CN105710385B - A kind of preparation method of Porous hollow gold and silver Nanoalloy particle - Google Patents
A kind of preparation method of Porous hollow gold and silver Nanoalloy particle Download PDFInfo
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- CN105710385B CN105710385B CN201610056490.6A CN201610056490A CN105710385B CN 105710385 B CN105710385 B CN 105710385B CN 201610056490 A CN201610056490 A CN 201610056490A CN 105710385 B CN105710385 B CN 105710385B
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0549—Hollow particles, including tubes and shells
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
A kind of preparation method of Porous hollow gold and silver Nanoalloy particle, method comprise the following steps：200mL is added in reaction vessel and distilled water and is heated to 60 70 DEG C three times, add 30 40mg silver nitrates, continue after being heated to 90 95 DEG C, add the sodium citrate aqueous solution that 4mL concentration is 10 30mg/mL, react 5 10 minutes, temperature is maintained into 85 90 DEG C reacts 30 60 minutes, and regulation reaction temperature is 60 90 DEG C, aqueous solution of chloraurate 20 240mL of the concentration as 1.0 × 10 4mol/L is added dropwise using the speed of 20 30 drops/minute, requires to determine dripping quantity according to different；Obtained Porous hollow gold-silver alloy nano particle is centrifuged, and is dispersed in again in distilled water three times, is produced.This method can realize that the product LSPR absworption peaks of preparation tune in total visible light region.
Description
Technical field
The present invention relates to a kind of preparation method of Nanoalloy particle, more particularly to a kind of Porous hollow gold-silver nanoparticle
The preparation method of alloying pellet.
Background technology
In recent years, metal nanoparticle because its unique optics and photoelectric characteristic, good biocompatibility it is physico
Learn property be catalyzed, electronics, biomedical sector receives much concern.Metallic particles in nanoscale is by external electromagnetic field
During effect, collective oscillation of the valence electron relative to cation background will occur for its surface, if the frequency of incident light is exactly equal to
The frequency of oscillation, then it can produce surface local surface plasma resonance (LSPR) in metal nanoparticle.LSPR can cause gold
The very big enhancing of electric field near metal surface, so that metal has unique optical property, produces brand-new optical application, surface
It is wherein most one of application of attraction to strengthen Raman scattering (SERS).
SERS refers to that its Raman scattering signal is obvious compared to bulk mole signal when molecule is in roughened metal surface
The phenomenon of enhancing, the Single Molecule Detection to material is had been achieved with this basis, be widely used in environment, medicine, biology
Deng field.Research shows, when the LSPR wavelength of SERS enhancing substrates is in laser light incident wavelength and molecule special groups scattered wave
When between length, maximum SERS enhancings will be produced.This requires the LSPR of substrate to have tunability.But single metallic nanoparticle
Son often shows strong and narrow absorption band in ultraviolet and visible waveband, significantly limit it in surface-enhanced Raman field
Using.
In order to solve this problem, the method two categories below of generally use at present：The first kind be prepare special appearance gold,
Silver nano-grain, such as cube, triangle, but such particle generally requires to come using substantial amounts of surfactant in synthesis
Control the growth of nano particle so that nano grain surface avtive spot greatly reduces particle occupied by surfactant
SERS enhancing and catalytic activity；Another kind of method is then to prepare gold-silver bimetal core shell structure, is made by bimetallic collaboration
With and two kinds of particles between the coupling of electromagnetic field improve the tuning of catalytic activity and LSPR wavelength.However, such method is to synthesis
The control of condition requires relatively harsh, and reappearance is undesirable between different batches.
So far, both at home and abroad in report there is not yet definite credible and simple and quick preparation can divide steadily in the long term
Dissipate, possess superpower SERS enhancing ability, favorable reproducibility, and visible ray is region-wide and near infrared region in realize surface etc. from
The method of the adjustable gold-silver alloy nano particle of daughter resonant frequency.Therefore, Jin-silver that invention possesses above special performance closes
The preparation method of gold nano grain is important technology problem urgently to be resolved hurrily.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of Porous hollow gold-silver nanoparticle alloying pellet and its preparation side
Method, poor to solve existing technology of preparing stability, particle LSPR can not realize hypersorption and SERS letters in visible region
The problem of number poor reproducibility.
