CN105598442A - One-dimensional chainlike Au-Ag core-shell nanostructure, self-assembly preparing method and SERS application - Google Patents
One-dimensional chainlike Au-Ag core-shell nanostructure, self-assembly preparing method and SERS application Download PDFInfo
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Abstract
The invention relates to a one-dimensional chainlike Au-Ag core-shell nanostructure, a self-assembly preparing method and SERS application. Nanoparticles of an Au core and Ag shell structure are synthesized through a liquid-phase synthesis method and a seed crystal growth method; the obtained nanoparticles of the core and shell structure are dispersed in a mixed solution of inorganic salt and ethyl alcohol; a certain quantity of alkaline solution is taken, and the mixed solution is added to be stirred and centrifuged to obtain the one-dimensional chainlike structure. By controlling the electrostatic mutual acting force between the core-shell nanoparticles, the one-dimensional nanometer structure of different Au core sizes and different Ag shell thicknesses is obtained through self-assembly; the method does not need the aid of any templates or surface active agents, the assembly process is simple, the Au core sizes and shell thicknesses are easy to regulate and control, products are easy to separate, the surface Raman enhancing effect of organic substance molecules is remarkable, a preparation system is green and environmentally friendly, no toxic or harmful solvent is added, prepared products are stable in performance, preparation cost is low, the application range is wide, repeatability is high, and large-scale preparation is easy.
Description
Technical field
The invention belongs to Au, Ag nano particle preparation field, relate to the preparation method of Au-Ag core-shell nano structure, especiallyA kind of one-dimensional chain Au-Ag core-shell nano structure, self-assembly preparation method thereof and SERS with high surface Raman enhancement effect shouldWith.
Background technology
Raman spectrum, as a kind of inelastic scattering spectrum, is by the scattering spectrum different from incident light frequency carried out to analyzing moleculesVibration, rotation, the various normal mode vibration frequencies of intramolecule and the information about vibration level aspect can be provided. Traditional drawsGraceful scattering spectrum signal a little less than, often lack high sensitivity as Information Read-Out means.
SERS (SurfaceEnhancedRamanscattering, SERS) refers to and is positioned at raw sugar metal surfaceThe phenomenon that the Raman signal of little molecule itself is enhanced. This phenomenon is at necks such as Surface Science, analysis science and bioscienceTerritory is widely used, for structure and the process on the various surfaces of deep sign (interface) provide the information on molecular level, as mirrorOther molecule or ion are at the surface texture of surperficial bonding, configuration and orientation and material. About the enhancing mechanism of SERS, thoughSo still there is up till now dispute, but comparatively accreditation be Electromagnetic enhancement mechanism, and " focus " (hot relating in this mechanismSpot)-as refer in the molecular aggregation of some nanoparticles, the region of the space part between adjacent nano particle. ThisThe SERS effect in region is the strongest. How to build efficient homogeneous and contain the more SERS substrate of " focus ", become SERSThe focus of research field and difficult point.
Au and Ag nano particle, especially have surface plasma resonance effect (surfaceplasmonicresonance, SPR)Au-Ag heterogeneous structural nano particle, enjoy numerous researchers' of industrial quarters and scientific research circle extensive concern, such as nucleocapsid alwaysThe AuAg nano particle of structure. If AuAg nano particle is formed to more complicated higher structure by self assembly,Such as thering is the one-dimensional chain nanostructured of coupling effect of surface plasma effect. Thus, between nano particle due toThe coupling effect of surface plasma effect produces local Electromagnetic enhancement, under the exciting of laser, thereby obtains organic moleculeSurface Raman enhancement signal. The one-dimensional nano structure of some simple Ag of currently reported confirmation or Au nano particle compositionCan significantly strengthen surface-enhanced raman scattering. Therefore the Raman matrix that, exploitation has this class formation is current materials chemistry area researchFocus. In fact, the self assembly of metal nanoparticle has become the focus in preparation and the application study of nanostructured at present,Especially one dimension Au-Ag core-shell nano structure, has very important researching value for research and the application of SPR effect.
Although there is at present the existing bibliographical information of nucleocapsid structure Au-Ag nano particle, but one-dimensional chain Au-Ag up to nowThe preparation of core-shell nano structure remains a difficult problem, not yet has at present bibliographical information, has also greatly limited one-dimensional nano structureResearch.
