CN101433966B - Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method - Google Patents
Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method Download PDFInfo
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Abstract
The invention relates to a method for preparing tadpole-shaped gold nano-particles by a microwave accelerating water-phase soft template method. The method for preparing tadpole-shaped gold nano-particles comprises the following steps: polyethylene glycol (PEG), sodium dodecyl sulfate (SDS), and sodium sulfate (Na2SO4) self-assemble into soft matter clusters in an aqueous solution to form soft templates for preparing gold nano-particles; and chloroauric acid is added into the aqueous solution containing the soft matter clusters to be reduced chemically in the aqueous solution by the polyethylene glycol (PEG) serving as a reducing agent under the condition of radiation of ultrasonic waves and 300 to 400 nanometers of tadpole-shaped gold nanoparticle products are prepared by adjusting the soft templates. The method for preparing the tadpole-shaped gold nanoparticles uses radiation of ultrasonic waves and self-reduction of macromolecules instead of reduction by ultraviolet light and takes polyethylene glycol (PEG) as the reducing agent to reduce the chloroauric acid in the aqueous solution chemically to reduce gold irons into the tadpole-shaped gold nanoparticles. The final products of the invention contain few impurities and high purity. The method uses less surface active agent and saves cost.
Description
Technical field
The present invention relates to nanometer particle process method in a kind of metal material, particularly a kind of method that is equipped with tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system.
Background technology
The golden nanometer particle of special shape, as ball, sheet or band shape particle at molecular labeling, chemical sensitisation, aspects such as nanoelectronic device have very big using value, and are increasingly extensive in the application of aspects such as catalysis, biomedicine and photoelectron device.For example the method for preparing gold-nano-piece or nanometer band at present both at home and abroad adopts template more, and this method is simple to operate, convenient separation.
Patent publication No. is that the patent of invention of CN101091992 discloses a kind of method for preparing color of spherical gold with ultrasonic wave promotion photo-reduction in aqueous phase soft mould, it is to use the soft matter cluster of polyethylene glycol (PEG) and lauryl sodium sulfate (SDS) formation as preparation golden nanometer particle soft template, promote photo-reduction with ultrasonic wave, under the ultraviolet light reduction, divide one-step inducing synthetic, obtain not having inorganic salts Na
2SO
4The color of spherical gold that participates in.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method that is equipped with tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind ofly being equipped with the method for tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system, is to utilize polyethylene glycol (PEG), lauryl sodium sulfate (SDS) and sodium sulphate (Na
2SO
4) in the aqueous solution, can self assembly form soft matter cluster, form the soft template of preparation golden nanometer particle, gold chloride is joined in the described soft matter cluster aqueous solution, under the ultrasonic radiation effect by polyethylene glycol (PEG) as reducing agent, electronation gold chloride in the aqueous solution, by adjusting soft template, preparation length is the tadpole shape golden nanometer particle product of 300-400nm.Gold ion is reduced into tadpole shape golden nanometer particle, and its technology is:
(1) join polyethylene glycol, lauryl sodium sulfate, sodium sulphate and gold chloride in the deionized water respectively, be heated to 41-59 ℃ it fully dissolved, obtain containing the 4# solution of the 3# solution of 2# solution, 100mmol/L sodium sulphate of 1# solution, the 520mmol/L lauryl sodium sulfate of 0.3-35mmol/L polyethylene glycol and 240mmol/L gold chloride respectively and be cooled to 25-30 ℃ stand-by;
(2) get an amount of 1-4# solution mixing and adding deionized water respectively, make 5# solution; Each component ultimate density in the 5# solution is respectively: gold chloride 0.1-1mmol/L, polyethylene glycol 0.5-20mmol/L, lauryl sodium sulfate 40-80mmol/L, sodium sulphate 0.2-10mmol/L;
(3) with 5# solution under normal pressure, after 400r/min stirs 1min, at 30 ± 1 ℃, lucifuge, ultrasonic wave radiation effects reaction 15-20h down, make 6# solution after the reaction end again;
(4) with carrying out centrifugal dehydration in the 6# solution input 3000-10000r/min supercentrifuge, obtain the precipitation separation product;
(5) with deionized water the precipitation separation product that step (4) obtains is washed three times, make the golden nanometer particle product.
The mean molecule quantity of described polyethylene glycol is 5990-179990.
The power of described ultrasonic wave radiation is 20-99W and 101-150W.
The invention has the beneficial effects as follows:
1, the present invention adopts polyethylene glycol (PEG) and lauryl sodium sulfate (SDS) as protective agent, utilizes sodium sulphate (Na
2SO
4) control self assembly formation soft matter cluster in the aqueous solution, and the soft matter cluster that can form shape under the different condition and vary in size.
