CN102103086B - Method for detecting single molecule of single silicon nanowire in real time based on surface enhanced Raman effect - Google Patents
Method for detecting single molecule of single silicon nanowire in real time based on surface enhanced Raman effect Download PDFInfo
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Abstract
本发明公开了一种基于表面增强拉曼效应的单根硅纳米线实时检测单分子的方法。该方法包括如下步骤：1)将除去表面氧化层的硅纳米线分散在CTAB的水溶液中，在搅拌条件下，向所述硅纳米线的分散液中加入含有金属银离子的溶液，反应一段时间后将产物离心，收集沉淀，将得到的表面负载银颗粒的硅纳米线分散于乙醇中；2)将硅纳米线的乙醇分散液滴于带有凹槽的载玻片的凹槽处，待乙醇挥发后，在凹槽处加入待测分子的水溶液，并用盖玻片将其密封，选用一定波长的激光对凹槽处的硅纳米线进行照射，并进行拉曼信号的收集，即实现对单分子的实时检测。该方法简单快捷，反应条件温和，制备的材料性能稳定，SERS响应很好，且实现了溶液体系中单个分子的检测，为研究溶液体系中单个分子的反应提供了良好的平台。The invention discloses a method for real-time detection of a single molecule by a single silicon nanowire based on a surface-enhanced Raman effect. The method comprises the following steps: 1) dispersing the silicon nanowires from which the surface oxide layer has been removed in an aqueous solution of CTAB, adding a solution containing metal silver ions to the dispersion of the silicon nanowires under stirring conditions, and reacting for a period of time Finally, the product is centrifuged, the precipitate is collected, and the obtained silicon nanowires loaded with silver particles on the surface are dispersed in ethanol; 2) the ethanol dispersion of the silicon nanowires is dropped on the grooves of the glass slide with grooves, and wait for After the ethanol volatilizes, add the aqueous solution of the molecule to be measured in the groove, and seal it with a cover glass, select a laser with a certain wavelength to irradiate the silicon nanowires in the groove, and collect Raman signals, that is, to realize the detection of Real-time detection of single molecules. The method is simple and fast, the reaction conditions are mild, the prepared material has stable performance, and the SERS response is very good, and the detection of a single molecule in a solution system is realized, which provides a good platform for studying the reaction of a single molecule in a solution system.
Description
Technical field
The present invention relates to a kind of single silicon nanowires and detect monomolecular method in real time based on surface-enhanced Raman effects.
Background technology
(surface enhanced raman scattering SERS) combines the sensitivity of individual molecule fingerprint recognition, and becomes the individual molecule dynamics of research surface adsorption even the strong instrument of the unimolecular reaction in the solution unimolecule SERS.Yet, be applied to Single Molecule Detection in the reality, need a kind of simple and convenient preparation to have the method that unimolecule strengthens the detection substrate of ability, detection also requires substrate to have certain stability under the solution situation.Up to the present, think in theory that the silver-colored agglomeration of particles body of size in the 30-100nm scope combines spacing under the situation of 1-9nm scope, to can be used as " focus " that SERS detects between particle.People generally adopt silver nano-grain that people such as nineteen eighty-two Lee-Misel utilizes citric acid reduction preparation as detecting substrate; Yet the silver nano-grain of this gathering only has the situation less than 1% can detect effective SERS activity; Furtherly; When in solution, detecting, owing to the Brownian movement of silver colloidal particles with and in detection volume change of configuration be difficult to obtain the real signal of unimolecule.Thereby, develop a kind of simple, reliable, stable substrate that can be used for detecting in the solution of preparation and become most important with unimolecule enhancing ability.
Silicon nanowires most possibly combines and widespread adoption with existing silicon-based semiconductor technology as a kind of integration module material.Since characteristics such as himself distinctive optics, electrical properties and high surface, silicon nanowires aspect various nano-devices such as nano-sensor, field emission display by broad research.Rarely have report with silicon nanowires as the document that SERS detects substrate, and reach document that single molecules level detects report not especially.
Summary of the invention
The purpose of this invention is to provide a kind of single silicon nanowires and detect monomolecular method in real time based on surface-enhanced Raman effects.