For achieving the above object, technical scheme provided by the invention is：
A kind of preparation method of Porous hollow gold-silver nanoparticle alloying pellet, methods described comprise the following steps：
(1) 200mL is added in reaction vessel and distilled water and is heated to 60-70 DEG C three times, adds 30-40mg silver nitrates,
Continue after being heated to 90-95 DEG C, add the sodium citrate aqueous solution that 4mL concentration is 10-30mg/mL, react 5-10 minutes, then
Temperature is maintained into 85-90 DEG C of reaction 30-60 minute, the single dispersing silver nano-grain that particle diameter is 30-50nm is made；
(2) it is 60-90 DEG C to adjust reaction temperature, and concentration is added dropwise as 1.0 × 10-4mol/L using the speed of 20-30 drops/minute
Aqueous solution of chloraurate 20-240mL, product is detected in real time using ultraviolet spectrophotometry, according to subsequent applications to gold-
The different of silver alloy particles LSPR require to determine dripping quantity；
(3) Porous hollow gold-silver alloy nano particle made from step (2) is centrifuged, and be dispersed in again three times
In distilled water, produce.
Further, the aqueous solution of chloraurate is to be added portionwise, and adds 20mL within every 30 minutes.
Further, without using the reducing agent and stabilizer beyond trisodium citrate.
Further, 60-80 DEG C of the reaction temperature of step (2).
Further, 70 DEG C of the reaction temperature of step (2).
A kind of Porous hollow gold-silver nanoparticle alloying pellet.
Porous hollow gold-application of the silver nanoparticle alloying pellet as surface enhanced Raman substrate.
Using above-mentioned technical proposal, the present invention has the advantages that：
Firstth, single reducing agent is used in the present invention, and without using stabilizer, particle diameter point is prepared under Particular craft
The uniform silver nano-grain of cloth, it is the first solution；It is at a certain temperature, past using the active sex differernce of metal between silver and gold
Chlorauric acid solution is quantitatively adding in first solution, gold therein is displaced using reaction is replaced, and the silver ion generated is further
Silver nano-grain is reduced to by the reducing agent in solution, forms the hollow alloying pellet of gold and silver.By to reaction temperature, silver, gold
The precision control to particle size and surface gold and silver ratio is realized in reactant ratio, the control of the dosage of reducing agent, so as to real
Now to gained gold-silver alloy particle LSPR effective tuning.
Secondth, in preparation method, this law is bright by the way that chlorauric acid solution and temperature adjusting is added portionwise, and is allowed to what is prepared
Gold-silver alloy particle possesses excellent SERS enhancing effects.
3rd, substrate is strengthened as a kind of new Raman, gold-silver alloy particle of the invention can use different laser
When meet that LSPR is absorbed between peak position excitation wavelength and characteristic peak Raman scattering wavelength, obtain optimal SERS enhancing effects and
Excellent signal reproducibility.
4th, preparation method of the invention is simple, and " one kettle way " completion can be achieved in all prepare；Only need to go back using single
Former agent, without using surfactant and other stabilizers, made alloying pellet can long-time stable preserve without occurring
The reunion of intergranular；Using the single reducing agent that adsorption is weak in preparation, avoid and reacted using caused by more reducing agents
Some in journey are complicated and uncontrollable influence, and effectively prevent adsorption；Adjusted by the way that chlorauric acid solution and temperature is added portionwise
Control, the gold-silver alloy particle for being allowed to prepare possess excellent SERS enhancing effects.
5th, it can realize gold-silver alloy nano particle LSPR in visible region by the regulation and control to reaction condition
Full regulation and control, and may extend near infrared region, it tunes the breakthrough that effect realizes matter with existing patent and reported in literature；It is prominent
SERS enhancing effects, under 785nm laser excitations, gold-silver alloy nano particle to the enhancer of benzenethiol up to 7.8 ×
107The order of magnitude, to benzenethiol optimum detection concentration up to 2.0 × 10-14mol/L.50 data points of random detection, its relative mark
Quasi- deviation is only 4.3%.