2, the present invention utilizes polyethylene glycol (PEG), lauryl sodium sulfate (SDS) and sodium sulphate (Na under ultrasonic radiation is auxiliary
2SO
4) soft matter cluster that forms is as the soft template of preparation golden nanometer particle, the particle diameter that can regulate and control nano particle distributes the tadpole shape golden nanometer particle that obtains the about 300-400nm of diameter easily and have narrow particle diameter distribution characteristics.
3, do not need ultraviolet light reduction, but utilize ultrasonic wave radiation effects and big molecule autoreduction ability, by polyethylene glycol (PEG) as reducing agent, electronation gold chloride in the aqueous solution.
4. 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.
5. the present invention's method of producing tadpole shape golden nanometer particle has easy and simple to handlely, and dosage of surfactant is few, product separates easily and advantage with low cost.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the tadpole shape golden nanometer particle of the embodiment of the invention 1 preparation.
Fig. 2 is the transmission electron microscope picture of the tadpole shape golden nanometer particle of the embodiment of the invention 2 preparations.
Fig. 3 is the transmission electron microscope picture of the tadpole shape golden nanometer particle of the embodiment of the invention 3 preparations.
The specific embodiment
The present invention is further described below in conjunction with drawings and Examples.
Embodiment 1; Na
2SO
4The method of the synthetic tadpole shape golden nanometer particle of-SDS-PEG (mean molecule quantity 5900) soft template:
(1) join polyethylene glycol, lauryl sodium sulfate, sodium sulphate and gold chloride in the deionized water respectively, be heated to 47 ℃ it fully dissolved, obtain containing the 4# solution of the 3# solution of 2# solution, 100mmol/L sodium sulphate of 1# solution, the 520mmol/L lauryl sodium sulfate of 35mmol/L polyethylene glycol and 240mmol/L gold chloride respectively and be cooled to 26 ℃ stand-by;
(2) get an amount of 1-4# solution mixing and adding deionized water respectively, make 5# solution; Each component ultimate density in the 5# solution is respectively: gold chloride 0.1mmol/L, polyethylene glycol (PEG) 16mmol/L, lauryl sodium sulfate (SDS) 80mmol/L, sodium sulphate (Na
2SO
4) 0.2mmol/L;
(3) with 5# solution under normal pressure, after 400r/min stirs 1min, at 30 ± 1 ℃, lucifuge, ultrasonic power 140W radiation effects reaction 20h down, make 6# solution after the reaction end again;
(4) 6# solution is imported in the 3000 r/min supercentrifuges carried out centrifugal dehydration, obtain the precipitation separation product;
(5) with deionized water the precipitation separation product that step (4) obtains is washed three times, make golden nanometer particle product as shown in Figure 1, nano particle average length 300nm.
Embodiment 2; Na
2SO
4The method of the synthetic tadpole shape golden nanometer particle of-SDS-PEG (mean molecule quantity 179000) soft template:
(1) polyethylene glycol, lauryl sodium sulfate, sodium sulphate and gold chloride are joined respectively in the deionized water, be heated to 58 ℃ make the 4# solution of its 2# solution, 100mmol/L sodium sulphate 3# solution and 240mmol/L gold chloride that fully dissolves the 1# solution that obtains containing the 0.35mmol/L polyethylene glycol respectively, 520mmol/L lauryl sodium sulfate and be cooled to 28 ℃ stand-by;
(2) get an amount of 1-4# solution mixing and adding deionized water respectively, make 5# solution; Each component ultimate density in the 5# solution is respectively: gold chloride 1mmol/L, polyethylene glycol (PEG) 0.5mmol/L, lauryl sodium sulfate (SDS) 40mmol/L, sodium sulphate (Na
2SO
4) 8mmol/L;
(3) with 5# solution under normal pressure, after 400r/min stirs 1min, at 30 ± 1 ℃, lucifuge, ultrasonic power 50W radiation effects reaction 15h down, make 6# solution after the reaction end again;
(4) with carrying out centrifugal dehydration in the 6# solution input 10000r/min supercentrifuge, obtain the precipitation separation product;
(5) with deionized water the precipitation separation product that step (4) obtains is washed three times, make golden nanometer particle product as shown in Figure 2, nano particle average length 400nm.
