CN108372314A - A kind of preparation method of the hollow gold-silver alloy nanoparticles of high SERS activity - Google Patents
A kind of preparation method of the hollow gold-silver alloy nanoparticles of high SERS activity Download PDFInfo
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- CN108372314A CN108372314A CN201810268295.9A CN201810268295A CN108372314A CN 108372314 A CN108372314 A CN 108372314A CN 201810268295 A CN201810268295 A CN 201810268295A CN 108372314 A CN108372314 A CN 108372314A
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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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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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
- B82Y35/00—Methods or apparatus for measurement or analysis of nanostructures
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a kind of preparation methods of the hollow gold-silver alloy nanoparticles of high SERS activity, and it is template to prepare silver nanocubes by polyol process first, then using deionized water as solvent, PVP is stabilizer, and ascorbic acid is reducing agent.React with the electric current displacement between chlorauric acid solution by silver-colored simple substance and ascorbic acid reduction deposits the double action of silver ion and gold chloride and obtained that outer wall is complete, the cubic type gold-silver alloy nanoparticles of boring；The preparation processes of the hollow gold-silver alloy nanoparticles is simple, conveniently, process control；Electrum characteristic makes the nano-particle stability high, can resist Strong oxdiative reagent（Such as H2O2）Etching, application range is more extensive；Cube structure with sharp angle and rib makes the nano-particle with high SERS activity, and detection sensitivity is high, can carry out Raman detection to micro harmful food additives, therefore have a good application prospect.
Description
Technical field
The invention belongs to technical field of food safety detection, and in particular to a kind of hollow electrum nanometer of high SERS activity
The preparation method of particle.
Background technology
Silver nano material has unique optical property, electrical properties, catalytic property and excellent sensing capability and life
Analyte detection ability, therefore the silver nano material of various patterns receives extensive research.Compared to spherical shape, grain of rice type, rodlike, band
The Nano silver grain of the patterns such as shape, threadiness, cubic type is of greatest concern.Silver nanocubes corner angle are sharp, pattern is uniform, can be with
As highly sensitive local plasmon sensing and surface enhanced Raman substrate.But Ag simple substance is unstable, is easy by H2O2、O2, halogen
Oxidizing element etc. is silver ion, causes crystal structure to destroy, especially the etching to silver nanocubes sharp corners, greatly
Its SERS activity is reduced greatly.And the silver ion toxic side effect that Ag simple substance is generated by oxidation more limits it and is led in biology
The application in domain.
It is well known that Au nanocrystals have excellent chemical stability and good biocompatibility and nontoxic secondary work
With being had a wide range of applications in biological field.It is found that after silver and gold form electrum, the stability of silver element greatly increases
By force, the galactic pole difficulty in electrum is aoxidized.Therefore the SERS substrates of high stability can be obtained by preparing electrum structure, be opened up
The SERS application ranges of wide silver nano material.As SERS substrates, the sharp corners of nanoparticle surface are to generate strong electromagnetic to increase
Strong site enhances the active site of Raman signal.It is template using silver nanocubes, can obtains retaining its cube
Structure is the hollow gold-silver alloy nanoparticles of the sharp corners with strong electromagnetic enhancing, which has high stable simultaneously
Property and high SERS activity, field of food detection have important application.
Invention content
It is an object of the invention to overcome disadvantage existing in the prior art, a kind of simple for process, reproducible, grain is proposed
The preparation method for the hollow gold-silver alloy nanoparticles of high SERS activity that sub- size is controllable, stability is high.
In order to solve the above technical problems, the technical scheme is that：A kind of hollow electrum nanometer of high SERS activity
The preparation method of particle, it is characterised in that the specific steps are：
Step 1：Silver nanocubes are prepared using polyol process, is dispersed in water and is made into mass concentration as 7.4 g/L
Dispersion liquid；
Step 2：10~100 uL of silver nanocubes dispersion liquid and stabilizer PVP and the reducing agent for measuring step 1 preparation are anti-
Magnetic agitation is uniformly mixed bad hematic acid at room temperature；
Step 3：After step 2 acquired solution continuing magnetic force is stirred evenly, aqueous solution of chloraurate is slowly added dropwise into it, obtains
The length of side is the hollow cube type gold-silver alloy nanoparticles colloidal sol of 45~80nm；
Step 4：It is obtained after the gold-silver alloy nanoparticles colloidal sol that step 3 obtains is washed repeatedly repeatedly with second alcohol and water hollow
Gold-silver alloy nanoparticles, and be dispersed in water and preserve.
