CN103264166A - Preparation method of self-assembled silver ball SERS (Surface Enhanced Raman Scattering) base with controllable silver nano sheet thickness - Google Patents
Preparation method of self-assembled silver ball SERS (Surface Enhanced Raman Scattering) base with controllable silver nano sheet thickness Download PDFInfo
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Abstract
The invention belongs to the field of a nanometer material science and a laser Raman detection technology, and particularly relates to a preparation method of a self-assembled silver ball SERS (Surface Enhanced Raman Scattering) base with a controllable silver nano sheet thickness. The method takes silver nitrate as a silver source and L-ascorbic acid as a reducing agent, and comprises the following steps of: adding one organic acid with controlled amount to react in an ice bath (2-5 DEG C) for 2-15 minutes to obtain a silver micro-ball which is formed by self-assembling silver nano sheets with the controllable thickness in a range of 20-110nm. The silver micro-ball formed by self-assembling the silver nano sheets, which is prepared by the method, not only has the characteristic of high specific surface area of a common nano material, but also has the characteristics of controllable thickness of the surface silver nano sheets and serial and comparable surface roughness; and the silver micro-ball formed by self-assembling the silver nano sheets is a surface enhanced Raman base with the very good activity and is hopeful to be applied to aspects of surface enhanced fluorescence and photocatalysis.
Description
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Technical field
The invention belongs to nanometer material science and LR laser raman detection technique field, be specifically related to a kind of preparation of surface-enhanced Raman (SERS) substrate of self assembly silver microballoon of surperficial Nano silver piece controllable thickness.
Background technology
SERS (SERS) is a kind of microanalysis technology with high sensitivity, be characterized in that sample does not need special preparation when the detection molecules structure, and do not need directly to contact with sample, pollution-free nothing is destructive, and with respect to infrared spectrum, Raman spectrum has more been avoided the influence of moisture to detecting.The key of obtaining high-quality SERS signal is that the surface strengthens substrate.It is nanostructured that the surface strengthens substrate common.Particle size, shape and arrangement and the SERS activity of surface enhancing substrate are closely related.In order to improve the SERS activity, the researcher is exploring the preparation method of the higher substrate of SERS activity always from theoretical and experiment two aspects both at home and abroad.
At present, the pattern of the SERS substrate that people obtain is varied, and sample or substrate surface by specially treated also can obtain good SERS signal, but roughness is uncontrollable or do not have serial comparativity, and the preparation method complexity is expensive etc.Document 1(J. Mater. Chem., 2011,21,2495-2501) report is reducing agent with the ascorbic acid, the reduction liquor argenti nitratis ophthalmicus, by adding three kinds of different acid (citric acid, mandelic acid, p-methyl benzenesulfonic acid), the SERS substrate that has prepared four kinds of surface topographies with liquid phase reduction, these four kinds of substrate patterns have nothing in common with each other, though roughness there are differences, are not patterns of the same race, there is not comparativity, can not be in order to study the pattern roughness to the influence of SERS.Document 2(Nano Research, 2013, Volume 6, and Issue 3, pp159-166) report, send out with template to have prepared silver-colored centrum array, not that self assembly forms, sample only is two-dimensional structure, and preparation method's complexity.Patent 200810106420.2 discloses the preparation method of the micron-grade superfine silver powder of the preparation pinecone, flower or dendritic morphology, although pattern is various, is not the controllable growth of same type pattern, and the ping-pong ball volume is bigger in the patent, and is not used as the SERS substrate.
Said method or can not provide the substrate sample of comparable a series of system research SERS, perhaps non-self assembly, just two-dimensional structure, and preparation method's complexity.The advantage of SERS test is the measurement sensitivity height, convenient and swift, and the complexity of substrate preparation, SERS will be used to be limited to greatly, therefore, prepare SERS series substrate quick and pollution-free and that can be used for system research and will make the application of SERS more extensive fast, also provide experiment basis to the research of SERS mechanism.
Summary of the invention
Guardian technique problem to be solved by this invention is that to prepare a series of surface roughnesses by the method for simple and fast controlled, and the comparable a series of SERS substrates of pattern, is used for the measurement of SERS and the research of SERS mechanism.The present invention uses conventional liquid-phase reduction method, by adding an amount of organic acid as modifier, makes the controllable thickness of the silver-colored microsphere surface nanometer sheet that Nano silver piece is self-assembled into, thereby makes surface roughness controlled, obtains the comparable SERS substrate of series.