Summary of the invention
The object of this invention is to provide a kind of easy and simple to handle, environmental protection, and there is the one-dimensional chain of high surface Raman enhancement effectAu-Ag core-shell nano structure, self-assembly preparation method thereof and SERS application.
For achieving the above object, the technical solution used in the present invention is:
A self-assembly preparation method thereof for one-dimensional chain Au-Ag core-shell nano structure, step is as follows:
By the nanoparticulate dispersed of golden core silver shell in the alcohol-water mixture that contains inorganic salts, obtain A solution, leave standstill 1 minute-4 hours;
(2) get a certain amount of alkaline solution or contain alkali alcosol and join A solution, stir 5min-24 hour, centrifugalSeparate, obtain chain one-dimensional nucleocapsid nanostructured.
And described inorganic salts are NaCl, KCl, NaNO3、KNO3、NH4Cl、MgCl2、AlCl3A kind of or twoMixture more than kind.
And described alcoholic solution is ethanol or propyl alcohol or isopropyl alcohol.
And the described step (1) concentration of inorganic salts is 0.001～100mmol/L, preferably (0.1-30mmol/L), most preferably(1-15mmol/L). In alcohol-water mixture, the volume ratio of water and alcohol is 0.001～100, preferably (0.1-50), most preferably (1-25).
And described alkaline solution is ammoniacal liquor or the NaOH aqueous solution or the KOH aqueous solution, or the alcohol of ammoniacal liquor is moltenThe alcoholic solution of liquid or NaOH, in the alcoholic solution of described ammoniacal liquor or NaOH alcoholic solution, the volume ratio of water and alcohol is0.01～100, preferably (0.1-50), most preferably (1-30).
And the volume ratio of described alkaline solution and A solution is 0.01～100, preferably (0.05-20), most preferably (0.1-15).
And the preparation method of the nano particle of described golden core silver shell is:
(1) under the condition stirring, the aqueous solution of certain density natrium citricum is joined in aqueous solution of chloraurate, reaction is certainTime, obtains nano particle, and the mol ratio of natrium citricum and gold chloride is 10:1-0.5:1, and reaction temperature is 95-120 degree, anti-Between seasonable, be 3-60 minute, then naturally cool to room temperature, obtain the colloidal solution of gold nano grain;
(2) the colloidal solution of getting a certain amount of gold nano grain is dispersed in the aqueous solution of silver nitrate and natrium citricum, adds a certain amount ofThe reducing agent aqueous solution, reaction 5-120 minute, obtains the nanoparticles solution of golden core silver shell.
And described reducing agent is ascorbic acid or sodium borohydride or hydrazine hydrate, concentration is 1-100mmol/L, preferably (2-50Mmol/L), most preferably (2-20mmol/L).
And the particle diameter of described golden core is 5-100 nanometer.
And described silver-colored shell thickness is 0.5-50 nanometer.
The one-dimensional chain Au-Ag core-shell nano structure obtaining is utilized to Raman beacon molecule 1, and it is multiple that 4-dimercaptobenzene carries out functionalizationClose, get the aqueous solution 100uL of one-dimensional chain core-shell nano structure, add Isosorbide-5-Nitrae-dimercaptobenzene of the 100umol/L of 10uLReactant aqueous solution 2-10h, centrifugation, precipitation is the one-dimensional chain core-shell nano structure of Raman molecular functionalization, 4 DEG C of preservations,Stand-by.
The invention provides a kind of simple and effective self-assembly system, in this system, pass through to regulate repulsive force and attraction between particleReach a balance, AuAg Core-shell Structure Nanoparticles is assembled into chain one-dimensional nano structure, this structure has very highSurface Raman enhancement effect. The method is without very granular size and the pattern of homogeneous, and can assemble larger nanometerGrain, has realized the one dimension assembling with Core-shell Structure Nanoparticles, and Au core is big or small and Ag shell thickness easily regulates, stepRapid simple, with low cost, packaging efficiency is high, environmental protection, is easy to separation, functionalization and application.
