CN100431754C - Process for preparing gold nano particle by using aqueous phase soft mould plate method - Google Patents
Process for preparing gold nano particle by using aqueous phase soft mould plate method Download PDFInfo
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- CN100431754C CN100431754C CNB2007100201994A CN200710020199A CN100431754C CN 100431754 C CN100431754 C CN 100431754C CN B2007100201994 A CNB2007100201994 A CN B2007100201994A CN 200710020199 A CN200710020199 A CN 200710020199A CN 100431754 C CN100431754 C CN 100431754C
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Abstract
A method for preparing gold nanometer particles via water-phase soft template method uses water-phase soft template method, the soft group formed by carbowax (PEG) and dodecyl sodium sulfate (SDS) as soft template, mixes the water solution of chlorauric acid (HAuCl4) and said soft group, uses PEG as reducer to reduce the gold ion into gold nanometer particles in special shape and size. In reaction, the soft template and reaction period can control the size and shape of gold nanometer particles. And the reactant via high-speed eccentric treatment, deposition and washed via water to obtain the gold nanometer ball, tablet, ring or arc. The invention is characterized in narrow size and size distribution, with simple operation on shape control.
Description
Technical field
A kind of method of process for preparing gold nano particle by using aqueous phase soft mould plate belongs to nano particle preparing technical field in the metal material.The present invention relates to a kind of soft matter cluster that forms with polyethylene glycol (PEG) and lauryl sodium sulfate (SDS) is soft template, by polyethylene glycol as reducing agent, with gold chloride (HAuCl
4) be raw material, the water reducing process prepares the method for golden nanometer particle, and the gained golden nanometer particle can be nanosphere, nanometer sheet, nano-rings or nanometer arc.
Background technology
The golden nanometer particle of special shape, as ball, sheet, ring or arc particle more and more widely in the application of aspects such as catalysis, biomedicine and photoelectron device, especially at molecular labeling, chemical sensitisation, there is very big using value aspects such as nanoelectronic device.For example preparing gold nano ring method at present both at home and abroad is as hard template, then by displacement reaction generation gold nano ring by Nano silver piece.This kind method is easy to take place side reaction, complicated operation and product separation difficulty, and easily pollute.Polyethylene glycol of using among the present invention (PEG) and lauryl sodium sulfate (SDS) can self assembly form soft matter cluster in the aqueous solution; By the effect of soft template, the golden nanometer particle of the given shapes such as ball, sheet, ring or arc that the golden nanometer particle self assembly formed respectively have narrow distribution is not seen relevant report at present both at home and abroad as yet.
Summary of the invention
The object of the invention is: provide a kind of aqueous phase soft mould plate legal system to be equipped with the gold nano ball, nanometer sheet, the method of nano-rings or nanometer arc, utilize the soft template of the soft matter cluster of polyethylene glycol (PEG) and lauryl sodium sulfate (SDS) formation as the preparation golden nanometer particle, with PEG as reducing agent, electronation gold chloride in the aqueous solution, by adjusting soft template and reaction time, prepare the about 20 ± 5nm gold nano of the narrower particle mean size of distribution of shapes ball respectively, about 500 ± 50nm the gold-nano-piece of diameter, diameter about 500 ± 50nm gold nano ring or length are about the golden nanometer particle product of 200-300nm gold nano arc.
Technical scheme of the present invention: utilize the soft template of the soft matter cluster of polyethylene glycol and lauryl sodium sulfate formation as the preparation golden nanometer particle, aqueous solution of chloraurate is joined in the above-mentioned soft matter cluster aqueous solution, utilize polyethylene glycol as reducing agent, adjust the polyethylene glycol mean molecule quantity and the control reaction time of soft template, gold ion is reduced into the golden nanometer particle of specific morphology, and technology is:
A certain amount of polyethylene glycol 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, 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, polyethylene glycol 60-120g/L, lauryl sodium sulfate 3-15mmol/L, room temperature, after 400r/min stirs 1min under the normal pressure, at 25 ± 1 ℃ of lucifuge reaction 2-480h, reaction is used 3000-10000r/min supercentrifuge centrifugation product with reaction solution after finishing, and the precipitate with deionized water washing obtains the golden nanometer particle product three times.
The mean molecule quantity of used polyethylene glycol is 8000-180000.
The polyethylene glycol mean molecule quantity of adjusting soft template is 8000 and controls reaction time 2-6h that products obtained therefrom is the gold nano ball.
The polyethylene glycol mean molecule quantity of adjusting soft template is 20000 and controls reaction time 24-48h that products obtained therefrom is a gold-nano-piece.
The polyethylene glycol mean molecule quantity of adjusting soft template is 10000 and controls reaction time 180-240h that products obtained therefrom is the gold nano ring.
The polyethylene glycol mean molecule quantity of adjusting soft template is 180000 and controls reaction time 400-480h that products obtained therefrom is the gold nano arc.
Beneficial effect of the present invention: polyethylene glycol of using among the present invention (PEG) and lauryl sodium sulfate (SDS) can self assembly form soft matter cluster as protective agent in the aqueous solution; Wherein PEG is again the reducing agent of gold chloride simultaneously.The present invention utilizes the soft template of the soft matter cluster of PEG and SDS formation as the preparation golden nanometer particle, and in conjunction with controlling reaction time, pattern and the particle diameter that can regulate and control nano particle distribute, and obtain the golden nanometer particle that ball, sheet, ring or arc etc. have specific morphology and narrow particle diameter distribution characteristics easily respectively.
