CN105710385A - Preparation method for porous hollow gold-silver nano-alloy particles - Google Patents
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Abstract
Provided is a preparation method for porous hollow gold-silver nano-alloy particles. The method includes the following steps that 200 ml of tri-distilled water is added into a reaction vessel and heated to 60-70 DEG C, 30-40 mg of silver nitrate is added, heating is continued until the temperature reaches 90-95 DEG C, afterward, 4 mL of a sodium citrate aqueous solution with the concentration being 10-30 mg/mL is added, a reaction is performed for 5-10 minutes, and the reaction is performed for 30-60 minutes by keeping the temperature at 85-90 DEG C; the reaction temperature is adjusted to 60-90 DEG C, 20-240 mL of a chloroauric acid aqueous solution with the concentration being 1.0*10<-4> mol/L is added dropwise at the speed of 20-30 drops/minute, and the drop addition quantity is determined according to different requirements; and prepared porous hollow gold-silver nano-alloy particles are subjected to centrifugal separation and dispersed in tri-distilled water again, and the porous hollow gold-silver nano-alloy particles can be obtained. By means of the method, tuning of the localized surface plasmon resonance (LSPR) absorption peak of the porous hollow gold-silver nano-alloy particles in a full visible light region can be realized.
Description
Technical field
The present invention relates to the preparation method of a kind of Nanoalloy granule, particularly relate to a kind of Porous hollow gold-silver nanoparticle
The preparation method of alloying pellet.
Background technology
In recent years, metal nanoparticle because of the optics of its uniqueness and photoelectric characteristic, good biocompatibility physico
Learning character be catalyzed, electronics, biomedical sector receives much concern.It is in the metallic particles of nanoscale by external electromagnetic field
During effect, will there is the valency electron collective oscillation relative to cation background in its surface, if the frequency of incident illumination is exactly equal to
This frequency of oscillation, then can produce surface local surface plasma resonance (LSPR) at metal nanoparticle.LSPR can cause gold
Near metal surface, the very big enhancing of electric field, so that metal has the optical property of uniqueness, produces brand-new optical application, surface
Strengthen one of Raman scattering (SERS) application being the most most captivation.
SERS refers to when molecule is in roughened metal surface, and its Raman scattering signal is obvious compared to bulk mole signal
The phenomenon strengthened, has been achieved with the Single Molecule Detection to material on this basis, is widely used at environment, medicine, biology
In field.Research shows, when the LSPR wavelength of SERS enhancing substrate is in laser light incident wavelength and molecule special groups scattered wave
Time between length, maximum SERS will be produced and strengthen.This just requires that the LSPR of substrate has 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
Application.
In order to solve this problem, the method two categories below used at present generally: the first kind be prepare the gold of special appearance,
Silver nano-grain, such as cube, triangle etc., but this type of granule generally requires the substantial amounts of surfactant of use in synthesis and comes
Control the growth of nano-particle so that nano grain surface avtive spot, by occupied by surfactant, greatly reduces granule
SERS strengthen and catalysis activity；Another kind of method is then to prepare gold-silver bimetal nucleocapsid structure, by bimetallic collaborative work
With and two kinds of particles between the coupling of electromagnetic field propose high catalytic activity and the tuning of LSPR wavelength.But, this type of method is to synthesis
The control of condition requires relatively harsh, and between different batches, repeatability is undesirable.
Up to now, there is not yet the most credible and simple and quick preparation in reporting both at home and abroad can divide steadily in the long term
Dissipate, possess in superpower SERS strengthens ability, favorable reproducibility, and and near infrared region region-wide at visible ray realize surface etc. from
The method of daughter resonant frequency adjustable gold-silver alloy nano-particle.Therefore, invention possesses Jin-silver conjunction of above special performance
The preparation method of gold nano grain is an important technology difficult problem urgently to be resolved hurrily.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of Porous hollow gold-silver nanoparticle alloying pellet and preparation side thereof
Method, to solve existing technology of preparing poor stability, granule LSPR cannot realize hypersorption and SERS letter in visible region
The problem of number poor reproducibility.