The molecular weight of stabilizer PVP is one kind in 15000,30000,55000 in the step 2.
The volume of stabilizer PVP is 1~20 mL, a concentration of 0.05~1 × 10 in the step 2-2Mol/ L, reduction
The volume of agent ascorbic acid is 0.1~5 mL, a concentration of 0.01~1 mol/ L.
The volume of aqueous solution of chloraurate is 0.5~10 mL, a concentration of 0.1~2 mmol/ L in the step 3.
The rate of addition of aqueous solution of chloraurate is 0.01~0.2 mL/min in the step 3.
The hollow gold-silver alloy nanoparticles that the step 4 obtains can operate with micro harmful addition in detection food
Agent.
The step of step 1 prepares silver nanocubes be：By 12mL without water glycol（EG）Three mouthfuls of round bottoms are added to burn
In bottle, 50 min are heated under the conditions of oil bath at 160 DEG C, a concentration of 3 mmol/ of 140 uL are then rapidly added into flask
The Na of L2S ethylene glycol solutions are continuously added to the PVP second that a concentration of 180 mmol/ L molecular weight of 3 mL is 40000 after 2min
The AgNO of glycol solution and a concentration of 265 mmol/ L of 1mL3Ethylene glycol solution, whole process all carry out under magnetic stirring,
The degree carried out with ultraviolet-visible absorption spectroscopy monitoring reaction, when even a feature ultraviolet absorption peak appears in 350 nm and 435nm
When neighbouring, flask is taken out and immerses ice-water bath to terminate reaction, is then centrifuged for the silver nanoparticle cube that particle separation diameter is about 43 nm
Body.
Hollow gold-silver alloy nanoparticles made from this method have the characteristics that：（1）Structure-controllable, uniform particle sizes；（2）
Boring structure reduces the dosage of metallic element, reduces material cost；（3）Chemical stability is high, and it is severe to can be used for condition
The monitoring system at quarter；（4）With sharp rib and angle, SRES activity is high, when p-aminophenyl thiophenol（4-ABT）A concentration of 10- 11It when mol/ L, remains to detect its characteristic peak, the detection sensitivity to additive melamine in food is 10-8mol/ L；
（5）It is versatile as SERS substrates, it can be used for detecting multiple analytes matter.
The present invention has been obtained by the reaction hollow gold and silver by the electric current displacement between aqueous solution of chloraurate and silver nanocubes and has closed
Gold nanoparticle has slowed down the speed of electrostatic displacement reaction so that the gold ion of addition and quiet in reaction by the way of titration
The silver ion of electricity displacement is reduced simultaneously deposits to template surface, forms uniformly, the wall in no cavity, simultaneously because the hollow knot
The outer wall of structure is electrum ingredient, so having high SERS effects, is used for the detection of micro poisonous substance.The present invention reaction condition
Mildly, easy to operate, equipment requirement is low and reaction efficiency is high, therefore have a good application prospect.
