CN108941612A - A kind of preparation method for the small particle gold nanoparticle that size is controllable - Google Patents
A kind of preparation method for the small particle gold nanoparticle that size is controllable Download PDFInfo
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- CN108941612A CN108941612A CN201811128936.7A CN201811128936A CN108941612A CN 108941612 A CN108941612 A CN 108941612A CN 201811128936 A CN201811128936 A CN 201811128936A CN 108941612 A CN108941612 A CN 108941612A
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- gold nanoparticle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
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- 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
Abstract
The present invention relates to a kind of preparation methods of small particle gold nanoparticle that size is controllable.Pass through aqueous phase oxidation reduction method; using sodium borohydride as reducing agent; polyvinylpyrrolidone (PVP) is used as protective agent; gold chloride is reduced to gold nanoparticle under conditions of ice bath; carrying out characterization to it by transmission electron microscope (TEM) can observe its partial size less than 10nm, and the preparation-obtained small particle gold nanoparticle of the present invention can be used for blocking mesoporous material duct, label detection and catalytic field.
Description
Technical field
The invention belongs to gold nanoparticle and its preparation field, in particular to a kind of small particle Jenner's grain of rice that size is controllable
The preparation method of son.
Background technique
Nanogold particle refers to gold particle of the size within the scope of 1~100nm.The hydrosol being generally dispersed in water,
Therefore also known as colloidal gold.Gold nanoparticle has many advantages, such as high electron density, dielectric property, catalysis and good biocompatibility.
As the nano gold mark technology of one of modern four big labelling techniques, by its high electron density and to the strong absorption of protein
Ability, can be used for qualitative or sxemiquantitative tachysynthesis detection and with glucose coccus A albumen, immunoglobulin, toxin, sugar
The Non-covalent bindings such as albumen, enzyme, antibiotic, hormone, bovine serum albumin, the advantages of showing simple, quick, high sensitivity,
Residue of veterinary drug, zoonosis, pesticide residue, pathogenic microorganisms and mycotoxin detection in play and its important work
With.Gold nanoparticle also has good catalytic capability, such as carbon monoxide oxidation, catalysis epoxidation of propylene, acetylene hydrogen chlorine
Change etc., it is generally recognized that when gold particle is in very little, shows quantum effect, with the reduction of its partial size, catalytic activity is in
Exponential growth, therefore gold catalysis has become current catalyticing research field research direction of greatest concern.In biosensor
Aspect, nanogold may be designed as immunosensor, be to lead to electrochemistry in conjunction with antibody specificity using organism endoantigen
Variation designs.Since nanogold has the extremely strong bio-sensing taken electronic capability by force, can greatly improve as measurement blood glucose
The activity of device glucose oxidase film, gold particle is smaller, and activity is bigger.The gold nanoparticle of small particle is in mesoporous material as load
Porter is alternatively arranged as in the biosensor of body to play the role of opening and block duct.The synthetic method master of gold nanoparticle
It is divided into physical method and two kinds of chemical method, physical method mainly includes vacuum deposition method and laser ablation etc., and chemical method is main
Including aqueous phase oxidation reduction method, crystal seed method, micro emulsion method and template etc..Wherein aqueous phase oxidation reduction method because preparation step it is relatively simple
It is single, to the of less demanding of equipment, it is at low cost and be widely used.It can be prepared using the aqueous solution of reduction of sodium citrate gold chloride
Particle diameter distribution is relatively narrow out, and the gold nano grain that shape is single.However the gold nanometer particle grain size of this method preparation it is much in
16nm, and it is then higher and complicated for operation to equipment dependence in the method for 8nm or less gold nanoparticle in relation to preparing partial size.
Summary of the invention
(1) technical problems to be solved
The preparation method of the object of the present invention is to provide a kind of small particle gold nanoparticle with quantum effect.In experiment
Gold nanoparticle is prepared by the way that sodium borohydride and polyvinylpyrrolidone are added into chlorauric acid solution.Gold nano of the invention
Particle has high electron density, catalytic and quantum effect, good monodispersity, and preparation method is simple.
(2) technical solution
The purpose of the present invention is implemented with the following technical solutions: in aqueous solution by gold chloride dispersion, polyethylene pyrrole is added
Pyrrolidone stirs under ice bath, and sodium borohydride solution is then added, and shading reaction obtains the gold nanoparticle of small particle after centrifugation.
The method is simple and easily operated.Prepared gold nanometer particle grain size is 2~10nm.
(3) specific reaction process
A kind of controllable small particle gold nanoparticle of size provided by the invention, particle size range are 2~10nm, form list
One, epigranular.
The preparation method of the controllable small particle gold nanoparticle of size of the present invention, the specific steps are as follows:
Under condition of ice bath, the gold chloride that mass fraction is 1% is added in 25ml secondary water, the poly- second being then added
Alkene pyrrolidone (PVP), stirs evenly.Then aqueous solution of the 5ml containing sodium borohydride is added, solution becomes sepia from colourless,
Revolving speed is adjusted, continues stirring 3~6 hours, 12~48h of standing, solution in 4 DEG C of refrigerators is put into after the reaction was completed and gradually becomes pink
Color, then solution is taken out into centrifugation and obtains the gold nanoparticle of small particle.