Technical scheme of the present invention is: the preparation method of the self assembly ping-pong ball SERS substrate of Nano silver piece controllable thickness is characterized in that concrete steps are as follows:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and organic acid is modifier, above-mentioned raw materials is added make solution in the deionized water respectively, and is standby; Wherein, described silver nitrate: L-ascorbic acid: the organic acid mol ratio is 1:1:0.0025-0.025;
(2) liquor argenti nitratis ophthalmicus that step (1) is prepared is under stirring condition, join in the water that in ice bath, cools off, prepare organic acid soln with micropipettor step (1), join in the described liquor argenti nitratis ophthalmicus, stir, obtain mixed solution, the L-ascorbic acid solution that step (1) is prepared once adds in the described mixed solution rapidly again, in ice bath, reacted 2-15 minute under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of the Nano silver piece controllable thickness of 20 nm-110 nm with washed with de-ionized water.
Further, described organic acid is mandelic acid, citric acid, a kind of in the p-methyl benzenesulfonic acid.
The advantage that the present invention compared with prior art has is:
(1) silver nitrate of the present invention: L-ascorbic acid ratio is the 1:1 mol ratio, and reaction condition is simple, and is easy to operate, and the reaction time is short, and only by adding a kind of acid, need not to add other acid or pure modifications, just can control the thickness of ping-pong ball nano surface sheet.
(2) Nano silver piece is self-assembled into ping-pong ball, and surface topography becomes series to have comparativity, can do the research of series.
Description of drawings
SEM * 5000 shape appearance figures of the about 26nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 1 makes for example one of the present invention.
SEM * 100000 shape appearance figures of the about 26nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 2 makes for example one of the present invention.
SEM * 5000 shape appearance figures of the about 41nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 3 makes for example two of the present invention.
SEM * 100000 shape appearance figures of the about 41nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 4 makes for example two of the present invention.
SEM * 5000 shape appearance figures of the about 57nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 5 makes for example three of the present invention.
SEM * 100000 shape appearance figures of the about 57nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 6 makes for example three of the present invention.
SEM * 5000 shape appearance figures of the about 110nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 7 makes for example four of the present invention.
SEM * 100000 shape appearance figures of the about 110nm Nano silver piece of the thickness self assembly silver microballoon that Fig. 8 makes for example four of the present invention.
Fig. 9 for the surperficial controlled self assembly ping-pong ball surface-enhanced Raman substrate of the present invention preparation (Rhodamine B, concentration is 10 with rhodamine B
-6Mol/L) be surface-enhanced Raman (SERS) collection of illustrative plates of molecular detection.
Figure 10 is X-ray diffraction (XRD) collection of illustrative plates of the self assembly ping-pong ball SERS substrate of the Nano silver piece controllable thickness of the present invention's preparation.
Figure 11 reduces changing trend diagram along with adding acid with the increase of silver nitrate mol ratio for self assembly ping-pong ball surface Nano silver piece thickness.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further.
Embodiment one:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and citric acid is that modifier is made the aqueous solution respectively, wherein, silver nitrate: L-ascorbic acid ratio is the 1:1 mol ratio, organic acid: silver nitrate is the 0.0025:1 mol ratio, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 2 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 26 nm with washed with de-ionized water.This material X-ray diffraction (XRD) collection of illustrative plates is seen accompanying drawing 10.As seen from the figure, the product purity height does not have other material dephasigns and exists in the XRD collection of illustrative plates.
Embodiment two:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and citric acid is that modifier is made the aqueous solution respectively, wherein, silver nitrate: L-ascorbic acid ratio is the 1:1 mol ratio, organic acid: silver nitrate is the 0.0075:1 mol ratio, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 7 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 41 nm with washed with de-ionized water.Its XRD result is identical with embodiment one.
Embodiment three:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and citric acid is that modifier is made the aqueous solution respectively, wherein, silver nitrate: L-ascorbic acid ratio is the 1:1 mol ratio, organic acid: silver nitrate is the 0.01-0.025:1 mol ratio, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 10 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 57nm with washed with de-ionized water.Its XRD result is identical with embodiment one.
Embodiment four:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and citric acid is that modifier is made the aqueous solution respectively, and wherein, silver nitrate: L-ascorbic acid ratio is the 1:1 mol ratio, organic acid: silver nitrate is the 0.015:1 mol ratio, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 15 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 110nm with washed with de-ionized water.Its XRD result is identical with embodiment one.
Embodiment five:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and mandelic acid is that modifier is made the aqueous solution respectively, wherein, silver nitrate: L-ascorbic acid ratio is the 1:1 mol ratio, organic acid: silver nitrate is the 0.025:1 mol ratio, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 5 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 26 nm with washed with de-ionized water.