For achieving the above object, present invention provide the technical scheme that
The preparation method of a kind of Porous hollow gold-silver nanoparticle alloying pellet, described method comprises the steps:
(1) in reaction vessel, add No. tri-distilled water of 200mL and be heated to 60-70 DEG C, adding 30-40mg silver nitrate,
After continuing to be heated to 90-95 DEG C, adding 4mL concentration is the sodium citrate aqueous solution of 10-30mg/mL, reacts 5-10 minute, then
Temperature maintaining 85-90 DEG C react 30-60 minute, prepared particle diameter is the single dispersing silver nano-grain of 30-50nm；
(2) regulation reaction temperature be 60-90 DEG C, with 20-30 drip/minute speed dropping concentration for 1.0 × 10-4mol/L
Aqueous solution of chloraurate 20-240mL, use ultraviolet spectrophotometry product is detected in real time, according to subsequent applications to gold-
The different requirement of silver alloy particles LSPR determines dripping quantity；
(3) the Porous hollow gold-silver alloy nano-particle centrifugation that step (2) is prepared, and again it is dispersed in three times
In distilled water, to obtain final product.
Further, described aqueous solution of chloraurate is to be dividedly in some parts, and within every 30 minutes, adds 20mL.
Further, the reducing agent beyond trisodium citrate and stabilizer are not used.
Further, reaction temperature 60-80 DEG C of step (2).
Further, the reaction temperature of step (2) 70 DEG C.
A kind of Porous hollow gold-silver nanoparticle alloying pellet.
Porous hollow gold-silver nanoparticle alloying pellet is as the application of surface enhanced Raman substrate.
Use technique scheme, there is advantages that
The first, in the present invention single reducing agent is used, it is not necessary to use stabilizer, under Particular craft, prepare particle diameter divide
The uniform silver nano-grain of cloth, is the first solution；Utilize the metal activity difference between silver and gold, at a certain temperature, past
First solution is quantitatively adding chlorauric acid solution, utilizes displacement reaction to displace gold therein, and the silver ion generated is further
It is reduced to silver nano-grain by the reducing agent in solution, defines the hollow alloying pellet of gold silver.By to reaction temperature, silver-colored, golden
Reactant ratio, the control realization of the dosage of reducing agent is to particle size and the precision control of surface gold silver ratio, thus reality
The now effective tuning to gained gold-silver alloy granule LSPR.
The second, in preparation method, this law is bright by being dividedly in some parts chlorauric acid solution and temperature adjusting, is allowed to preparation
Gold-silver alloy granule possesses the SERS reinforced effects of excellence.
3rd, strengthening substrate as a kind of novel Raman, the gold-silver alloy granule of the present invention can use different laser
Time meet LSPR and absorb between peak position excitation wavelength and characteristic peak Raman scattering wavelength, it is thus achieved that optimal SERS reinforced effects and
Excellent signal reproducibility.
4th, the preparation method of the present invention is simple, and the ownership is standby can be realized " one kettle way " and complete；Only need to use single going back
Former dose, it is not necessary to use surfactant and other stabilizers, made alloying pellet can long-time stable preserve without generation
The reunion of intergranular；Preparation uses the weak single reducing agent of surface adsorption, it is to avoid the many reducing agents of use and the reaction that causes
Some complicated and uncontrollable impacts in journey, and effectively prevent surface adsorption；Adjust by being dividedly in some parts chlorauric acid solution and temperature
Control, the gold-silver alloy granule being allowed to preparation possesses the SERS reinforced effects of excellence.
5th, by the regulation and control of reaction condition being realized gold-silver alloy nano-particle LSPR in visible region
Full regulation and control, and may extend near infrared region, its tuning effect and existing patent and reported in literature realize the breakthrough of matter；Prominent
SERS reinforced effects, under 785nm laser excitation, gold-silver alloy nano-particle to the enhancer of phenylmercaptan. up to 7.8 ×
107The order of magnitude, to phenylmercaptan. optimum detection concentration up to 2.0 × 10-14mol/L.50 data points of random detection, it is marked relatively
Quasi-deviation is only 4.3%.
Accompanying drawing explanation
Fig. 1 be embodiment 2 made Nano silver grain TEM figure, hollow porous gold-silver alloy nano-particle TEM figure and
EDX element image；
Fig. 2 is the TEM figure of the hollow porous gold-silver alloy nano-particle of preparation in embodiment 1-4；
Fig. 3 is the ultraviolet-visible-near-infrared spectrum of different gold chloride consumption gained nano-particle in embodiment 5；
Fig. 4 is the SERS figure preparing gold-silver alloy nano grain surface in embodiment 5-6；
Fig. 5 is that phenylmercaptan. is at the gold-silver alloy nano grain surface two dimension SERS spectrogram obtained by the present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with the accompanying drawings and embodiment, right
The present invention is further elaborated.Should be appreciated that structure chart described herein and specific embodiment are only in order to explain this
Invention, is not intended to limit the present invention.