The solvent is water.
The protective agent is polyvinylpyrrolidone.
The reducing agent is sodium borohydride.
Polyvinylpyrrolidone is 1: 1~1: 2 with the mass ratio of gold chloride.
The molar ratio of sodium borohydride and gold chloride is 3.25: 1~1: 1.
The pH of reaction system is 3~6, and mixing speed is 240~600r/min, and reaction temperature is 5~15 DEG C.
Detailed description of the invention
Fig. 1 is that the TEM of the resulting small particle gold nanoparticle of the embodiment of the present invention 1 schemes；Fig. 2 obtains small for embodiment 1
The ultraviolet-visible absorption spectroscopy of partial size gold nanoparticle；Fig. 3 is the particle diameter distribution for the small particle gold nanoparticle that embodiment 1 obtains
Figure；Fig. 4 is the TEM figure for the small particle gold nanoparticle that embodiment 2 obtains；Fig. 5 is small particle Jenner's grain of rice that embodiment 3 obtains
The TEM figure of son；Fig. 6 is the TEM figure for the small particle gold nanoparticle that embodiment 4 obtains.
Specific embodiment
The following is specific embodiments of the present invention, and the embodiment described is rather than to limit this hair for describing the present invention
It is bright.
Embodiment 1
Under condition of ice bath, the gold chloride that 0.4ml mass fraction is 1% is added in 25ml secondary water, is then added
The polyvinylpyrrolidone (PVP) of 2.0mg, stirs evenly.Then the aqueous solution of 5ml sodium borohydride containing 1mg is added, solution is by nothing
Discoloration is sepia, and adjustment revolving speed to 480rpm continues stirring 6 hours, is put into 4 DEG C of refrigerators after the reaction was completed and stands 12h, molten
Liquid gradually becomes pink, then solution is taken out centrifugation and obtains the gold nanoparticle of small particle.
Embodiment 2
Under condition of ice bath, the gold chloride that 0.4ml mass fraction is 1% is added in 25ml secondary water, is then added
The polyvinylpyrrolidone (PVP) of 3.0mg, stirs evenly.Then be added 5ml sodium borohydride containing 0.8mg aqueous solution, solution by
Colourless to become sepia, adjustment revolving speed to 480rpm continues stirring 6 hours, is put into 4 DEG C of refrigerators after the reaction was completed and stands 12h,
Solution gradually becomes pink, then solution is taken out centrifugation and obtains the gold nanoparticle of small particle.
Embodiment 3
Under condition of ice bath, the gold chloride that 0.4ml mass fraction is 1% is added in 25ml secondary water, is then added
The polyvinylpyrrolidone (PVP) of 2.0mg, stirs evenly.Then be added 5ml sodium borohydride containing 0.8mg aqueous solution, solution by
Colourless to become sepia, adjustment revolving speed to 480rpm continues stirring 6 hours, is put into 4 DEG C of refrigerators after the reaction was completed and stands 12h,
Solution gradually becomes pink, then solution is taken out centrifugation and obtains the gold nanoparticle of small particle.
Embodiment 4
Under condition of ice bath, the gold chloride that 0.4ml mass fraction is 1% is added in 25ml secondary water, is then added
The polyvinylpyrrolidone (PVP) of 2.0mg, stirs evenly.Then be added 5ml sodium borohydride containing 1.0mg aqueous solution, solution by
Colourless to become sepia, adjustment revolving speed to 120rpm continues stirring 6 hours, is put into 4 DEG C of refrigerators after the reaction was completed and stands 12h,
Solution gradually becomes pink, then solution is taken out centrifugation and obtains the gold nanoparticle of small particle.
Claims (6)
1. a kind of preparation method for the small particle gold nanoparticle that size is controllable, it is characterised in that method includes the following steps:
Under the conditions of certain temperature, protective agent is added in the aqueous solution containing gold chloride, 3~5min is quickly stirred, is then added
Mixed liquor is moved to 12~48h of standing in 4 DEG C of refrigerators, then mixed liquor is taken out by reducing agent, shading and after continuing 3~6h of stirring
Particle size range can be obtained after centrifugation in 2~10nm, and form is uniform, the gold nanoparticle of dispersion.
2. a kind of preparation method of the controllable small particle gold nanoparticle of size according to claim 1, it is characterised in that
The reducing agent is sodium borohydride, and the molar ratio with gold chloride is 3.25: 1~1: 1.
3. a kind of preparation method of the controllable small particle gold nanoparticle of size according to claim 1, it is characterised in that
The protective agent is polyvinylpyrrolidone (PVP), and the mass ratio with gold chloride is 1: 1~1: 2.
4. a kind of preparation method of the controllable small particle gold nanoparticle of size according to claim 1, it is characterised in that
The reaction condition is ice-water bath.
5. a kind of preparation method of the controllable small particle gold nanoparticle of size according to claim 1, it is characterised in that
The system pH is 3~6.
6. a kind of preparation method of the controllable small particle gold nanoparticle of size according to claim 1, it is characterised in that
Churned mechanically rate is 240~600r/min when the described reaction.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115592124A (en) * | 2022-09-14 | 2023-01-13 | 苏州大学（Cn） | Nano colloidal gold and preparation method thereof |
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Application publication date: 20181207 |