One-dimensional chain AuAg core-shell nano structure has adjustable Au core and Ag shell knot as a kind of novel nano-materialStructure, both all can demonstrate good SPR effect, by forming chain structure, can between particle, form " focus " (hotSpot) region is the desirable matrix of SERS. The Au nuclear particle of different sizes and different Ag shell thicknesses pairThe effect of surface Raman enhancement is also by difference.
Advantage of the present invention and good effect:
1. the present invention utilizes inorganic salts and alkaline solution, the balance of adjusting between intergranular repulsion and gravitation, and not only cost is low, formerMaterial is easy to get, and easy operating, is beneficial to repetition and environmental protection.
2. the present invention utilizes water to prepare the metal nanoparticle of nucleocapsid structure, nothing as reducing agent as solvent, natrium citricumNeed special installation, process repeatability is high and be beneficial to amplification, easily realizes extensive preparation.
3. assembling process of the present invention is to the not restriction of metallic particles size, and the size of metal nanoparticle can be appointed between 5-100nmMeaning is selected, even if granular size and pattern are inhomogeneous, still can assemble, and obtains one-dimensional nano structure, and the method hasThe advantages such as applied widely, packaging efficiency is high, and built-up time is short.
4. what the present invention's assembling obtained has nucleocapsid structure one-dimensional nano structure, and stable in properties is easy to separate and functionalization, is convenient toApplication.
5. what the present invention's assembling obtained has nucleocapsid structure one-dimensional nano structure because the coupling of surface plasma effect can produceHotspot in a large number " ", therefore there is very high surface Raman enhancement effect.
6, the present invention is for the self assembly of AuAg nano particle with nucleocapsid structure, and not only efficiency is high, and process is simple,Au nuclear particle size and Ag shell thickness easily regulate and control, and required solvent environmental protection is nontoxic, and product is highly stable, obtainsOne-dimentional structure surface Raman enhancement successful, is easy to application. The present invention assembling obtain one-dimensional nano structure be expected to photocatalysis,The fields such as photoelectric conversion, biological thermotherapy, biology sensor, surface Raman enhancement spectrum, nano-device obtain large-scale application.
Brief description of the drawings
Fig. 1 is the solution colour comparison diagram before and after the assembling of AuAg nano particle;
Fig. 2 is the ultraviolet-visible light spectrogram of chain one dimension AuAg nanostructured;
Fig. 3 is that chain one dimension AuAg nanostructured is dispersed in the transmission electron microscope photo in ethanolic solution;
Fig. 4 is the Raman spectrum before and after the assembling of chain one dimension AuAg nanostructured;
Detailed description of the invention
Below in conjunction with accompanying drawing and by specific embodiment, the invention will be further described, and following examples are descriptive, noBe determinate, can not limit protection scope of the present invention with this.
Embodiment 1
1) get 50mL deionized water and join in there-necked flask, then add the HAuCl of 2mL left and right4(concentration is 25mM)Solution, stirs, and is heated to 100 degree left and right, refluxes, and then adds 5mL sodium citrate solution (concentration is 38.8mM), anti-Answer 10min left and right, obtain the colloidal solution of Au;
2) get the Au colloidal solution about 5mL, be dispersed in silver nitrate and sodium citrate aqueous solution (concentration is 38.8mM),Then add ascorbic acid solution (concentration is 10mM), reaction 30min left and right, the colloid that obtains AuAg nano particle is moltenLiquid, for subsequent use;
3) get the colloidal solution of AuAg nano particle of about 2mL centrifugal, be precipitated, be dispersed in the NaCl of 5mMIn solution;
4) in above-mentioned solution, add ethanol, the mixed solution that the volume ratio of ethanol/water is 5:1, leaves standstill 60min, then addsThe ethanolic solution of 0.5mLNaOH, stirs and obtains chain one dimension AuAg nanostructured (Fig. 1);
5) centrifugation obtains product, adds the NaOH solution of Isosorbide-5-Nitrae-dimercaptobenzene, stirs 2-6 hour, then centrifugal, waterWash 2-3 time, product is dispersed in the aqueous solution, to be measured.