Embodiment 1-4
Prepared by silver nano-grain: add 36mg after adding No. tri-distilled water of 200mL in there-necked flask and being heated to 70 DEG C
Silver nitrate, and to continue to be heated to solution be to be rapidly added the sodium citrate aqueous solution that 4mL concentration is 30mg/mL after slight boiling condition,
Reacting 8 minutes at 95 DEG C, then temperature maintains 85-90 DEG C and reacts 60 minutes, prepared particle diameter is about the single dispersing of 30-40nm
Silver nano-grain.Regulation reaction temperature is respectively 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, within every 30 minutes, add 20mL concentration be 1.0 ×
10-4The aqueous solution of chloraurate of mol/L is to 160mL.SPR and the Raman of test gained alloy nano particle strengthens respectively.
Embodiment 5
Add 36mg silver nitrate after adding No. tri-distilled water of 200mL in there-necked flask and being heated to 70 DEG C, and continue to add
Heat is rapidly added, after being slight boiling condition to solution, the sodium citrate aqueous solution that 4mL concentration is 30mg/mL, reacts 8 minutes at 95 DEG C,
Then temperature maintaining 85-90 DEG C react 60 minutes, prepared particle diameter is about the single dispersing silver nano-grain of 30-40nm.Regulation
Reaction temperature is 70 DEG C, and every 30 minutes add 20mL concentration is 1.0 × 10-4The aqueous solution of chloraurate of mol/L is to 240mL.Often
Sample and test the different SPR adding product under volume conditions during 20mL sample-adding interval and Raman strengthens.
Embodiment 6
Add 36mg silver nitrate after adding No. tri-distilled water of 200mL in there-necked flask and being heated to 70 DEG C, and continue to add
Heat is rapidly added, after being slight boiling condition to solution, the sodium citrate aqueous solution that 4mL concentration is 30mg/mL, reacts 8 minutes at 95 DEG C,
Then temperature maintaining 85-90 DEG C react 60 minutes, prepared particle diameter is about the single dispersing silver nano-grain of 30-40nm.Regulation
Reaction temperature is 70 DEG C, and using and dripping concentration continuously without interval mode continuously is 1.0 × 10-4The aqueous solution of chloraurate of mol/L is extremely
160mL.When sampling and test different injection volume, SPR and the Raman of product strengthen.
It is substrate by hollow gold-silver nanoparticle alloying pellet obtained in embodiment 1-6,785nm excitation wavelength, identical inspection
Under the conditions of survey, test it in SERS reinforced effects with phenylmercaptan. for probe molecule.
For ease of comparing, main for above-described embodiment 1-6 preparation condition, result are arranged list.
Table one
Above-mentioned test result indicate that at 70 DEG C, it is thus achieved that hollow electrum granule have best SERS reinforced effects；And
It is dividedly in some parts the hollow gold silver conjunction that the gold chloride hollow electrum granule obtained and the same amount gold chloride once added obtain
Gold grain is compared, and also has more preferable reinforced effects.By the regulation and control of reaction condition can be realized gold-silver alloy nano-particle
The LSPR full regulation and control in visible region, and may extend near infrared region, its tuning effect and existing patent and document report
Lead and compare the breakthrough realizing matter；
Described in detail below in conjunction with the accompanying drawings.
From Fig. 1 a, silver nano-grain even particle size distribution, size about 30-40nm.Can clearly be observed by Fig. 1 b
Hollow structure and the loose structure of particle surface to granular center position.Fig. 1 c is the high-resolution transmission electricity of single alloying pellet
Mirror figure, Fig. 1 d-g is the details in a play not acted out on stage, but told through dialogues photo of single alloy nanoparticle and the silver-colored and element image of gold.In figure, gold and silver are closing
Gold grain surface is fusion together, is uniformly distributed, thus demonstrating alloying pellet is an entirety rather than simple by Jin Heyin
Nano-particle is piled up by the method for physics and is formed.Fig. 1 g is the C element image at particle surface, shows at alloying pellet table
Face is adsorbed with citrate ion, and the characteristic of its negative charge makes particle surface electrostatic repulsion, it is ensured that particle is without adding
Any protectant under the conditions of, do not occur in the long period reunite and be stabilized preservation.
Suitably temperature is prepared extremely critical for the success of alloying pellet.When temperature is set as between 70 DEG C-80 DEG C,
When especially temperature controls 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 the most clear.More importantly, the pattern of nano-particle and surface plasma resonance frequency can be because of
This obtains finely regulating.
In the present invention, the feed postition of chlorauric acid solution is most important.Comparative example 2 and embodiment 6, identical
Reaction condition under, take in batches and combine sample-adding interval method be slowly added dropwise Porous hollow Jin-silver that gold chloride is obtained
Alloying pellet is compared with continuously every continuous dropping mode, and its reinforced effects adds nearly 7 times.
