CN109530718A - A kind of preparation method of flower-shaped nanowires of gold composite nanoparticle - Google Patents

A kind of preparation method of flower-shaped nanowires of gold composite nanoparticle Download PDF

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CN109530718A
CN109530718A CN201811490724.3A CN201811490724A CN109530718A CN 109530718 A CN109530718 A CN 109530718A CN 201811490724 A CN201811490724 A CN 201811490724A CN 109530718 A CN109530718 A CN 109530718A
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gold
sio
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nanowires
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CN109530718B (en
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刘振中
徐鑫磊
应佳蕾
陈虹宇
谭文军
马春新
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Research Institute of Zhejiang University Taizhou
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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention discloses a kind of preparation methods of flower-shaped nanowires of gold composite nanoparticle, and this method is with colloidal nanoparticles Au@SiO2For template, regulate and control Jenner's line growth course by parameters such as control ligand species, reaction ratio, reaction time, to obtain a series of flower-like structure nanowires of gold composite materials with different-shape.The material structure includes Au@SiO2Core and nanowires of gold to external radiation constitute flower-like micro/nano structure.The present invention is low in cost, and experimental implementation is simple, product short preparation period, reproducible, and uniform flower-shaped nanowires of gold composite nanoparticle can be made, be a feasible technology path to prepare Jenner's nano composite material by macromolecule ligand and providing.