Embodiment 3; Na
2SO
4The method of the synthetic tadpole shape golden nanometer particle of-SDS-PEG (mean molecule quantity 20000) soft template:
(1) polyethylene glycol, lauryl sodium sulfate, sodium sulphate and gold chloride are joined respectively in the deionized water, be heated to the 4# solution of 41-59 ℃ of 3# solution that makes its 2# solution that fully dissolves the 1# solution that obtains containing the 10mmol/L polyethylene glycol respectively, 520mmol/L lauryl sodium sulfate, 100mmol/L sodium sulphate and 240mmol/L gold chloride and be cooled to 29 ℃ stand-by;
(2) get an amount of 1-4# solution mixing and adding deionized water respectively, make 5# solution; Each component ultimate density in the 5# solution is respectively: gold chloride 0.6mmol/L, polyethylene glycol (PEG) 5mmol/L, lauryl sodium sulfate (SDS) 60mmol/L, sodium sulphate (Na
2SO
4) 4mmol/L;
(3) with 5# solution under normal pressure, after 400r/min stirs 1min, at 30 ± 1 ℃, lucifuge, ultrasonic power 120W radiation effects reaction 15h down, make 6# solution after the reaction end again;
(4) with carrying out centrifugal dehydration in the 6# solution input 6000r/min supercentrifuge, obtain the precipitation separation product;
(5) with deionized water the precipitation separation product that step (4) obtains is washed three times, make golden nanometer particle product as shown in Figure 3, nano particle average length 350nm.
Claims (3)
1. method that is equipped with tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system, it is characterized in that: utilize the soft template of the soft matter cluster of polyethylene glycol, lauryl sodium sulfate and sodium sulphate formation as the preparation golden nanometer particle, gold chloride is joined in the aqueous solution of described soft matter cluster, under the ultrasonic radiation effect by polyethylene glycol as reducing agent, gold ion is reduced into tadpole shape golden nanometer particle, and its technology is:
(1) join polyethylene glycol, lauryl sodium sulfate, sodium sulphate and gold chloride in the deionized water respectively, be heated to 41-59 ℃ it fully dissolved, obtain containing the 4# solution of the 3# solution of 2# solution, 100mmol/L sodium sulphate of 1# solution, the 520mmol/L lauryl sodium sulfate of 0.3-35mmol/L polyethylene glycol and 240mmol/L gold chloride respectively and be cooled to 25-30 ℃ stand-by;
(2) get an amount of 1-4# solution mixing and adding deionized water respectively, make 5# solution; Each component ultimate density in the 5# solution is respectively: gold chloride 0.1-1mmol/L, polyethylene glycol 0.5-20mmol/L, lauryl sodium sulfate 40-80mmol/L, sodium sulphate 0.2-10mmol/L;
(3) with 5# solution under normal pressure, after 400r/min stirs 1min, at 30 ± 1 ℃, lucifuge, ultrasonic radiation effect reaction 15-20h down, make 6# solution after the reaction end again;
(4) with carrying out centrifugal dehydration in the 6# solution input 3000-10000r/min supercentrifuge, obtain the precipitation separation product;
(5) with deionized water the precipitation separation product that step (4) obtains is washed three times, make the golden nanometer particle product.
2. according to claim 1ly a kind ofly be equipped with the method for tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system, it is characterized in that: the mean molecule quantity of described polyethylene glycol is 5990-179990.
3. according to claim 1ly a kind ofly be equipped with the method for tadpole shape golden nanometer particle with the ultrasonic promoted aqueous phase soft moulding plate legal system, it is characterized in that: the power of described ultrasonic wave radiation is 20-99W or 101-150W.
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| CN104445437A (en) * | 2014-12-08 | 2015-03-25 | 上海应用技术学院 | Preparation method of ferriferrous oxide magnetic nanoparticles |
| CN110465653A (en) * | 2019-09-19 | 2019-11-19 | 安徽工业大学 | A kind of silver wire and preparation method thereof |
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| CN102294491B (en) * | 2010-06-24 | 2013-01-16 | 安徽建筑工业学院 | Polliwog-shaped metal copper nanomaterial and preparation method thereof |
| CN105642916B (en) * | 2016-04-07 | 2017-07-14 | 江西农业大学 | A kind of method that the golden micro materials of featheriness are prepared with chemical method |
| CN111778525A (en) * | 2020-07-06 | 2020-10-16 | 江西农业大学 | Method for preparing chain-link gold nanowire by electrochemical method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104445437A (en) * | 2014-12-08 | 2015-03-25 | 上海应用技术学院 | Preparation method of ferriferrous oxide magnetic nanoparticles |
| CN104445437B (en) * | 2014-12-08 | 2016-09-14 | 上海应用技术学院 | A kind of preparation method of ferroferric oxide magnetic nano-particles |
| CN110465653A (en) * | 2019-09-19 | 2019-11-19 | 安徽工业大学 | A kind of silver wire and preparation method thereof |
| CN110465653B (en) * | 2019-09-19 | 2021-11-05 | 安徽工业大学 | Silver wire and preparation method thereof |
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