Brief description of the drawings
Fig. 1 be embodiment 2 it is made Nano silver grain TEM figure, Porous hollow gold-silver nanoparticle alloying pellet TEM figure and
EDX element images；
Fig. 2 is the TEM figures of the Porous hollow gold-silver nanoparticle alloying pellet prepared in embodiment 1-4；
Fig. 3 be Porous hollow gold-silver nanoparticle alloying pellets obtained by different gold chloride dosages in embodiment 5 ultraviolet-visible-
Near infrared spectrum；
Fig. 4 is the SERS figures that Porous hollow gold-silver nanoparticle alloying pellet surface is made in embodiment 5-6；
Fig. 5 is benzenethiol in the Porous hollow gold obtained by the present invention-silver nanoparticle alloying pellet surface two dimension SERS spectrograms.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings and embodiment, it is right
The present invention is further elaborated.It should be appreciated that structure chart described herein and specific embodiment are only explaining this
Invention, is not intended to limit the present invention.
Embodiment 1-4
It is prepared by silver nano-grain：200mL is added in three-necked flask and distilled water and adds 36mg after being heated to 70 DEG C three times
Silver nitrate, and continue to be heated to solution in being rapidly added the sodium citrate aqueous solution that 4mL concentration is 30mg/mL after slight boiling condition,
Reacted at 95 DEG C 8 minutes, temperature is then maintained 85-90 DEG C and reacted 60 minutes, the single dispersing that obtained particle diameter is about 30-40nm
Silver nano-grain.Regulation reaction temperature is respectively 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, add within every 30 minutes 20mL concentration be 1.0 ×
10-4Mol/L aqueous solution of chloraurate is to 160mL.The SPR of test gained alloy nano particle and Raman enhancing respectively.
Embodiment 5
200mL is added in three-necked flask and distilled water and 36mg silver nitrates are added after being heated to 70 DEG C three times, and continue plus
Heat, in the sodium citrate aqueous solution that 4mL concentration is 30mg/mL is rapidly added after slight boiling condition, is reacted 8 minutes to solution at 95 DEG C,
Then temperature is maintained into 85-90 DEG C to react 60 minutes, the single dispersing silver nano-grain that obtained particle diameter is about 30-40nm.Regulation
Reaction temperature is 70 DEG C, and it is 1.0 × 10 to add within every 30 minutes 20mL concentration-4Mol/L aqueous solution of chloraurate is to 240mL.Often
Sampled during 20mL sample-adding intervals and test the SPR of product and Raman enhancing under different addition volume conditions.
Embodiment 6
200mL is added in three-necked flask and distilled water and 36mg silver nitrates are added after being heated to 70 DEG C three times, and continue plus
Heat, in the sodium citrate aqueous solution that 4mL concentration is 30mg/mL is rapidly added after slight boiling condition, is reacted 8 minutes to solution at 95 DEG C,
Then temperature is maintained into 85-90 DEG C to react 60 minutes, the single dispersing silver nano-grain that obtained particle diameter is about 30-40nm.Regulation
Reaction temperature is 70 DEG C, uses and concentration is continuously continuously added dropwise without interval mode as 1.0 × 10-4Mol/L aqueous solution of chloraurate is extremely
160mL.The SPR of product and Raman enhancing when sampling and testing different injection volumes.
It is substrate by hollow gold-silver nanoparticle alloying pellet obtained in embodiment 1-6,785nm excitation wavelengths, identical inspection
Under the conditions of survey, it is tested in SERS enhancing effects by probe molecule of benzenethiol.
For ease of comparing, the main preparation conditions of above-described embodiment 1-6, result are arranged into list.
Table one
It is above-mentioned test result indicates that at 70 DEG C, the hollow electrum particle of acquisition has best SERS enhancing effects；And
The hollow gold and silver for the same amount gold chloride acquisition that the hollow electrum particle of gold chloride acquisition is added portionwise and once adds closes
Gold grain is compared, and also has more preferable enhancing effect.Gold-silver alloy nano particle can be realized by the regulation and control to reaction condition
Full regulation and control of the LSPR in visible region, and near infrared region is may extend into, it tunes effect and existing patent and document report
Lead compared to the breakthrough for realizing matter；
Described in detail below in conjunction with the accompanying drawings.