Gold-silver alloy nano-particle absorption spectrum in ultraviolet-visible-near infrared region is had aobvious by gold chloride consumption
The impact write.The uv absorption of embodiment 5 gained gold-silver nanoparticle alloying pellet is listed in accompanying drawing 3, and as seen from the figure, silver sol is can
Seeing that the LSPR peak in light region is positioned at 409nm, along with the addition of gold chloride, the absworption peak at 409nm is gradually lowered, until disappearing
Lose.Meanwhile, occurring in that new absworption peak on long wave direction, this can be attributed to the resonance coupling between gold-silver alloy granule
And the new LSPR peak produced.Break through previous patent and reported in literature is (displacement 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, by changing
Reaction condition even can realize the absorption near infrared region.
Fig. 4 show 785nm wavelength and excites down, and phenylmercaptan. molecule is schemed at 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 peak of silver nano-grain is wholly absent, but the SPR of now gold silver coupling absorbs
Peak is at 630nm, and away from excitation wavelength and the dispersion wavelength of phenylmercaptan. characteristic peak, therefore reinforced effects is poor, shows as peak intensity
Minimum.With the further increase of dosage, absworption peak continues red shift, and the SERS intensity of phenylmercaptan. characteristic peak gradually strengthens.Work as throwing
When dosage is 160mL, nano-particle SPR absworption peak is positioned near 800nm, and this formant is placed exactly in optical maser wavelength and feature
Between peak dispersion wavelength, therefore obtain maximum and strengthen.Continuing to increase with dosage, SPR continues red shift, arrives near infrared region,
Its reinforced effects presents reduction trend owing to being gradually distance from 785nm excitation wavelength, but SPR now is for using near-infrared
The light source that 830nm laser and 1064nm laser both have been commercialized provides guarantee, this be previously reported in do not occurred.
Through calculating, under 785nm excitation wavelength, the SERS of this gold-silver alloy nano-particle phenylmercaptan. molecule to being adsorbed in surface increases
The strong factor is up to 7.8 × 107, when phenylmercaptan. concentration as little as 2.0 × 10-14Mol/L remains to detect that phenylmercaptan. is positioned at 1074cm-1
The Characteristic Raman peak at place.
From accompanying drawing 5 figure, same batch difference sample spot and different batches substrate have shown excellent measurement weight
Existing property, its relative standard deviation is calculated as 4.3%.
Embodiment described above only have expressed embodiments of the present invention, and it describes more concrete and detailed, but can not
Therefore the restriction to the scope of the claims of the present invention it is interpreted as.It should be pointed out that, for the person of ordinary skill of the art,
Without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the protection model of the present invention
Enclose.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet, it is characterised in that described method includes walking as follows
Rapid:
(1) in reaction vessel, add No. tri-distilled water of 200mL and be heated to 60-70 DEG C, adding 30-40mg silver nitrate, continue
After being heated to 90-95 DEG C, adding 4mL concentration is the sodium citrate aqueous solution of 10-30mg/mL, reacts 5-10 minute, then by temperature
Degree maintains 85-90 DEG C and reacts 30-60 minute, and prepared particle diameter is the single dispersing silver nano-grain of 30-50nm；
(2) regulation reaction temperature be 60-90 DEG C, with 20-30 drip/minute speed dropping concentration for 1.0 × 10-4The chlorine of mol/L
Auric acid aqueous solution 20-240mL, uses ultraviolet spectrophotometry to detect product in real time, closes Jin-silver according to subsequent applications
The different requirement of gold grain LSPR determines dripping quantity；
(3) the Porous hollow gold-silver alloy nano-particle centrifugation that step (2) is prepared, and again it is dispersed in three distillations
In water, to obtain final product.
2. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, it is characterised in that described chlorine gold
Aqueous acid is to be dividedly in some parts, and within every 30 minutes, adds 20mL.
3. the method as described in any one of claim 2, is characterized by: does not use the reducing agent beyond trisodium citrate and stablizes
Agent.
4. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, is characterized by: step (2)
Reaction temperature 60-80 DEG C.
5. the preparation method of Porous hollow gold-silver nanoparticle alloying pellet as claimed in claim 1, is characterized by: step (2)
Reaction temperature 70 DEG C.
6. the Porous hollow gold-silver nanoparticle alloying pellet prepared by preparation method as arbitrary in claim 1-5.
7. the Porous hollow gold-silver nanoparticle alloying pellet prepared by preparation method as arbitrary in claim 1-5 is as surface enhanced
The application of Raman substrate.
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