Single silicon nanowires based on surface-enhanced Raman effects provided by the present invention detects monomolecular method in real time, comprises the steps:
1) silicon nanowires that will remove surface oxide layer is dispersed in the WS of cetyl trimethyl ammonium bromide (CTAB), obtains the dispersion liquid of silicon nanowires; Under stirring condition; In the dispersion liquid of said silicon nanowires, add the solution that contains silver ion and react, reaction is carried out centrifugal to reactant liquor after finishing; Collecting precipitation; Promptly obtain the silicon nanowires of area load silver particle, the silicon nanowires with said area load silver particle washes with deionized water, absolute ethyl alcohol successively then, and the silicon nanowires with said area load silver particle after the flushing is scattered in the ethanol;
2) alcohol dispersion liquid of using internal diameter to draw the silicon nanowires of a small amount of above-mentioned area load silver particle as the kapillary of 0.9-1.1mm is dripped in the groove of the microslide that has groove; After treating the ethanol volatilization; Add the WS of testing molecule at groove, and with cover glass it is sealed, the laser of selecting certain wavelength for use shines the silicon nanowires of groove; And carry out the collection of Raman signal, promptly realize monomolecular real-time detection.
Wherein, the concentration of cetyl trimethyl ammonium bromide is 0.5-1.5mmol/L in the WS of cetyl trimethyl ammonium bromide described in the step 1), is preferably 1mmol/L; The content of silicon nanowires is 0.2-0.5mg/ml in the said silicon nanowires dispersion liquid.Said argentiferous ion solution can be liquor argenti nitratis ophthalmicus or silver acetate solution etc., and when selecting liquor argenti nitratis ophthalmicus for use, silver nitrate concentration is 1-1.5mmol/L in the said liquor argenti nitratis ophthalmicus, is preferably 1mmol/L.
The temperature of reaction of the said reaction of step 1) is 15 ℃-25 ℃; Reaction time is 1min-5min, is preferably 2-3min; In the reaction system of said reaction, the mol ratio of CTAB and silver nitrate is 0.15-0.35.
The diameter of removing the silicon nanowires of surface oxide layer described in the present invention is more than or equal to 100nm, is preferably 100nm-500nm.
The above-mentioned silicon nanowires of removing surface oxide layer prepares according to following method:
1) make catalyzer with glass putty, the surface coverage that thermal evaporation SiO powder preparation obtains has the silicon nanowires of oxide layer;
2) there is the silicon nanowires of oxide layer to be immersed in the hydrofluoric acid aqueous solution that mass concentration is 5%-15% said surface coverage; Ultrasonic dispersion with solution centrifugal, is isolated deposition behind the placement 10-30min; And use deionized water rinsing, the silicon nanowires of the surface oxide layer that is removed.
When the WS of testing molecule step 2 of the present invention) was rhodamine (R6G) WS, the concentration of rhodamine was 5nmol/L in the said rhodamine WS, to guarantee in the detection volume 1 molecule being arranged at most.At this moment, the optical maser wavelength of being selected for use is 532nm, and laser power is 0.05mW, and the laser focusing spot diameter is 0.5 μ m.
The present invention utilizes the surface of silicon nanowires after the hydrofluoric acid treatment to have reductibility, can the solution metal ion is reduced into simple substance and be deposited on surface of silicon nanowires.Preparation method's simple and fast of the present invention, equipment is cheap, at room temperature can carry out, and can prepare in a large number, and the material of preparation can satisfy needed particle size of unimolecule SERS " focus " and the spacing of calculating in theory.Evidence detects substrate with the silicon nanowires for preparing among the present invention as SERS, has realized that single molecules level detects in the solution.
Description of drawings
Fig. 1 has the SEM and the TEM photo of the silicon nanowires of silver nano-grain for the area load of embodiment 1 preparation.
Fig. 2 is the reduced graph of Raman detection architecture among the embodiment 2.
Fig. 3 is the optical photograph of single silicon nanowires among the embodiment 2.
Fig. 4 is the mean value of the raman spectral signal of different points of irradiation among the embodiment 2.
Fig. 5 is the Raman spectrum wave pattern in time of single point of irradiation among the embodiment 3.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment the present invention is done further detailed description.But protection scope of the present invention is not limited to the scope that embodiment explains.
Experimental technique described in the following embodiment like no specified otherwise, is conventional method; Said reagent and material like no specified otherwise, all can obtain from commercial sources.