Description of the drawings
Fig. 1 is the ultraviolet-visible absorption spectroscopy figure that embodiment 1 prepares sample 1；
Fig. 2 is the ultraviolet-visible absorption spectroscopy figure that embodiment 2 prepares sample 2；
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure that embodiment 3 prepares sample 3；
Fig. 4 is the transmission electron microscope photo that embodiment 1 prepares sample 1；
Fig. 5 is the transmission electron microscope photo that embodiment 2 prepares sample 2；
Fig. 6 is the transmission electron microscope photo that embodiment 2 prepares sample 3；
Fig. 7 is the distribution diagram of element that embodiment 1 prepares sample 1；
Fig. 8 is the Raman spectrogram that embodiment 1 prepares that sample 1 detects p-aminophenyl thiophenol.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to a kind of tool of the preparation method of the hollow gold-silver alloy nanoparticles of high SERS activity proposed according to the present invention
Body embodiment, method, step, feature and its effect, detailed description are as follows：
Implementation column 1：
Step 1：The preparation of silver nanocubes：By 12m L without water glycol（EG）It is added in three neck round bottom flask, at 160 DEG C
50 min are heated under the conditions of lower oil bath, the Na of a concentration of 3mmol/ L of 140 uL is then rapidly added into flask2S second two
Alcoholic solution is continuously added to a concentration of 180 mmol/ L PVP of 3 mL after 2min（Molecular weight is 40000）Ethylene glycol solution and
The AgNO of a concentration of 265mmol/ L of 1mL3Ethylene glycol solution, whole process all carry out under magnetic stirring.It is inhaled with UV, visible light
Receiving the degree that spectrum monitoring reaction carries out will burn when two feature ultraviolet absorption peaks appear near 350 nm and 435 nm
Bottle, which takes out, immerses ice-water bath to terminate reaction, is then centrifuged for the silver nanocubes that particle separation diameter is about 43 nm, repeatedly with acetone
After washing repeatedly, it is 7.4 g/L to be dispersed in water and be made into mass concentration；
Step 2：The preparation of hollow gold-silver alloy nanoparticles：At room temperature, by 20 μ L silver nanocubes made from step 1
50 mL reagent bottles are added in the PVP aqueous solutions that aqueous solution and a concentration of 0.1mmol/L molecular weight of 5 mL are 30000, and magnetic agitation is equal
After even, the aqueous ascorbic acid of a concentration of 0.1mol/L of 0.5 mL is added, 1 mL concentration then is slowly added dropwise using syringe pump
For the aqueous solution of chloraurate of 1mmol/L, rate of addition is 0.05 mL/min, obtains the cubic type electrum of boring
Nanoparticle sol, its side length is 50 nm, then wash hollow gold-silver alloy nanoparticles repeatedly with second alcohol and water repeatedly
Afterwards, it is dispersed in water preservation.
Implementation column 2：
At room temperature, the 40 μ L silver nanocubes aqueous solutions and a concentration of 0.3mmol/ of 10 mL prepared by 1 step 1 of embodiment
50 mL reagent bottles are added in the PVP aqueous solutions that L molecular weight is 15000, and after magnetic agitation is uniform, 2 mL a concentration of 0.05 are added
The aqueous ascorbic acid of mol/L, the gold chloride that a concentration of 1.6m mol/L of 6 mL are then slowly added dropwise using syringe pump are water-soluble
Liquid, rate of addition are 0.1 mL/min.The cubic type gold-silver alloy nanoparticles colloidal sol of boring is obtained, its side length is
60nm.Then after hollow gold-silver alloy nanoparticles being washed repeatedly with second alcohol and water repeatedly, it is dispersed in water preservation.
Implementation column 3：
At room temperature, the 80 μ L silver nanocubes aqueous solutions and a concentration of 0.8m of 15 mL prepared by 1 step 1 of embodiment
50 mL reagent bottles are added in the PVP aqueous solutions that mol/L molecular weight is 55000, and after magnetic agitation is uniform, it is a concentration of that 4 mL are added
Then the gold chloride of a concentration of 0.2mmol/L of 10mL is slowly added dropwise in the aqueous ascorbic acid of 0.6 mol/L using syringe pump
Aqueous solution, rate of addition 0.17mL/min.Obtain the cubic type gold-silver alloy nanoparticles colloidal sol of boring, the length of side
For 72nm.Then after hollow gold-silver alloy nanoparticles being washed repeatedly with second alcohol and water repeatedly, it is dispersed in water preservation.
