CN1994634A - Method for preparing polypodia shaped Au nanoparticle using microwave to promote water phase soft template - Google Patents
Method for preparing polypodia shaped Au nanoparticle using microwave to promote water phase soft template Download PDFInfo
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- CN1994634A CN1994634A CN 200610166435 CN200610166435A CN1994634A CN 1994634 A CN1994634 A CN 1994634A CN 200610166435 CN200610166435 CN 200610166435 CN 200610166435 A CN200610166435 A CN 200610166435A CN 1994634 A CN1994634 A CN 1994634A
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Abstract
The invention uses microwave accelerating water-phase soft template method to prepare multi-foot gold nanometer particles, wherein it uses polyvinyl pyrrolidon (PVP) and sodium dodecyl sulfate (SDS0 to form soft group as soft template; mixes water solution with chlorauric acid (HAuCl4) with said soft group; under microwave radiation, using sodium citrate as reducer to quickly reduce gold ion into multi-food gold nanometer particles; in the reaction, the soft template formed by PVP and SDS will control the shape and size of gold nanometer particles; high-speed eccentrically treating the reaction product, depositing and washing with water to obtain the multi-food gold nanometer particles at 20-50mm and narrow diameter distribution. The invention has low consumption of surface activator, short process, simple separation and easy preparation.
Description
Technical field
Be equipped with the method for polypody shape golden nanometer particle with the microwave to promote water phase soft template legal system, the present invention relates to a kind of soft matter cluster that forms with polyvinylpyrrolidone (PVP) and lauryl sodium sulfate (SDS) is soft template, with gold chloride (HAuCl
4) and natrium citricum be raw material, promote the water reducing process to prepare the method for polypody shape golden nanometer particle with microwave.Belong to nano particle preparing technical field in the metal material.
Background technology
Because polypody shape golden nanometer particle has special shape and optical property, they in the application of catalysis, photoelectron device and biomedical aspect more and more widely, especially at molecular labeling, chemical sensitisation, there is very big using value aspects such as nanoelectronic device.Polypody shape golden nanometer particle itself also can be used as potential template and removes the further nano particle of synthetic different structure.At present both at home and abroad the method for synthetic polypody shape golden nanometer particle mainly be by with little Nano silver grain or golden nanometer particle as seed, in the aqueous solution, divide one-step inducing to prepare polypody shape golden nanometer particle (granularity 30-500nm) through chemical reduction method.The gold nanometer particle grain size of these methods preparations distributes wide, and the reaction time is grown (1-20 days), needs the surfactant of high concentration, and product separation difficulty and cost are higher.
Summary of the invention
The object of the invention is: a kind of method that is equipped with polypody shape golden nanometer particle with the microwave to promote water phase soft template legal system is provided, utilize the soft template of the soft matter cluster of polyvinylpyrrolidone (PVP) and lauryl sodium sulfate (SDS) formation, be equipped with the about 20-50nm of particle mean size and have the method for the polypody shape golden nanometer particle of narrow particle diameter distribution characteristics with the microwave to promote water phase soft template legal system as the preparation golden nanometer particle.
Technical scheme of the present invention: utilize the soft template of the soft matter cluster of PVP and SDS formation as the preparation golden nanometer particle, thus regulation and control golden nanometer particle pattern and size; To contain gold chloride (HAuCl
4) the aqueous solution and above-mentioned soft matter cluster aqueous solution, under microwave irradiation effect, use natrium citricum fast gold chloride to be reduced into polypody shape golden nanometer particle as reducing agent.Product washes the polypody shape golden nanometer particle that obtains the about 20-50nm of granularity and have narrow particle diameter distribution characteristics with water after high speed centrifugation separates.
Concrete technology is: a certain amount of PVP and SDS are joined in the deionized water, being heated to 40-60 ℃ fully dissolves it and is self-assembled into soft matter cluster, treat that solution is cooled to after the room temperature and the aqueous solution that contains gold chloride, make that each component ultimate density is respectively in the solution: gold chloride 0.1-1mmol/L, PVP 0.1-10g/L, SDS0.3-15mmol/L.Heat above-mentioned solution to boiling, add the sodium citrate aqueous solution of 8.5mmol/L then rapidly, the molar ratio of gold chloride and natrium citricum is 1: 10-30, and behind the stir about 10s (400r/min), put into microwave field heating 1-5min and carry out reduction reaction.After reaction finishes reaction solution used supercentrifuge centrifugal (10,000r/min) separated product, the precipitate with deionized water washing obtains product three times.
The PVP that uses in the said method is the polymer of mean molecule quantity between 8000 to 360000.
The microwave power that uses in the said method is between 100-1200W.
Beneficial effect of the present invention: polyvinylpyrrolidone of using among the present invention (PVP) and lauryl sodium sulfate (SDS) can self assembly form soft matter cluster as protective agent in the aqueous solution; And the soft matter cluster that can form shape under the different condition and vary in size.The present invention is in the auxiliary soft template of utilizing the soft matter cluster of PVP and SDS formation as the preparation golden nanometer particle down of microwave radiation, the particle diameter that can regulate and control nano particle distributes the polypody shape golden nanometer particle that obtains the about 20-50nm of diameter easily and have narrow particle diameter distribution characteristics.
Application the present invention produces polypody shape golden nanometer particle and has the time weak point, and easy and simple to handle, dosage of surfactant is few, product separates the characteristics of being easy to, and has reduced cost.
Employed reducing agent and protective agent can be through simple washing and centrifugal removing after reaction is finished among the present invention, so the end-product impurities is few, purity is high.
Description of drawings
The transmission electron microscope picture of Fig. 1 polypody shape golden nanometer particle and corresponding electron diffraction diagram.