Application the present invention produces golden nanometer particle and has the reaction condition gentleness, does not need additional reducing agent, reactions steps to be reduced to a step, and easy and simple to handle, the segregative characteristics of product have 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, environmental friendliness.
Description of drawings
The sem photograph of the transmission electron microscope picture of Fig. 1 gold nano ball (a) and gold nano ring (c) and gold-nano-piece (b) and gold nano arc (d).
The specific embodiment
Embodiment 1SDS-PEG (PEG mean molecule quantity 8000) soft template is synthesized the gold nano ball.
A certain amount of PEG 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 0.1mmol/L, PEG 60g/L, SDS 5mmol/L.Behind the stir about 1min (400r/min), (25 ± 1) ℃ lucifuge is reacted 2-6h near room temperature under room temperature, the normal pressure.Reaction is used supercentrifuge centrifugal (10000r/min) separated product with reaction solution after finishing, and the precipitate with deionized water washing obtains color of spherical gold three times, and its average grain diameter is 20 ± 5nm.
Embodiment 2SDS-PEG (PEG mean molecule quantity 20000) soft template is synthesized gold-nano-piece.
A certain amount of PEG 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 0.5mmol/L, PEG 85g/L, SDS 10mmol/L.Behind the stir about 1min (400r/min), (25 ± 1) ℃ lucifuge is reacted 24-48h near room temperature under room temperature, the normal pressure.Reaction is used supercentrifuge centrifugal (3000r/min) separated product with reaction solution after finishing, and the precipitate with deionized water washing obtains gold-nano-piece three times, and its average diameter is 500 ± 50nm.
Embodiment 3SDS-PEG (PEG mean molecule quantity 10000) soft template is synthesized the gold nano ring.
A certain amount of PEG 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 0.3mmol/L, PEG 120g/L, SDS 3mmol/L.Behind the stir about 1min (400r/min), (25 ± 1) ℃ lucifuge is reacted 180-240h near room temperature under room temperature, the normal pressure.Reaction is used supercentrifuge centrifugal (3000r/min) separated product with reaction solution after finishing, and the precipitate with deionized water washing obtains the gold nano ring three times, and its average diameter is 500 ± 50nm.
Embodiment 4SDS-PEG (PEG mean molecule quantity 180000) soft template is synthesized the gold nano arc.
A certain amount of PEG 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 1mmol/L, PEG 70g/L, SDS 15mmol/L.Behind the stir about 1min (400r/min), (25 ± 1) ℃ lucifuge is reacted 400-480h near room temperature under room temperature, the normal pressure.Reaction is used supercentrifuge centrifugal (8000r/min) separated product with reaction solution after finishing, and the precipitate with deionized water washing obtains the gold nano arc three times, and its average length is 250 ± 50nm.
Claims (6)
1. the method for a process for preparing gold nano particle by using aqueous phase soft mould plate, it is characterized in that utilizing the soft template of the soft matter cluster of polyethylene glycol and lauryl sodium sulfate formation as the preparation golden nanometer particle, aqueous solution of chloraurate is joined in the above-mentioned soft matter cluster aqueous solution, utilize polyethylene glycol as reducing agent, adjust the polyethylene glycol mean molecule quantity and the control reaction time of soft template, gold chloride is reduced into the golden nanometer particle of specific morphology, and technology is:
A certain amount of polyethylene glycol 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, 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, polyethylene glycol 60-120g/L, lauryl sodium sulfate 3-15mmol/L, room temperature, after 400r/min stirs 1min under the normal pressure, at 25 ± 1 ℃ of lucifuge reaction 2-480h, reaction is used 3000-10000r/min supercentrifuge centrifugation product with reaction solution after finishing, and the precipitate with deionized water washing obtains the golden nanometer particle product three times.
2. method according to claim 1, the mean molecule quantity that it is characterized in that used polyethylene glycol is 8000-180000.
3. method according to claim 1 is characterized in that the polyethylene glycol mean molecule quantity of adjusting soft template is 8000 and controls reaction time 2-6h that products obtained therefrom is the gold nano ball.
4. method according to claim 1 is characterized in that the polyethylene glycol mean molecule quantity of adjusting soft template is 20000 and controls reaction time 24-48h that products obtained therefrom is a gold-nano-piece.
5. method according to claim 1 is characterized in that the polyethylene glycol mean molecule quantity of adjusting soft template is 10000 and controls reaction time 180-240h that products obtained therefrom is the gold nano ring.
6. method according to claim 1 is characterized in that the polyethylene glycol mean molecule quantity of adjusting soft template is 180000 and controls reaction time 400-480h that products obtained therefrom is the gold nano arc.
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| CN102921958A (en) * | 2012-11-06 | 2013-02-13 | 上海交通大学 | Method for preparing luminous nano-silver with pH adjusting phase transfer behaviors |
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| CN109865844B (en) * | 2018-03-16 | 2022-03-15 | 南京林业大学 | Preparation method of flaky cobalt powder |
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