CN103406546B - The method of the flower-shaped golden nanometer particle of a kind of controlled synthesis - Google Patents
The method of the flower-shaped golden nanometer particle of a kind of controlled synthesis Download PDFInfo
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- CN103406546B CN103406546B CN201310321978.3A CN201310321978A CN103406546B CN 103406546 B CN103406546 B CN 103406546B CN 201310321978 A CN201310321978 A CN 201310321978A CN 103406546 B CN103406546 B CN 103406546B
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Abstract
Prepare a method for flower-shaped golden nanometer particle, the method adopts color of spherical gold seed solution and gold chloride and reducing agent and has the protective agent of the Surface Modification Effect as reaction reagent.At 20 DEG C ~ 40 DEG C, the color of spherical gold seed solution getting 1ml ~ 10ml joins in 10ml ~ 30ml deionized water, rapid stirring; Add a certain amount of chlorauric acid solution, then add reductant solution; Stop after Keep agitation a period of time stirring, obtain aurosol solution; Protective agent solution is added in aurosol solution; Operate this process and once or continuously repeat this process 2 ~ 4 times, and in repeatedly repetitive process, each seed solution is the aurosol solution that its back obtains, and finally obtains flower-shaped golden nanometer particle.Compared to prior art, the present invention utilizes reduction reaction reduction gold chloride to prepare flower-shaped golden nanometer particle, does not need by special installation, also without the need to hot environment, simple to operate.
Description
Technical field
The present invention relates generally to the method for the flower-shaped golden nanometer particle of a kind of controlled synthesis, belongs to technical field of nanometer material preparation.
Background technology
Golden nanometer particle is due to the optical, electrical of its uniqueness and catalytic performance compared with body phase gold copper-base alloy, in field extensive application such as sensing and analysis detections.Because its performance is comparatively large by the impact of the shape and size of nano particle, scientific research personnel is devoted to the preparation studying the controlled golden nanometer particle of shape and size always.
Wherein, the preparation of flower-shaped golden nanometer particle is particularly noticeable, special electromagnetic field-effect in the surface coarse due to flower-shaped golden nanometer particle and branch, make it in SERS, biomedicine, the field such as environmental analysis and catalysis has using value widely.Due to the optical, electrical and magnetic effect that these are special, the controlled synthesis how realizing flower-shaped golden nanometer particle is the focus of research now.
In prior art, the preparation method of flower-shaped golden nanometer particle is divided into Physical and chemical method, wherein Physical mainly comprises vacuum vapour deposition, electrical dispersion and soft landing method etc., and chemical method is primarily of oxidation-reduction method, electrochemical process, photochemical method, microwave method and sol method etc.Dong group and the Wang group flower-shaped golden nanometer particle that utilized electrochemical process to synthesize respectively; Xie etc. are with the ammonium formate reducing agent flower-shaped golden nanometer particle that utilized hydro-thermal method to prepare under the condition of polyvinylpyrrolidone for dressing agent; Ren etc. utilize polyvinylpyrrolidone and lauryl sodium sulfate reaction to form template, have synthesized flower-shaped golden nanometer particle; Jia etc. are the flower-shaped golden nanometer particle of Template preparation with tree-like polyamine surfactant C18N3; The method that the electricity consumption depositions such as KimJH are formed sediment and photoetching combines has prepared flower-shaped golden nanometer particle.Although there has been the method for the flower-shaped golden nanometer particle of above preparation, but, because these methods existing are in the course of reaction of the flower-shaped golden nanometer particle of preparation, generally need to add coating material or template makes preparation process and complicated condition, or need under the high temperature conditions, or need by special installation.
Summary of the invention
In order to overcome above-mentioned prior art shortcoming, the object of the present invention is to provide a kind of preparation method simple and the method for the flower-shaped golden nanometer particle of the preparation of controllable precise.
A kind of method preparing flower-shaped golden nanometer particle, the method comprises color of spherical gold seed solution and chlorauric acid solution and has the reductant solution of reproducibility and have the protective agent solution of nanoparticle surface modified effect, at 20 DEG C ~ 40 DEG C, the color of spherical gold seed solution getting 1ml ~ 10ml joins in 10ml ~ 30ml deionized water, rapid stirring; Add a certain amount of chlorauric acid solution, then add reductant solution; Stop after Keep agitation a period of time stirring, obtain aurosol solution; Protective agent solution is added in aurosol solution; Operate this process and once or continuously repeat this process repeatedly, and in repeatedly repetitive process, the seed solution at every turn added is the aurosol solution that its back obtains.
Described color of spherical gold seed sizes is 5nm-30nm.