The hollow gold and silver conjunction of the sample 2 of sample 1, the preparation of embodiment 2 prepared by embodiment 1, the sample 3 of the preparation of embodiment 3
The performance characterization of gold nanoparticle：
1, ultraviolet-visible absorption spectroscopy detects：
By sample 1, the aqueous solution of sample 2 and sample 3 uses ultraviolet-visible absorption spectroscopy instrument to detect respectively, obtains ultravioletvisible absorption
Spectrum, specifically as shown in Fig. 1, Fig. 2 and Fig. 3.It can be seen that 3 samples have stronger absorption in visible-range,
Maximum absorption wavelength is respectively 565 nm, 580 nm and 600 nm, illustrates the table of the hollow gold-silver alloy nanoparticles prepared
Face plasma resonance absorption has adjustability, increases with the wall thickness of hollow gold-silver alloy nanoparticles, surface plasma is total
Red shift gradually occurs for absorption of shaking.
2, transmission electron microscope detection and model schematic
By sample 1, sample 2 and sample 3 shoot transmission electron microscope figure, shown in such as Fig. 4, Fig. 5 and Fig. 6, it can be seen that three
A sample is all cube structure, and there are sharp rib and angle in surface, to enhance the active site of SERS effects；Inside be it is hollow,
Surrounding uniform wall thickness is complete, and all very uniformly, the cube length of side respectively may be about 50 nm, 60 nm and 73 nm, wall thickness difference to grain size
About 5nm, 10nm and 14nm.
3, the distribution diagram of element of sample 1
The distribution diagram of element of sample 1 is measured using X-ray energy disperse spectroscopy, as shown in fig. 7, showing to contain Jin Heyin simultaneously in sample 1
Element, and two kinds of Elemental redistributions are uniform.
4, the surface-enhanced Raman scattering activity of sample 1
In order to characterize the SERS activity of nano-particle, by the p-aminophenyl thiophenol of sample 1 and various concentration（4-ABT）It is tried in centrifugation
It is mixed in pipe, after standing 1h at room temperature, the nano-particle ethyl alcohol of functionalization and washing is removed into extra 4-ABT.Finally will
The nano-particle of 4-ABT functions is dispersed in water, and monitors Raman signal, as shown in figure 8, when a concentration of the 10 of 4-ABT-11 mol/
It when L, remains to detect its characteristic peak, illustrates that the hollow gold-silver alloy nanoparticles in sample 1 as SERS substrates, have very high
SERS activity, can be applied to highly sensitive detection.
5, sample 1 detects melamine as SERS substrates
Sample 1 is mixed with the melamine of various concentration in centrifuge tube, after standing 3 h at room temperature, is washed with water not
The melamine of absorption.Then the nano-particle for having adsorbed melamine is dispersed in water, detects Raman signal, works as melamine
A concentration of the 10 of amine-8 It when mol/ L, remains to detect its characteristic peak, illustrates that the hollow gold-silver alloy nanoparticles in sample 1 are made
For SERS substrates, the detection sensitivity for melamine is 10-8 Mol/ L can be applied in highly sensitive detection food
Toxic additive.
Claims (7)
1. a kind of preparation method of the hollow gold-silver alloy nanoparticles of high SERS activity, it is characterised in that the specific steps are：
Step 1：Silver nanocubes are prepared using polyol process, is dispersed in water and is made into mass concentration as 7.4 g/L
Dispersion liquid；
Step 2：10~100 uL of silver nanocubes dispersion liquid and stabilizer PVP and the reducing agent for measuring step 1 preparation are anti-
Magnetic agitation is uniformly mixed bad hematic acid at room temperature；
Step 3：After step 2 acquired solution continuing magnetic force is stirred evenly, aqueous solution of chloraurate is slowly added dropwise into it, obtains
The length of side is the hollow cube type gold-silver alloy nanoparticles colloidal sol of 45~80nm；
Step 4：It is obtained after the gold-silver alloy nanoparticles colloidal sol that step 3 obtains is washed repeatedly repeatedly with second alcohol and water hollow
Gold-silver alloy nanoparticles, and be dispersed in water and preserve.
2. preparation method according to claim 1, it is characterised in that：The molecular weight of stabilizer PVP is in the step 2
15000, one kind in 30000,55000.
3. preparation method according to claim 1, it is characterised in that：In the step 2 volume of stabilizer PVP be 1~
20 mL, a concentration of 0.05~1 × 10-2The volume of mol/L, reducing agent ascorbic acid are 0.1~5 mL, a concentration of 0.01~1
mol/ L。
4. preparation method according to claim 1, it is characterised in that：The volume of aqueous solution of chloraurate is in the step 3
0.5~10 mL, a concentration of 0.1~2 mmol/ L.