Employed silver nitrate among the embodiment, hydrofluorite (mass concentration is 40%) is all purchased the chemical reagents corporation in Beijing; CTAB (purity 99%) purchases the company in Alfa, and rhodamine 6G (AG) is purchased in lark prestige company, all is not for further processing before the use.Experimental technique described in the following embodiment like no specified otherwise, is conventional method; Said reagent and biomaterial like no specified otherwise, all can obtain from commercial sources.
The silicon nanowires of embodiment 1, the surperficial uniform load silver nano-grain of preparation
Employed silicon nanowires is to adopt existing method in the present embodiment: as catalyzer, thermal evaporation SiO powder preparation obtains with glass putty; Specific as follows: as to take by weighing 3.0gSiO powder and 0.5gSn powder, be placed in the porcelain boat and mix, porcelain boat is put in the high-temperature region of vacuum tube furnace, sealing vacuum tube furnace; Be pumped to pressure to 5 in the furnace chamber * 10
-2Behind the mbar, feed in combination gas to the stove of argon gas and hydrogen pressure behind 350mbar, the furnace high-temperature district be heated to 1360 ℃ with the speed of 40 ℃/min, be incubated 7-8h after, be cooled to room temperature.The silicon nanowires diameter of preparation is about the 100-500 nanometer, and the surface coats the oxide layer of one deck silicon.The ultrasonic dispersion in ethanolic solution earlier of the thick product of the silicon nanowires of Experiment Preparation could be used after the filtration.
Taking by weighing the above-mentioned silicon nanowires of about 2.5mg and be put in the plastic tube, is 5% hydrofluoric acid solution to wherein adding the 2-5ml massfraction, after the ultrasonic dispersion, leaves standstill and removes surface oxide layer in 20 minutes, centrifuging, the silicon nanowires of the surface oxide layer that is removed.
In the WS with the ultrasonic 5ml of the being dispersed in concentration of the silicon nanowires of the removing surface oxide layer CTAB that is 1mM, silicon nanowires can disperse therein preferably.Get this dispersion liquid 1ml, after stirring at ambient temperature, to wherein adding the AgNO that 3mL concentration is 1mM rapidly
3Solution, room temperature condition is reaction 3min down, with final solution centrifugal 2min under the 8000r/min rotating speed, product is separated from solution system after reaction finishes.Then product is used deionized water, absolute ethyl alcohol ultrasonic irrigation 3 times successively, each flushing back solution is centrifugal 5min under the 8000r/min rotating speed all, and the silicon nanowires with the area load silver particle for preparing is dispersed in the absolute ethyl alcohol for use at last.
The alcohol dispersion liquid of product is dropped on the silicon chip, treat after the ethanol evaporation that (SEM HitachiS-4300) observes its pattern down, and area load has the pattern of silicon nanowires of silver nano-grain shown in Fig. 1 a at ESEM.Right Fig. 1 a can know that a large amount of surface of silicon nanowires are coated with equally distributed silver nano-grain.The transmission electron microscope of this sample (TEM) photo can be known that by Fig. 1 b the mean grain size of silver nano-grain is about 34nm shown in Fig. 1 b, the spacing of adjacent particle is 1-7nm.
Embodiment 2, detect unimolecule in real time based on the single silicon nanowires of surface-enhanced Raman effects
The dispersant liquid drop of drawing the sample for preparing among a small amount of embodiment 1 with kapillary is having on the microslide of groove; After treating the ethanol volatilization; Silicon nanowires is adsorbed on glass surface, and to the WS of the R6G of groove Dropwise 5 nM, surperficial covered prevents solution evaporation then.Adopt renishaw confocal laser ramanspectroscopy to collect single silicon nanowires and detect monomolecular spectrum, the reduced graph of this detection architecture is as shown in Figure 2, and the optical photograph that detects single silicon nanowires is as shown in Figure 3.Selecting enlargement factor for use is that (numerical aperture NA=0.85, laser point diameter are 0.5 μ m, and the depth of field is 2 μ m for 100 times object lens; In detection volume, can not surpass 1 molecule through calculating), excitation wavelength is 532nm, the laser that power is about 50 μ W shines points different on the single silicon nanowires; Collect 30 spectrum, wherein each spectrum acquisition time is 10s, and cumulative frequency is 1; Get its mean value, Raman spectrum is as shown in Figure 4.Can know that by Fig. 4 sample has good unimolecule and strengthens ability.