The described reductant solution with reproducibility is ascorbic acid solution, sodium hydroxide solution or sodium borohydride solution.
The described protective agent solution with nanoparticle surface modified effect is the reagent that natrium citricum or polydiene diemethylamine have electrostatic stabilization effect.
Described rapid stirring rotating speed is 3000r/min ~ 6000r/min.
Described chlorauric acid solution and the mol ratio of reducing agent are 1: 1 ~ 1: 100.
The described Keep agitation time is 10min ~ 40min.
Described crystal seed and protectant mol ratio are 1: 1 ~ 1: 100.
The described number of times repeatedly repeating this process is 2 ~ 4 times.
Compared to prior art; the present invention at a lower temperature; take gold chloride as the predecessor of gold, with ascorbic acid, NaOH or sodium borohydride are reducing agent; with natrium citricum or polydiene diemethylamine for protective agent; prepare flower-shaped golden nanometer particle with reducing agent reduction gold chloride, do not need by special installation, also without the need to hot environment; protective agent is beneficial to the pattern accurately controlling the golden nanometer particle that each step generates, simple to operate.
Accompanying drawing explanation
Fig. 1 is color of spherical gold ESEM (SEM) photo prepared by the embodiment of the present invention, and scale is 200nm;
Fig. 2 is color of spherical gold SEM photo prepared by the embodiment of the present invention, and scale is 200nm;
Fig. 3 is flower-shaped golden nanometer particle SEM photo prepared by the embodiment of the present invention, and scale is 200nm;
Fig. 4 is flower-shaped golden nanometer particle SEM photo prepared by the embodiment of the present invention, and scale is 200nm;
Fig. 5 is flower-shaped golden nanometer particle SEM photo prepared by the embodiment of the present invention, and scale is 200nm;
Detailed description of the invention
The preparation method of the flower-shaped golden nanometer particle of the invention process is described in detail below in conjunction with accompanying drawing:
The preparation of spherical Au crystal seed
By the color of spherical gold of citrate reduction legal system for 20nm.Specific practice is the HAuCl of 50ml
4solution (0.24mM) was heated to boiling maintenance after 15 minutes, then added 1ml natrium citricum (1%) fast, and keep boiling 20min, solution becomes claret.Finally make solution under agitation cool to room temperature, be gained color of spherical gold seed A
0.
Embodiment 1
The preparation of Jenner's popped rice
Step (1)
The crystal seed A of 10ml with vigorous stirring
0join in the deionized water of 25ml; Then, the ascorbic acid (1M) of 0.5ml is added; Then the HAuCl of 0.5ml is added fast
4solution (24mM); Keep rotating speed 5000r/min to stir 30min, add the sodium citrate solution (1%) of 0.25ml, stop stirring; Obtain mixture A.Get this mixture centrifugation to be scattered in deionized water again, be illustrated in figure 1 the stereoscan photograph of the product that the present embodiment step (1) obtains, the golden nanometer particle pattern that as shown in Figure 1 prepared by the present embodiment step (1) is spherical.
Step (2)
The A of 9ml joins in the deionized water of 25ml with vigorous stirring; Then, the ascorbic acid (1M) of 0.5ml is added; Then the HAuCl of 0.5ml is added fast
4solution (24mM); Keep rotating speed 5000r/min to stir 30min, add the sodium citrate solution (1%) of 0.25ml, stop stirring; Obtain mixture B.Get this mixture centrifugation to be scattered in deionized water again, be illustrated in figure 2 the stereoscan photograph of the product that the present embodiment step (2) obtains, the golden nanometer particle pattern that as shown in Figure 2 prepared by the present embodiment step (2) is spherical.
Step (3)
The B of 8ml joins in the deionized water of 25ml with vigorous stirring; Then, the ascorbic acid (1M) of 0.5ml is added; Then the HAuCl of 0.5ml is added fast
4solution (24mM); Keep rotating speed 5000r/min to stir 30min, add the sodium citrate solution (1%) of 0.25ml, stop stirring; Obtain mixture C.Get this mixture centrifugation to be scattered in deionized water again, be illustrated in figure 3 the stereoscan photograph of the product that the present embodiment step (3) obtains, the golden nanometer particle pattern that as shown in Figure 3 prepared by the present embodiment step (3) is flower-shaped.
Step (4)
The C of 7ml joins in the deionized water of 25ml with vigorous stirring; Then, the ascorbic acid (1M) of 0.5ml is added; Then the HAuCl of 0.5ml is added fast
4solution (24mM); Keep rotating speed 5000r/min to stir 30min, add the sodium citrate solution (1%) of 0.25ml, stop stirring; Obtain mixture D.Get this mixture centrifugation to be scattered in deionized water again, be illustrated in figure 4 the stereoscan photograph of the product that the present embodiment step (4) obtains, the golden nanometer particle pattern that as shown in Figure 4 prepared by the present embodiment step (4) is flower-shaped.