In Fig. 1, left side yellow solution is AuAg nanoparticles solution, and Au core size is 13 nanometers, and Ag shell thickness is 5-10Nanometer; The right pale pink solution is the solution of assembling the one-dimensional chain nucleocapsid AuAg nanostructured obtaining;
Ultraviolet-visible collection of illustrative plates (Fig. 2) confirms that this one-dimentional structure has two obvious SPR absworption peaks, is positioned at 680nm left and rightAbsworption peak be major axis plasma coupling peak, prove the formation of chain one-dimentional structure, and absolutely prove that most of particle all assemblesFor one-dimensional nano structure, and transmission electron microscope picture (Fig. 3) further proves to obtain as having one-dimensional nucleocapsid AuAg nanostructured,
The Raman spectrum for one-dimensional nucleocapsid AuAg after assembling above in Fig. 4, below be single AuAg nano particleRaman spectrum, from Fig. 4 can prove to assemble, Raman signal been significantly enhanced.
Embodiment 2: as different from Example 1, in step (4), the volume ratio of ethanol/water is 100:1.
Embodiment 3: as different from Example 1, in step (4), the volume ratio of ethanol/water is 10:1.
Embodiment 4: as different from Example 1, in step (4), the volume ratio of ethanol/water is 0.05:1.
Embodiment 5: as different from Example 1, in step (4), the volume ratio of ethanol/water is 0.5:1.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art,Not departing under the prerequisite of inventive concept, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (10)
1. a self-assembly preparation method thereof for one-dimensional chain Au-Ag core-shell nano structure, is characterized in that: step is as follows:
By the nanoparticulate dispersed of golden core silver shell in the alcohol-water mixture that contains inorganic salts, obtain A solution, leave standstill;
(2) get a certain amount of alkaline solution or contain alkali alcosol and join A solution, stir, centrifugation, obtains chainShape one-dimensional nucleocapsid nanostructured.
2. preparation method according to claim 1, is characterized in that: described inorganic salts are NaCl, KCl, NaNO3、KNO3、NH4Cl、MgCl2、AlCl3One or more mixture.
3. preparation method according to claim 1, is characterized in that: described alcoholic solution is ethanol or propyl alcohol or isopropyl alcohol.
4. preparation method according to claim 1, is characterized in that: the described step (1) concentration of inorganic salts is 0.001～100Mmol/L, in alcohol-water mixture, the volume ratio of water and alcohol is 0.001～100.
5. preparation method according to claim 1, is characterized in that: described alkaline solution is ammoniacal liquor or NaOH waterSolution or the KOH aqueous solution, or the alcoholic solution of ammoniacal liquor or the alcoholic solution of NaOH, the alcoholic solution of described ammoniacal liquor orIn NaOH alcoholic solution, the volume ratio of water and alcohol is 0.01～100, and the volume ratio of this alkaline solution and A solution is 0.01～100.
6. preparation method according to claim 1, is characterized in that: the preparation method of the nano particle of described golden core silver shellFor:
(1) under the condition stirring, the aqueous solution of certain density natrium citricum is joined in aqueous solution of chloraurate, reaction is certainTime, obtains nano particle, and the mol ratio of natrium citricum and gold chloride is 10:1-0.5:1, and reaction temperature is 95-120 degree, anti-Between seasonable, be 3-60 minute, then naturally cool to room temperature, obtain the colloidal solution of gold nano grain;
(2) the colloidal solution of getting a certain amount of gold nano grain is dispersed in the aqueous solution of silver nitrate and natrium citricum, adds a certain amount ofThe reducing agent aqueous solution, reaction 5-120 minute, obtains the nanoparticles solution of golden core silver shell.
7. preparation method according to claim 6, is characterized in that: described reducing agent is ascorbic acid or sodium borohydrideOr hydrazine hydrate, concentration is 1-100mmol/L.
8. according to the preparation method described in any claim of claim 1 or 6, it is characterized in that: the particle diameter of described golden coreFor 5-100 nanometer, described silver-colored shell thickness is 0.5-50 nanometer.
9. the one-dimensional chain Au-Ag core-shell nano structure that method makes according to claim 1.
10. an one-dimensional chain Au-Ag core-shell nano structure claimed in claim 9 application in SERS.