From Fig. 1 a, silver nano-grain particle diameter distribution is uniform, particle size about 30-40nm.Can clearly it be observed by Fig. 1 b
To the hollow structure at granular center position and the loose structure of particle surface.Fig. 1 c are the high-resolution transmission electricity of single alloying pellet
Mirror figure, Fig. 1 d-g are the details in a play not acted out on stage, but told through dialogues photo and the element image of silver and gold of single alloy nanoparticle.Gold and silver are closing in figure
Gold grain surface is fusion together, is uniformly distributed, and is an entirety so as to demonstrate alloying pellet, rather than simply by Jin Heyin
Nano particle is piled up by the method for physics to be formed.Fig. 1 g be C element in the image of particle surface, show in alloying pellet table
Face is adsorbed with citrate ion, and the characteristic of its negative electrical charge causes particle surface electrostatic repulsion, ensure that particle without addition
It is any it is protectant under the conditions of, do not occur in the long period reunite and be stabilized preservation.
Suitable temperature for alloying pellet it is successful prepare it is extremely critical.When temperature is set as between 70 DEG C -80 DEG C,
When especially temperature control is near 70 DEG C, as shown in Figure 2, electrum is generated in order, and hollow loose structure is with chlorine
The increase of auric acid addition is gradually clear.Can be because more important is the pattern and surface plasma resonance frequency of, nano particle
This obtains finely regulating.
In the present invention, the feed postition of chlorauric acid solution is most important.Comparative example 2 and embodiment 6, it is identical
Reaction condition under, take in batches and combine sample-adding interval method Porous hollow Jin-silver that gold chloride is obtained is slowly added dropwise
For alloying pellet compared with without continuous dropwise addition mode is spaced, its enhancing effect adds nearly 7 times.
Gold chloride dosage has aobvious to absorption spectrum of the gold-silver alloy nano particle in ultraviolet-visible-near infrared region
The influence of work.The UV absorption of the gained gold of embodiment 5-silver nanoparticle alloying pellet is listed in accompanying drawing 3, and as seen from the figure, silver sol is can
See that the LSPR peaks in light region are located at 409nm, with the addition of gold chloride, the absworption peak at 409nm gradually reduces, until disappearing
Lose.Meanwhile occurring new absworption peak on long wave direction, this can be attributed to the resonance coupling between gold-silver alloy particle
And caused new LSPR peaks.Break through previous patent and reported in literature is (displacement for being typically only capable of producing 20 nanometers), with this
Gold-silver alloy nano particle prepared by method, its LSPR absworption peak can realize the tuning in total visible light region, pass through change
Reaction condition can even realize the absorption near infrared region.
Fig. 4 show 785nm wavelength and excited down, and benzenethiol molecule is schemed in the SERS of gold-silver alloy nano grain surface.When
When gold chloride dosage is less, nano particle outer layer is not yet surrounded by gold-silver alloy, shows as SERS intensity with silver content
Reduce and reduce.When dosage is 100mL, the SPR peaks of silver nano-grain are wholly absent, but the SPR of now gold and silver coupling absorbs
Peak is at 630nm, the dispersion wavelength away from excitation wavelength and benzenethiol characteristic peak, therefore enhancing effect is poor, shows as peak intensity
It is minimum.With the further increase of dosage, absworption peak continues red shift, and the SERS intensity of benzenethiol characteristic peak gradually strengthens.Work as throwing
When dosage is 160mL, nano particle SPR absworption peaks are located near 800nm, and this formant is placed exactly in optical maser wavelength and feature
Between peak dispersion wavelength, therefore obtain maximum enhancing.Continuing to increase with dosage, SPR continues red shift, reaches near infrared region,
Reduction trend is presented due to being gradually distance from 785nm excitation wavelengths in its enhancing effect, but SPR now is to use near-infrared
830nm laser and 1064nm laser both light sources having been commercialized provide guarantee, this be it is previously reported in do not occurred.
By calculating, under 785nm excitation wavelengths, the gold-silver alloy nano particle increases to the SERS for being adsorbed in the benzenethiol molecule on surface
The strong factor is up to 7.8 × 107, when benzenethiol concentration as little as 2.0 × 10-14Mol/L remains to detect that benzenethiol is located at 1074cm-1
The Characteristic Raman peak at place.