Embodiment 3, detect unimolecule in real time based on the single silicon nanowires of surface-enhanced Raman effects
Method according to embodiment 2; Collect single silicon nanowires and in solution, detect monomolecular signal; Difference is in the present embodiment it is to choose same some employing continuous laser irradiation on the single silicon nanowires; Collect 100 spectrum, the spectrum time interval is 1s, and the variation diagram in time of the Raman spectrum that obtains is as shown in Figure 5.Can be known that by Fig. 5 the phenomenon that significantly flickers appears in spectrum in time, this is the peculiar phenomenon of unimolecule Raman spectrum, proves that further sample can realize in the solution system detecting in real time unimolecule.
Claims (8)
1. the single silicon nanowires based on surface-enhanced Raman effects detects monomolecular method in real time, comprises the steps:
1) silicon nanowires that will remove surface oxide layer is dispersed in the WS of cetyl trimethyl ammonium bromide, obtains the dispersion liquid of silicon nanowires; Under stirring condition; In the dispersion liquid of said silicon nanowires, add the solution that contains silver ion and react, reaction is carried out centrifugal to reactant liquor after finishing; Collecting precipitation; Promptly obtain the silicon nanowires of area load silver particle, the silicon nanowires with said area load silver particle washes with deionized water, absolute ethyl alcohol successively then, and the silicon nanowires with said area load silver particle after the flushing is scattered in the absolute ethyl alcohol for use;
2) alcohol dispersion liquid of the silicon nanowires of area load silver particle is dripped in the groove of the microslide that has groove; After treating the ethanol volatilization; Add certain density solution to be measured at groove, and with cover glass it is sealed, the laser of selecting certain wavelength for use shines the single silicon nanowires of groove; And carry out the collection of Raman signal, promptly realize monomolecular real-time detection;
The concentration of cetyl trimethyl ammonium bromide is 0.5-1.5mmol/L in the WS of cetyl trimethyl ammonium bromide described in the step 1); The content of silicon nanowires is 0.2-0.5mg/ml in the said silicon nanowires dispersion liquid;
The solution that contains silver ion described in the step 1) is liquor argenti nitratis ophthalmicus;
The concentration of silver nitrate is 1-1.5mmol/L in the said liquor argenti nitratis ophthalmicus;
The temperature of reaction of the said reaction of step 1) is 15 ℃-25 ℃; Reaction time is 1min-5min; In the reaction system of said reaction, the mol ratio of cetyl trimethyl ammonium bromide and silver nitrate is 0.15-0.35.
2. method according to claim 1 is characterized in that: the concentration of cetyl trimethyl ammonium bromide is 1mmol/L in the WS of cetyl trimethyl ammonium bromide described in the step 1).
3. method according to claim 1 is characterized in that: the concentration of silver nitrate is 1mmol/L in the said liquor argenti nitratis ophthalmicus.
4. method according to claim 1 is characterized in that: the said reaction time of step 1) is 2-3min.
5. according to arbitrary described method among the claim 1-4, it is characterized in that: the diameter of said silicon nanowires is 100-500nm.
6. method according to claim 5 is characterized in that: the said silicon nanowires of removing surface oxide layer prepares according to following method:
1) make catalyzer with glass putty, thermal evaporation SiO powder preparation obtains the silicon nanowires that surface coverage has oxide layer;
2) there is the silicon nanowires of oxide layer to be immersed in the hydrofluoric acid aqueous solution that mass concentration is 5%-15% said surface coverage; Ultrasonic dispersion with solution centrifugal, is isolated deposition behind the placement 10-30min; And use deionized water rinsing, the silicon nanowires of the surface oxide layer that is removed.
7. method according to claim 6 is characterized in that: said solution to be measured is the rhodamine 6G WS; The concentration of rhodamine 6G is 5nmol/L in the said rhodamine 6G WS.
8. method according to claim 7 is characterized in that: the optical maser wavelength of being selected for use is 532nm, and laser power is 0.05-0.5mW, and the laser focusing spot diameter is 0.5 μ m.
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| CN111129477B (en) * | 2019-12-10 | 2022-09-20 | 同济大学 | Method for preparing super-assembled lithium storage material with silicon nano dots embedded in carbon skeleton |
| CN111036930B (en) * | 2019-12-25 | 2022-06-24 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of silver nanowire block for SERS detection |
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