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Cited By (10)
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| CN106483116A (en) * | 2016-09-27 | 2017-03-08 | 东南大学 | A kind of preparation method of the hollow-core fiber SERS probe based on two kinds of Nano silver grain self assemblies |
| CN107225235A (en) * | 2017-06-02 | 2017-10-03 | 宁波大学 | A kind of gold/silver/polymer/silver core-shell nano mushroom material with SERS activity and its preparation method and application |
| CN107802843A (en) * | 2017-12-07 | 2018-03-16 | 天津理工大学 | A kind of preparation method and applications of metal nano chain |
| CN108088994A (en) * | 2017-12-15 | 2018-05-29 | 南京医科大学第二附属医院 | A kind of hollow core shell nanoparticles and preparation method, test strips and test method |
| CN108247041A (en) * | 2018-01-23 | 2018-07-06 | 中国科学院长春应用化学研究所 | A kind of Au@Ag core-shell structured nanomaterials, preparation method and the method for reducing cytotoxicity |
| CN108580919A (en) * | 2018-03-08 | 2018-09-28 | 温州大学 | Preparation method, surface-enhanced Raman detection probe and its application of the mesoporous gold nano structural material of galactic nucleus |
| CN109202064A (en) * | 2018-10-31 | 2019-01-15 | 大连民族大学 | A kind of short-cut method characterizing gold nanocrystals lattice structure and purity |
| CN111590085A (en) * | 2020-06-01 | 2020-08-28 | 中国农业科学院农业质量标准与检测技术研究所 | Au-Ag nano-chain composite SERS substrate and preparation method and application thereof |
| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
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| CN106483116A (en) * | 2016-09-27 | 2017-03-08 | 东南大学 | A kind of preparation method of the hollow-core fiber SERS probe based on two kinds of Nano silver grain self assemblies |
| CN106483116B (en) * | 2016-09-27 | 2019-12-06 | 东南大学 | Preparation method of hollow-core optical fiber SERS probe based on self-assembly of two silver nanoparticles |
| CN107225235B (en) * | 2017-06-02 | 2019-03-12 | 宁波大学 | One kind having the active gold/silver of SERS/polymer/silver core-shell nano mushroom material and its preparation method and application |
| CN107225235A (en) * | 2017-06-02 | 2017-10-03 | 宁波大学 | A kind of gold/silver/polymer/silver core-shell nano mushroom material with SERS activity and its preparation method and application |
| CN107802843A (en) * | 2017-12-07 | 2018-03-16 | 天津理工大学 | A kind of preparation method and applications of metal nano chain |
| CN108088994A (en) * | 2017-12-15 | 2018-05-29 | 南京医科大学第二附属医院 | A kind of hollow core shell nanoparticles and preparation method, test strips and test method |
| CN108088994B (en) * | 2017-12-15 | 2022-04-19 | 南京医科大学第二附属医院 | Hollow core-shell nanoparticle, preparation method, test strip and test method |
| CN108247041A (en) * | 2018-01-23 | 2018-07-06 | 中国科学院长春应用化学研究所 | A kind of Au@Ag core-shell structured nanomaterials, preparation method and the method for reducing cytotoxicity |
| 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 |
| CN108580919A (en) * | 2018-03-08 | 2018-09-28 | 温州大学 | Preparation method, surface-enhanced Raman detection probe and its application of the mesoporous gold nano structural material of galactic nucleus |
| CN109202064A (en) * | 2018-10-31 | 2019-01-15 | 大连民族大学 | A kind of short-cut method characterizing gold nanocrystals lattice structure and purity |
| CN111590085A (en) * | 2020-06-01 | 2020-08-28 | 中国农业科学院农业质量标准与检测技术研究所 | Au-Ag nano-chain composite SERS substrate and preparation method and application thereof |
| CN111590085B (en) * | 2020-06-01 | 2022-11-22 | 中国农业科学院农业质量标准与检测技术研究所 | Au-Ag nano-chain composite SERS substrate and preparation method and application thereof |
| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
| CN114082973A (en) * | 2021-10-22 | 2022-02-25 | 北京航空航天大学 | Ag shell thickness control method of Au @ Ag nano core-shell material and application thereof |
| CN114082973B (en) * | 2021-10-22 | 2023-02-28 | 北京航空航天大学 | Ag shell thickness control method of Au @ Ag nano core-shell material and application thereof |
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