Description

A kind of preparation method of flower-shaped nanowires of gold composite nanoparticle
Technical field
The present invention relates to a kind of preparation methods of flower-shaped nanowires of gold composite nanoparticle, belong to nano material technology neck Domain.
Background technique
Gold nano-material has unique physical and chemical performance, in drug delivery, catalysis, modified electrode and Pharmaceutical Analysis etc. Field has potential application, the extensive concern by researcher.Studies have shown that certain characteristics of gold nano-material and its shape and Size is closely related, therefore the specific structure of effectively control gold nano-material and pattern can obtain new physical and chemical performance.
Compared with zero-dimension structural, one-dimensional nanowires of gold shows big draw ratio, few lattice defect, high surface original The advantages that subnumber.In recent years, it is developed a kind of grow using small molecule thiol ligand by active surface and prepares gold nano The method of line.Yang etc. uses amidized SiO2There is provided high curvature surface, its surface successful growth have high length-diameter ratio and Flexible radial nanowires of gold composite nanoparticle.Similarly, Liz-Marz á n etc. also uses SiO2One kind is prepared in glue Plasma metal and dielectric nanoparticle of the body particle surface radiation growth nanowires of gold length between 40-200nm.Zhang etc. It first passes through seed mediated growth method and grows nanowires of gold in Surfaces of Polystyrene Microparticles, then remove polystyrene microsphere with tetrahydrofuran The nanowires of gold vesica for forming advanced cage structure provides tip and highdensity hot spot and detects for SERS.These are radial The preparation of nano wire composite nanoparticle is all based on the synthesis of small molecule thiol ligand, but can only generally prepare with general The nanowires of gold composite construction of logical pattern.
Rarely has research to the preparation of such nanowires of gold using macromolecule ligand.Macromolecule as important one of material, Have been applied to the every field such as science and technology, life.In terms of synthetic degree of angle, if macromolecule ligand to be introduced to the conjunction of gold nanoparticle Cheng Zhong, it is possible to obtain novel functional nanocomposite.
Summary of the invention
It is compound the purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, providing a kind of novel flower-shaped nanowires of gold The preparation method of nanoparticle.
To realize that the above goal of the invention, the present invention provide a kind of preparation method of flower-shaped nanowires of gold composite nanoparticle, Include the following steps:
(1) a certain amount of aqueous solution of chloraurate is boiled, proper amount of sodium citrate aqueous solution is then added, continued heating stirring and return Stream reaction obtains nano gold spherical solution；
(2) it by above-mentioned nano gold spherical solution centrifugal concentrating, is transferred in aqueous isopropanol under stiring, sequentially adds 11- Mercaptoundecanoic acid ethanol solution, ethyl orthosilicate aqueous solution and concentrated ammonia liquor, after room temperature reaction, centrifugation obtains Au@SiO2Nanometer Particle aqueous solution；
(3) in above-mentioned Au@SiO2In nanoparticle aqueous solution, 3- aminopropyl triethoxysilane is added, after room temperature reaction, It is centrifuged and is purified with ethyl alcohol, the absorption of 3-5nm gold seeds solution room temperature is then added, finally centrifugation obtains adsorbing seed-bearing Au SiO2@seeds composite nanoparticle saves spare in ethanol；
(4) a certain amount of seed-bearing Au SiO of absorption is taken2@seeds composite nanoparticle is added and matches containing small molecule sulfydryl Body, polyvinylpyrrolidone, gold chloride and ascorbic acid growth-promoting media, after room temperature reaction, centrifuge washing obtains having flower-shaped gold The composite nanoparticle of nano wire.
Further, the diameter of gold nanosphere described in step (1) is 15-30nm.
Further, Au@SiO described in step (2)2Diameter of nano particles is 20-40nm.
Further, the time of step (3) described absorption is 2~6h.
Further, step (4) thiol ligand is 3- mercaptobenzoic acid, 4- hydroxythiophenol and 4- mercaptophenylacetic acid One of or in which two kinds of mixture, reaction time be 0~15min.
Further, the molecular weight of step (4) described polyvinyl pyrrole is 8000-60000.
Further, step (4) thiol ligand, the molar ratio of polyvinylpyrrolidone, gold chloride and ascorbic acid Example is 1:25:3:7-1:250:3:7.
Compared with prior art, the beneficial effects of the present invention are:
The present invention uses new preparation method, on the one hand does template using the colloidal nanoparticles of core-shell structure, prepares Colloid Au@SiO with core-shell structure2Nanoparticle；On the other hand, it was grown using the change of the mixed ligands such as macromolecule ligand A kind of composite nanoparticle that flower-shaped nanowires of gold size is adjusted can be obtained in journey.
The present invention is with colloidal nanoparticles Au@SiO2For template, pass through control ligand species, reaction ratio, reaction time Etc. parameters regulate and control Jenner's line growth course, to obtain a series of flower-like structure nanowires of gold composite woods with different-shape Material.The material structure includes Au@SiO2Core and nanowires of gold to external radiation constitute flower-like micro/nano structure.
The present invention is low in cost, and experimental implementation is simple, product short preparation period, reproducible, can be made uniform flower-shaped Nanowires of gold composite nanoparticle is a feasible skill to prepare Jenner's nano composite material by macromolecule ligand and providing Art route.
Reaction condition of the present invention is simple, device simple, and entire process flow is shorter, and product uniformity is good, and repeatability It is good, there is preferable potential application foreground.
Detailed description of the invention
Fig. 1 is Au@SiO prepared by case study on implementation 1 of the present invention2SEM figure.
Fig. 2 is the SEM figure of flower-shaped nanowires of gold composite nanoparticle prepared by case study on implementation 1 of the present invention.
Fig. 3 is the SEM figure of flower-shaped nanowires of gold composite nanoparticle prepared by case study on implementation 2 of the present invention.