Embodiment 2
The preparation of Jenner's popped rice
The crystal seed A of 3ml with vigorous stirring
0join in the deionized water of 25ml; Then, the NaOH (1M) of 0.3ml is added; Then the HAuCl of 0.5ml is added fast
4solution (24mM); Keep rotating speed 5500r/min to stir 25min, add the sodium citrate solution (1%) of 0.25ml, stop stirring; Obtain mixture.Get this mixture centrifugation to be scattered in deionized water again, be illustrated in figure 5 the stereoscan photograph of the product that the present embodiment obtains, the golden nanometer particle pattern that as shown in Figure 5 prepared by the present embodiment is flower-shaped.
Claims (5)
1. prepare the method for flower-shaped golden nanometer particle for one kind, the method comprises color of spherical gold seed solution and chlorauric acid solution and has the reductant solution of reproducibility and have the protective agent solution of nanoparticle surface modified effect, at 20 DEG C ~ 40 DEG C, the color of spherical gold seed solution getting 1ml ~ 10ml joins in 10ml ~ 30ml deionized water, rapid stirring; Add a certain amount of chlorauric acid solution, then add reductant solution; Stop after Keep agitation a period of time stirring, obtain aurosol solution; Protective agent solution is added in aurosol solution; Operate this process and once or continuously repeat this process repeatedly, and in repeatedly repetitive process, the seed solution at every turn added is the aurosol solution that its back obtains;
The described reductant solution with reproducibility is ascorbic acid solution, sodium hydroxide solution or sodium borohydride solution; The described protective agent solution with nanoparticle surface modified effect is natrium citricum or polydiene diemethylamine;
Described chlorauric acid solution and the mol ratio of reducing agent are 1: 1 ~ 1: 100, and described color of spherical gold seed and protectant mol ratio are 1: 1 ~ 1: 100.
2. a kind of method preparing flower-shaped golden nanometer particle according to claim 1, is characterized in that: described color of spherical gold seed sizes is 5nm-30nm.
3. a kind of method preparing flower-shaped golden nanometer particle according to claim 1, is characterized in that: described rapid stirring rotating speed is 3000r/min ~ 6000r/min.
4. a kind of method preparing flower-shaped golden nanometer particle according to claim 1, is characterized in that: the described Keep agitation time is 10min ~ 40min.
5. a kind of method preparing flower-shaped golden nanometer particle according to claim 1, is characterized in that: the described number of times repeatedly repeating this process is 2 ~ 4 times.
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| CN103934467B (en) * | 2014-04-02 | 2016-08-17 | 南京邮电大学 | One has flower-shaped gold nano grain of silk ball and preparation method thereof |
| CN104308175B (en) * | 2014-09-30 | 2017-04-05 | 国家纳米科学中心 | A kind of spherical gold grain and its step by step fast synthesis method |
| CN104690288B (en) * | 2014-11-27 | 2017-03-22 | 南京邮电大学 | Preparation method of flower-like gold nanoparticles and application of flower-like gold nanoparticles serving as SERS (surface enhanced Raman scattering) enhanced substrates |
| CN104722773B (en) * | 2015-02-12 | 2016-08-17 | 苏州大学 | The preparation method stinging shape golden nanometer particle and the thorn shape golden nanometer particle prepared by the method |
| CN105158456B (en) * | 2015-09-01 | 2017-03-15 | 江南大学 | A kind of Jenner's popped rice immunological probe, its preparation method and application |
| CN105537583A (en) * | 2015-12-22 | 2016-05-04 | 哈尔滨工业大学 | Core-shell Au@TiO2 nano-particles and preparation method thereof |
| CN106001606A (en) * | 2016-06-30 | 2016-10-12 | 天津大学 | Preparing method capable of adjusting particle size of gold nanoparticles based on sodium citrate reduction method |
| CN108671915B (en) * | 2018-05-21 | 2021-08-03 | 浙江理工大学 | Micro-nano Au flower and preparation method thereof |
| CN108645840B (en) * | 2018-07-20 | 2021-02-26 | 江苏大学 | Surface-enhanced Raman pesticide detection method based on gold-magnetic nano sandwich type |
| CN111842928B (en) * | 2020-07-28 | 2022-09-13 | 南京医科大学第二附属医院 | Preparation method of raspberry-shaped gold nanoparticles |
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