5. preparation method according to claim 1, it is characterised in that：The dropwise addition speed of aqueous solution of chloraurate in the step 3
Degree is 0.01~0.2 mL/min.
6. preparation method according to claim 1, it is characterised in that：The hollow electrum nanometer that the step 4 obtains
Particle can operate with micro harmful additive in detection food.
7. preparation method according to claim 1, it is characterised in that：The step of step 1 prepares silver nanocubes
For：12mL is added without water glycol in three neck round bottom flask, 50 min are heated under the conditions of oil bath at 160 DEG C, then to burning
The Na of a concentration of 3 mmol/ L of 140 uL is rapidly added in bottle2S ethylene glycol solutions are continuously added to 3 mL concentration after 2min
For the AgNO of PVP ethylene glycol solutions and a concentration of 265 mmol/ L of 1mL that 180 mmol/ L molecular weight are 400003Second two
Alcoholic solution, whole process all carry out under magnetic stirring, the degree carried out with ultraviolet-visible absorption spectroscopy monitoring reaction, when two
When feature ultraviolet absorption peak is appeared near 350 nm and 435nm, by flask take out immerse ice-water bath come terminate reaction, then from
Heart particle separation diameter is about the silver nanocubes of 43 nm.
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| CN111347059A (en) * | 2020-03-30 | 2020-06-30 | 江南大学 | Synthesis method of porous gold @ silver @ gold nanocubes |
| CN112370079A (en) * | 2020-11-18 | 2021-02-19 | 景德镇陶瓷大学 | Method for detecting thrombus by using ultrasonic Doppler |
| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN113514413A (en) * | 2021-04-22 | 2021-10-19 | 华东师范大学 | Continuous flow synthesis method for controllable particle size of metal-organic framework material |
| CN114767852A (en) * | 2022-04-18 | 2022-07-22 | 杭州师范大学 | Application of light-controlled release type hollow gold-silver nanoprobe in preparation of tumor diagnosis and treatment integrated preparation |
| CN115125490A (en) * | 2022-05-18 | 2022-09-30 | 大连民族大学 | Preparation method of gold nanostructure ordered array SERS substrate with clean surface |
| CN115815612A (en) * | 2022-10-22 | 2023-03-21 | 上海微淳生物科技有限公司 | Preparation method of annular gold and silver nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110202163A (en) * | 2019-05-21 | 2019-09-06 | 山东理工大学 | A kind of preparation method of Ag@Au@Pd nano cubic hollow shell structure |
| CN110202163B (en) * | 2019-05-21 | 2023-03-21 | 山东理工大学 | Preparation method of Ag @ Au @ Pd nano cubic hollow shell structure |
| CN111347059A (en) * | 2020-03-30 | 2020-06-30 | 江南大学 | Synthesis method of porous gold @ silver @ gold nanocubes |
| CN112370079A (en) * | 2020-11-18 | 2021-02-19 | 景德镇陶瓷大学 | Method for detecting thrombus by using ultrasonic Doppler |
| CN112370079B (en) * | 2020-11-18 | 2022-08-26 | 景德镇陶瓷大学 | Method for detecting thrombus by using ultrasonic Doppler |
| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN113514413A (en) * | 2021-04-22 | 2021-10-19 | 华东师范大学 | Continuous flow synthesis method for controllable particle size of metal-organic framework material |
| CN114767852A (en) * | 2022-04-18 | 2022-07-22 | 杭州师范大学 | Application of light-controlled release type hollow gold-silver nanoprobe in preparation of tumor diagnosis and treatment integrated preparation |
| CN115125490A (en) * | 2022-05-18 | 2022-09-30 | 大连民族大学 | Preparation method of gold nanostructure ordered array SERS substrate with clean surface |
| CN115815612A (en) * | 2022-10-22 | 2023-03-21 | 上海微淳生物科技有限公司 | Preparation method of annular gold and silver nanoparticles |
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