Fig. 4 is the SEM figure of flower-shaped nanowires of gold composite nanoparticle prepared by case study on implementation 3 of the present invention.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples.
Embodiment 1
A kind of preparation method of flower-shaped nanowires of gold composite nanoparticle, comprising the following steps:
(1) by 10mg, the HAuCl of 100mL4Aqueous solution heating is boiled, and 3mL is then added, 1wt% sodium citrate is water-soluble Liquid, agitating and heating back flow reaction 30min, obtains claret solution at 600 rpm, and cooled to room temperature obtains gold nanosphere；
(2) by 3mL nano gold spherical solution in 4000g, 8min centrifugal concentrating removes supernatant and is dispersed in 500 μ L deionizations In water；It is transferred in 2.5mL aqueous isopropanol with vigorous stirring, the 11- alkyl hendecanoic acid second of 20 μ L, 2mM is then added Alcoholic solution；The ethyl orthosilicate aqueous solution of 600 μ L, 9mM is added, is eventually adding the concentrated ammonia liquor of 90 μ L, reacts at room temperature 12h.Reaction After, the Au@SiO of core-shell structure is obtained in 5200g centrifugation 9min2Nanoparticle is dispersed in 500 μ L deionized waters.From Fig. 1 can be seen that gained nano-particles size in 30nm or so, have apparent core-shell structure；
(3) in the Au@SiO of 500 μ L2In aqueous solution, the 3- aminopropyl triethoxysilane of 500 μ L, 1mM, room temperature is added React 1h；By it in 5200g, 9min centrifugation purification twice, is stored in 500 μ L ethyl alcohol；It is then added into 500 μ L gold kind Sub- solution, room temperature adsorb 2h, guarantee gold seeds at one layer of its adsorption；It is finally centrifuged 8min at 5200g and obtains Au@ SiO2@seeds is stored in spare in 1mL ethyl alcohol；
(4) the Au@SiO of 100 μ L is taken2Then the 4- mercaptophenylacetic acid containing 0.37mM, 72.5mM is added in@seeds solution Polyvinylpyrrolidone, the growth-promoting media of 1.13mM gold chloride and 2.73mM ascorbic acid react at room temperature 15min.So in 1000rpm Lower centrifugation 4min, is dispersed in water again.Figure it is seen that nanowires of gold in the flower-shaped gold nano composite nanoparticle of gained Size be about 300nm.The implementation case can be prepared using 4- mercaptophenylacetic acid mixed ligand has longer nanowires of gold multiple Close nanoparticle.
Embodiment 2
A kind of preparation method of flower-shaped nanowires of gold composite nanoparticle, comprising the following steps:
(1) by 10mg, the HAuCl of 100mL4Aqueous solution heating is boiled, and 3mL is then added, 1wt% sodium citrate is water-soluble Liquid, agitating and heating back flow reaction 30min, obtains claret solution at 600 rpm, and cooled to room temperature obtains gold nanosphere；
(2) by 3mL nano gold spherical solution in 4000g, 8min centrifugal concentrating removes supernatant and is dispersed in 500 μ L deionizations In water；It is transferred in 2.5mL aqueous isopropanol with vigorous stirring, the 11- Mercaptoundecanoic acid second of 20 μ L, 2mM is then added Alcoholic solution；600 μ L, 9mM ethyl orthosilicate aqueous solutions are added, are eventually adding 90 μ L concentrated ammonia liquors, react at room temperature 12h；Reaction terminates Afterwards, the Au@SiO of core-shell structure is obtained in 5200g centrifugation 9min2Nanoparticle is dispersed in 500 μ L deionized waters and saves；
(3) in the Au@SiO of 500 μ L2In aqueous solution, the 3- aminopropyl triethoxysilane of 500 μ L, 1mM, room temperature is added React 1h；By it in 5200g, 9min centrifugation purification twice, is stored in 500 μ L ethyl alcohol；It is then added into 500 μ L gold kind Sub- solution, room temperature adsorb 2h；It is finally centrifuged 8min at 5200g and obtains Au@SiO2@seeds is stored in spare in 1mL ethyl alcohol；
(4) the Au@SiO of 100 μ L is taken2Then the 4- hydroxythiophenol containing 0.37mM, 72.5mM is added in@seeds solution Polyvinylpyrrolidone, the growth-promoting media of 1.13mM gold chloride and 2.73mM ascorbic acid react at room temperature 15min；Nanoparticle exists It is centrifuged 4min under 1000rpm, is dispersed in water again.From figure 3, it can be seen that golden in the flower-shaped gold nano composite nanoparticle of gained The size of nano wire about 150nm.The implementation case can be prepared using 4- hydroxythiophenol mixed ligand has shorter flower-shaped gold The composite nanoparticle of nano wire.
Embodiment 3
A kind of preparation method of elctro-catalyst gold and silver plating palladium nanometer wire, comprising the following steps:
(1) by 10mg, the HAuCl of 100mL4Aqueous solution heating is boiled, and 3mL is then added, 1wt% sodium citrate is water-soluble Liquid, agitating and heating back flow reaction 30min, obtains claret solution at 600 rpm, and cooled to room temperature obtains gold nanosphere；
(2) by 9mL nano gold spherical solution in 4000g, 8min centrifugal concentrating is arrived, and is removed supernatant and is dispersed in 1.5mL again In deionized water；It is transferred in 7.5mL aqueous isopropanol with vigorous stirring, the 11- sulfydryl 11 of 60 μ L, 2mM is then added Alkanoic acid ethanol solution.600 μ L, 27mM ethyl orthosilicate aqueous solutions are then added, are eventually adding 270 μ L concentrated ammonia liquors, react at room temperature 12h.After reaction, the Au@SiO of core-shell structure is obtained in 5200g centrifugation 9min2Nanoparticle is dispersed in 1.5mL deionization In water；
(3) in the Au@SiO of 500 μ L2In aqueous solution, the 3- aminopropyl triethoxysilane of 500 μ L, 1mM, room temperature is added React 1h.By it in 5200g, 9min centrifugation purification twice, is stored in 500 μ L ethyl alcohol；It is then added into 500 μ L gold kind Sub- solution, room temperature adsorb 2h；It is finally centrifuged 8min at 5200g and obtains Au@SiO2@seeds is stored in spare in 1mL ethyl alcohol；
(4) the Au@SiO of 300 μ L is taken2Then the 4- mercaptophenylacetic acid containing 0.37mM, 72.5mM is added in@seeds solution Polyvinylpyrrolidone, the growth-promoting media of 1.13mM gold chloride and 2.73mM ascorbic acid react at room temperature 15min；Then exist It is centrifuged 4min under 1000rpm, is dispersed in water again.From fig. 4, it can be seen that golden in the flower-shaped gold nano composite nanoparticle of gained The size of nano wire about 100nm.The implementation case can be prepared multiple with shorter flower-shaped nanowires of gold by regulation seed concentration Close nanoparticle.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.