The specific embodiment
Embodiment 1SDS-PVP (mean molecule quantity 8000) soft template is synthesized polypody shape golden nanometer particle
A certain amount of SDS and PVP are joined in the deionized water, being heated to 40-60 ℃ fully dissolves it and is self-assembled into soft matter cluster, after treating that solution is cooled to room temperature, with this solution and the aqueous solution that contains gold chloride, make that each component ultimate density is respectively in the solution: gold chloride 0.6mmol/L, PVP 0.1mmol/L, SDS0.3mmol/L.Heat above-mentioned solution to boiling, add the sodium citrate aqueous solution of 8.5mmol/L then rapidly, the molar ratio of gold chloride and natrium citricum is 1: 17, and behind the stir about 10s (400r/min), puts into microwave field (200W) heating 4min and carry out reduction reaction.After reaction finishes reaction solution used supercentrifuge centrifugal (10,000r/min) separated product, precipitation obtains polypody shape golden nanometer particle for three times through water washing, its average grain diameter is 50nm.
Embodiment 2SDS-PVP (mean molecule quantity 360000) soft template is synthesized polypody shape golden nanometer particle
A certain amount of SDS and PVP are joined in the deionized water, being heated to 40-60 ℃ fully dissolves it and is self-assembled into soft matter cluster, after treating that solution is cooled to room temperature, with this solution and the aqueous solution that contains gold chloride, make that each component ultimate density is respectively in the solution: gold chloride 1mmol/L, PVP 10mmol/L, SDS12mmol/L.Heat above-mentioned solution to boiling, add the sodium citrate aqueous solution of 8.5mmol/L then rapidly, the molar ratio of gold chloride and natrium citricum is 1: 10, and behind the stir about 10s (400r/min), puts into microwave field (1000W) heating 1min and carry out reduction reaction.After reaction finishes reaction solution used supercentrifuge centrifugal (10,000r/min) separated product, precipitation obtains polypody shape golden nanometer particle for three times through water washing, its average grain diameter is 25nm.
Embodiment 3SDS-PVP (mean molecule quantity 40000) soft template is synthesized polypody shape golden nanometer particle
A certain amount of SDS and PVP are joined in the deionized water, being heated to 40-60 ℃ fully dissolves it and is self-assembled into soft matter cluster, after treating that solution is cooled to room temperature, with this solution and the aqueous solution that contains gold chloride, make that each component ultimate density is respectively in the solution: gold chloride 0.3mmol/L, PVP 5mmol/L, SDS6mmol/L.Heat above-mentioned solution to boiling, add the sodium citrate aqueous solution of 8.5mmol/L then rapidly, the molar ratio of gold chloride and natrium citricum is 1: 30, and behind the stir about 10s (400r/min), puts into microwave field (500W) heating 2.5min and carry out reduction reaction.After reaction finishes reaction solution used supercentrifuge centrifugal (10,000r/min) separated product, water washing obtains polypody shape golden nanometer particle for three times, its average grain diameter is 45nm.
Claims (3)
1. method that is equipped with polypody shape golden nanometer particle with the microwave to promote water phase soft template legal system, it is characterized in that utilizing the soft template of the soft matter cluster of polyvinylpyrrolidone and lauryl sodium sulfate formation as the preparation golden nanometer particle, gold chloride is joined in the above-mentioned soft matter cluster aqueous solution, under microwave irradiation effect, use natrium citricum as reducing agent, fast gold ion is reduced into polypody shape golden nanometer particle, technology is:
A certain amount of polyvinylpyrrolidone and lauryl sodium sulfate are joined in the deionized water, being heated to 40-60 ℃ fully dissolves it and is self-assembled into soft matter cluster, after treating that solution is cooled to room temperature, with this solution and the aqueous solution that contains gold chloride, make that each component ultimate density is respectively in the solution: gold chloride 0.1-1mmol/L, polyvinylpyrrolidone 0.1-10g/L, lauryl sodium sulfate 0.3-15mmol/L, heat above-mentioned solution to boiling, the sodium citrate aqueous solution that adds 8.5mmol/L then rapidly, the molar ratio of gold chloride and natrium citricum is 1: 10-30, and after stirring 10 seconds with 400 rev/mins, put into the microwave field heating and carried out reduction reaction in 1-5 minute, reaction is used the supercentrifuge centrifugation with reaction solution after finishing, the washing of gained precipitate with deionized water obtains polypody shape golden nanometer particle three times, and its average grain diameter is 20-50nm.
2. method according to claim 1, the mean molecule quantity that it is characterized in that described polyvinylpyrrolidone is 8000-360000.
3. method according to claim 1, the power that it is characterized in that described microwave radiation is 100-1200W.
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Cited By (1)
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| CN102426157A (en) * | 2011-11-16 | 2012-04-25 | 江南大学 | Method for analyzing tyrosinase activity based on functional Au nanoparticles |
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| CN1322952C (en) * | 2004-09-24 | 2007-06-27 | 昆明贵金属研究所 | Indirecting light chemical preparation for gold nanometer material |
| CN1302849C (en) * | 2004-12-02 | 2007-03-07 | 黄德欢 | Method for preparing supported nano gold powder |
| CN1876292A (en) * | 2006-06-02 | 2006-12-13 | 中国科学院长春应用化学研究所 | Nanometer gold grain microwave synthesis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102426157A (en) * | 2011-11-16 | 2012-04-25 | 江南大学 | Method for analyzing tyrosinase activity based on functional Au nanoparticles |
| CN102426157B (en) * | 2011-11-16 | 2013-02-27 | 江南大学 | Method for analyzing tyrosinase activity based on functional Au nanoparticles |
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