From the figure of accompanying drawing 5, same batch difference sample spot and different batches substrate have shown excellent measurement weight
Existing property, its relative standard deviation are calculated as 4.3%.
Embodiment described above only expresses embodiments of the present invention, and its description is more specific and detailed, but can not
Therefore it is interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art,
Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection model of the present invention
Enclose.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (7)
1. a kind of preparation method of Porous hollow gold-silver nanoparticle alloying pellet, it is characterised in that the preparation method includes as follows
Step：
(1) 200mL is added in reaction vessel and distilled water and is heated to 60-70 DEG C three times, 30-40mg silver nitrates is added, continues
After being heated to 90-95 DEG C, the sodium citrate aqueous solution that 4mL concentration is 10-30mg/mL is added, 5-10 minutes are reacted, then by temperature
Degree maintains 85-90 DEG C of reaction 30-60 minute, and the single dispersing silver nano-grain that particle diameter is 30-50nm is made；
(2) it is 60-90 DEG C to adjust reaction temperature, and concentration is added dropwise as 1.0 × 10 using the speed of 20-30 drops/minute-4Mol/L chlorine
Auric acid aqueous solution 20-240mL, Porous hollow gold-silver alloy nano particle is detected in real time using ultraviolet spectrophotometry,
The different of gold-silver alloy particle LSPR are required to determine dripping quantity according to subsequent applications；
(3) Porous hollow gold-silver alloy nano particle made from step (2) is centrifuged, and is dispersed in and distills three times again
In water, produce；
Wherein, the aqueous solution of chloraurate is to be added portionwise.
2. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, it is characterised in that the chlorine gold
Aqueous acid rate of addition is to add 20mL in every 30 minutes.
3. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 2, it is characterized in that：Without using lemon
Reducing agent and stabilizer beyond lemon acid trisodium.
4. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, it is characterized in that：Step (2)
60-80 DEG C of reaction temperature.
5. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, it is characterized in that：Step (2)
70 DEG C of reaction temperature.
6. Porous hollow gold-silver nanoparticle alloying pellet as prepared by any preparation methods of claim 1-5.
7. Porous hollow gold-silver nanoparticle alloying pellet as prepared by any preparation methods of claim 1-5 is as surface enhanced
The application of Raman substrate.
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| CN106501245B (en) * | 2016-10-20 | 2019-11-08 | 中南林业科技大学 | The preparation method of nanogold contracted payment colorimetric probe and its method for detecting lead ion |
| CN106862587B (en) * | 2017-01-20 | 2019-01-25 | 重庆市科学技术研究院 | The preparation method of porous nano silver |
| CN107151807B (en) * | 2017-04-28 | 2018-12-21 | 中国科学院合肥物质科学研究院 | Porous golden micro-nano structure of hemispherical shell and its preparation method and application |
| CN107350468B (en) * | 2017-06-22 | 2019-05-03 | 中国科学院合肥物质科学研究院 | A kind of three-dimensional porous gold-silver alloy nano material and the preparation method and application thereof |
| CN107999782A (en) * | 2017-11-09 | 2018-05-08 | 中国科学院合肥物质科学研究院 | A kind of preparation method of electrum hollow polyhedral |
| CN108580919B (en) * | 2018-03-08 | 2021-10-15 | 温州大学 | Preparation method of silver-core mesoporous gold nanostructure material, surface-enhanced Raman detection probe and application thereof |
| CN108372314B (en) * | 2018-03-29 | 2021-03-12 | 景德镇陶瓷大学 | Preparation method of hollow gold-silver alloy nanoparticles with high SERS activity |
| CN108941532A (en) * | 2018-07-24 | 2018-12-07 | 宝鸡文理学院 | A kind of gold nano-material and preparation method thereof of hollow porous tubes shape structure |
| CN109719305B (en) * | 2019-02-11 | 2021-11-16 | 石河子大学 | Preparation method of Au-Ag alloy nanoparticles with adjustable plasmon resonance |
| CN109967760B (en) * | 2019-04-17 | 2021-11-30 | 宁波大学 | Dendritic silver nanosheet material containing serrated inner surface and preparation method and application thereof |
| 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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