Claims (7)

1. the preparation method of flower-shaped nanowires of gold composite nanoparticle, which comprises the steps of:
(1) a certain amount of aqueous solution of chloraurate is boiled, proper amount of sodium citrate aqueous solution is then added, it is anti-to continue heating stirring reflux It should obtain nano gold spherical solution；
(2) it by above-mentioned nano gold spherical solution centrifugal concentrating, is transferred in aqueous isopropanol under stiring, sequentially adds 11- sulfydryl Hendecanoic acid ethanol solution, ethyl orthosilicate aqueous solution and concentrated ammonia liquor, after room temperature reaction, centrifugation obtains Au@SiO2Nanoparticle Aqueous solution；
(3) in above-mentioned Au@SiO2In nanoparticle aqueous solution, 3- aminopropyl triethoxysilane is added, after room temperature reaction, uses second Alcohol centrifugation purification, is then added the absorption of 3-5nm gold seeds solution room temperature, finally centrifugation obtains adsorbing seed-bearing Au SiO2@ Seeds composite nanoparticle saves spare in ethanol；
(4) a certain amount of seed-bearing Au SiO of absorption is taken2@seeds composite nanoparticle is added containing small molecule thiol ligand, gathers The growth-promoting media of vinylpyrrolidone, gold chloride and ascorbic acid, after room temperature reaction, centrifuge washing obtains having flower-shaped nanowires of gold Composite nanoparticle.
2. the method according to claim 1, wherein the diameter of gold nanosphere described in step (1) is 15- 30nm。
3. the method according to claim 1, wherein Au@SiO described in step (2)2Diameter of nano particles is 20- 40nm。
4. the method according to claim 1, wherein the time of step (3) described absorption is 2~6h.
5. the method according to claim 1, wherein step (4) thiol ligand is 3- mercaptobenzoic acid, 4- One of hydroxythiophenol and 4- mercaptophenylacetic acid or in which two kinds of mixture, reaction time are 0~15min.
6. the method according to claim 1, wherein the molecular weight of step (4) described polyvinylpyrrolidone is 8000-60000。
7. the method according to claim 1, wherein step (4) thiol ligand, polyvinylpyrrolidone, The molar ratio of gold chloride and ascorbic acid is 1:25:3:7-1:250:3:7.
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Cited By (5)

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CN110227815A (en) * 2019-06-11 2019-09-13 东南大学 A kind of preparation method of water dispersible nanowires of gold
CN110711610A (en) * 2019-10-17 2020-01-21 桂林理工大学 Preparation method of super-hydrophobic/super-hydrophilic mixed pattern microarray dendritic gold chip
CN112501651A (en) * 2020-12-03 2021-03-16 南京工业大学 Substrate-based gold nanowire and preparation method and application thereof
CN112705724A (en) * 2020-12-07 2021-04-27 南京工业大学 Adjustable gold nanostructure and preparation method and application thereof
CN115921886A (en) * 2023-01-17 2023-04-07 西安交通大学 Preparation method of asymmetric branch nano structure

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110227815A (en) * 2019-06-11 2019-09-13 东南大学 A kind of preparation method of water dispersible nanowires of gold
CN110711610A (en) * 2019-10-17 2020-01-21 桂林理工大学 Preparation method of super-hydrophobic/super-hydrophilic mixed pattern microarray dendritic gold chip
CN110711610B (en) * 2019-10-17 2021-10-29 桂林理工大学 Preparation method of super-hydrophobic/super-hydrophilic mixed pattern microarray dendritic gold chip
CN112501651A (en) * 2020-12-03 2021-03-16 南京工业大学 Substrate-based gold nanowire and preparation method and application thereof
CN112501651B (en) * 2020-12-03 2022-07-29 南京工业大学 Substrate-based gold nanowire and preparation method and application thereof
CN112705724A (en) * 2020-12-07 2021-04-27 南京工业大学 Adjustable gold nanostructure and preparation method and application thereof
CN115921886A (en) * 2023-01-17 2023-04-07 西安交通大学 Preparation method of asymmetric branch nano structure

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