Embodiment six:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and p-methyl benzenesulfonic acid is that modifier is made the aqueous solution respectively, wherein, silver nitrate: the mol ratio of L-ascorbic acid is 1:1, organic acid: the mol ratio of silver nitrate is 0.02:1, and above-mentioned raw materials is made the aqueous solution;
(2) with liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, get micro-organic acid soln with micropipettor, join in the liquor argenti nitratis ophthalmicus, stir, once add in the mixed solution rapidly the L-ascorbic acid solution again, in ice bath, reacted 12 minutes under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of 57nm with washed with de-ionized water.
Claims (2)
1. the preparation method of the self assembly ping-pong ball SERS substrate of Nano silver piece controllable thickness is characterized in that concrete steps are as follows:
(1) be silver-colored source with silver nitrate, the L-ascorbic acid is reducing agent, and organic acid is modifier, above-mentioned raw materials is added be prepared into solution in the deionized water respectively, and is standby; Wherein, described silver nitrate: L-ascorbic acid: the organic acid mol ratio is 1:1:0.0025-0.025:1;
(2) with above-mentioned liquor argenti nitratis ophthalmicus under stirring condition, join in the water that in ice bath, cools off, join in the described liquor argenti nitratis ophthalmicus with the organic acid soln of micropipettor with step (1) preparation, stir, obtain mixed solution, just the L-ascorbic acid solution of step (1) preparation once adds in the described mixed solution rapidly again, in ice bath, reacted 2-15 minute under the stirring condition, collecting precipitation, all over reaching 7 to the pH value, the thickness that namely obtains surperficial Nano silver piece is the self assembly ping-pong ball SERS substrate of the Nano silver piece controllable thickness of 20 nm-110 nm with the washed with de-ionized water number.
2. the preparation method of the self assembly ping-pong ball SERS substrate of Nano silver piece controllable thickness according to claim 1 is characterized in that described organic acid is mandelic acid, a kind of in citric acid or the p-methyl benzenesulfonic acid.
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Cited By (6)
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|---|---|---|---|---|
| CN106475022A (en) * | 2015-09-02 | 2017-03-08 | 南京理工大学 | A kind of active antibacterial microballoon and preparation method thereof |
| CN107377990A (en) * | 2017-06-30 | 2017-11-24 | 北京师范大学 | A kind of preparation method of trough of belt Nano silver piece package assembly |
| CN107589103A (en) * | 2017-08-05 | 2018-01-16 | 北京师范大学 | A step solution assemble method of the silver nano flower-like on fiber |
| CN107755685A (en) * | 2017-10-11 | 2018-03-06 | 中国科学院合肥物质科学研究院 | Three-dimensional silver micro-nano-sphere and preparation method thereof |
| CN109270046A (en) * | 2018-08-30 | 2019-01-25 | 东南大学 | A kind of construction method of the controllable micro-nano array based on gold and silver nano brick and its application |
| CN111218676A (en) * | 2020-01-09 | 2020-06-02 | 吉林师范大学 | Preparation method and application of Ag nano sheet SERS substrate assembled on aluminum foil |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106475022A (en) * | 2015-09-02 | 2017-03-08 | 南京理工大学 | A kind of active antibacterial microballoon and preparation method thereof |
| CN106475022B (en) * | 2015-09-02 | 2019-09-27 | 南京理工大学 | A kind of active antibacterial microballoon and preparation method thereof |
| CN107377990A (en) * | 2017-06-30 | 2017-11-24 | 北京师范大学 | A kind of preparation method of trough of belt Nano silver piece package assembly |
| CN107377990B (en) * | 2017-06-30 | 2019-06-04 | 北京师范大学 | A kind of preparation method of trough of belt Nano silver piece package assembly |
| CN107589103A (en) * | 2017-08-05 | 2018-01-16 | 北京师范大学 | A step solution assemble method of the silver nano flower-like on fiber |
| CN107755685A (en) * | 2017-10-11 | 2018-03-06 | 中国科学院合肥物质科学研究院 | Three-dimensional silver micro-nano-sphere and preparation method thereof |
| CN109270046A (en) * | 2018-08-30 | 2019-01-25 | 东南大学 | A kind of construction method of the controllable micro-nano array based on gold and silver nano brick and its application |
| CN111218676A (en) * | 2020-01-09 | 2020-06-02 | 吉林师范大学 | Preparation method and application of Ag nano sheet SERS substrate assembled on aluminum foil |
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Application publication date: 20130828 |