the above-mentioned organic modifier that contains different functional groups refers to sorbierite, two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of two hydrations.
Wherein the addition of organic modifier is: according to every 40 ml copper nitrates, add 0.05-1.0 g organic modifier.
Wherein the addition of sodium borohydride is: the ratio that is 2 ~ 5:1 according to the mol ratio of sodium borohydride and copper nitrate adds, and the concentration range of sodium borohydride is 0.2-2.5 mol/L.
The Nanometer Copper prepared by the method, grain diameter is little, even size distribution, good dispersion, and also the method reaction condition is easy to control, low cost, the advantage of manufacture craft and simple flow.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
Measure the 0.3 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add the sorbierite of 0.15 g after electric mixer stirring 10min.Under microwave irradiation, dropwise drip the 0.6 mol/L sodium borohydride of 40 ml, react 60 min.After reaction finishes, obtaining average diameter is the nano copper particle that 10 nm, distribution of sizes are 7 – 19 nm.
Embodiment 2
Measure the 0.1 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add the sorbierite of 0.1 g after electric mixer stirring 10min.Under microwave irradiation, dropwise drip the 0.2 mol/L sodium borohydride of 40 ml, react 30 min.After reaction finishes, obtaining average diameter is the nano copper particle that 3 nm, distribution of sizes are 2 – 5 nm.
Embodiment 3
Measure the 0.5 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add two (p-sulfonyl-phenyl) Phenylphosphine di-potassiums of two hydrations of 1.0 g after electric mixer stirring 10min.Under microwave irradiation, dropwise drip the 1.0 mol/L sodium borohydrides of 40 ml, react 90 min.After reaction finishes, obtaining average grain diameter is the ball shaped nano copper particle that 35 nm, particle diameter are distributed as 10-50 nm.
Embodiment 4
Measure the 0.1 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add two (p-sulfonyl-phenyl) Phenylphosphine di-potassiums of two hydrations of 0.2 g after electric mixer stirring 10min.Under microwave irradiation, dropwise drip the 0.5 mol/L sodium borohydride of 40 ml, react 120 min.After reaction finishes, obtaining average diameter is the nano copper particle that 80 nm, distribution of sizes are 30-108 nm.
Embodiment 5
Measure the 0.5 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add two (p-sulfonyl-phenyl) Phenylphosphine di-potassiums of two hydrations of 0.5 g after electric mixer stirring 10min.Under ultraviolet irradiation, dropwise drip the 1.5 mol/L sodium borohydrides of 40 ml, react 30 min.After reaction finishes, obtaining average diameter is the nano copper particle that 19 nm, distribution of sizes are 6-40 nm.
Embodiment 6
Measure the 0.3 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add the sorbierite of 0.6 g after electric mixer stirring 10min.Under ultraviolet irradiation, dropwise drip the 1.2 mol/L sodium borohydrides of 40 ml, react 120 min.After reaction finishes, obtaining average diameter is the nano copper particle that 72 nm, distribution of sizes are 50-96 nm.
Embodiment 7
Measure the 0.1 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add the sorbierite of 0.05 g after electric mixer stirring 10min.Under ultraviolet irradiation, dropwise drip the 0.3 mol/L sodium borohydride of 40 ml, react 90 min.After reaction finishes, obtaining average diameter is the nano copper particle that 12 nm, distribution of sizes are 6-22 nm.
Embodiment 8
Measure the 0.5 mol/L Cu (NO of 40 ml
3)
2, add in the three-neck flask of 100 ml, add the sorbierite of 1.0 g after electric mixer stirring 10min.Under ultraviolet irradiation, dropwise drip the 2.5 mol/L sodium borohydrides of 40 ml, react 60 min.After reaction finishes, obtaining average diameter is the nano copper particle that 28 nm, distribution of sizes are 5-49 nm.
Claims (4)
1. the synthetic method of different-grain diameter Nanometer Copper under microwave, ultraviolet irradiation is characterized in that the 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, in the three-neck flask that 0.1-0.5 mol/L copper nitrate is joined, electric mixer adds the 5wt%-20wt% organic modifier after stirring 10min, dropwise drip sodium borohydride, react 30-120 min, obtain the nano copper particle of different size.
2. the synthetic method of different-grain diameter Nanometer Copper under microwave according to claim 1, ultraviolet irradiation, is characterized in that described organic modifier refers to sorbierite, two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of two hydrations.
3. the synthetic method of different-grain diameter Nanometer Copper under microwave according to claim 1, ultraviolet irradiation, is characterized in that wherein the addition of organic modifier is: according to every 40 ml copper nitrates, add 0.05-1.0 g organic modifier.
4. the synthetic method of different-grain diameter Nanometer Copper under microwave according to claim 1, ultraviolet irradiation, it is characterized in that wherein the addition of sodium borohydride is: the ratio that is 2 ~ 5:1 according to the mol ratio of sodium borohydride and copper nitrate adds, and the concentration range of sodium borohydride is 0.2-2.5 mol/L.
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Citations (6)
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| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| US20080072706A1 (en) * | 2006-09-21 | 2008-03-27 | Samsung Electro-Mechanics Co. Ltd. | Method for manufacturing copper nanoparticles using microwaves |
| 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 |
| JP2011089153A (en) * | 2009-10-20 | 2011-05-06 | Mitsubishi Gas Chemical Co Inc | Method for producing copper fine particle |
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2013
- 2013-09-05 CN CN201310397592.0A patent/CN103464778B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080072706A1 (en) * | 2006-09-21 | 2008-03-27 | Samsung Electro-Mechanics Co. Ltd. | Method for manufacturing copper nanoparticles using microwaves |
| 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 |
| JP2011089153A (en) * | 2009-10-20 | 2011-05-06 | Mitsubishi Gas Chemical Co Inc | Method for producing copper fine particle |
| 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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