CN103569961A - Preparation method for silver nanoparticle chain under inducement of silicon nanowire - Google Patents
Preparation method for silver nanoparticle chain under inducement of silicon nanowire Download PDFInfo
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- CN103569961A CN103569961A CN201310589606.9A CN201310589606A CN103569961A CN 103569961 A CN103569961 A CN 103569961A CN 201310589606 A CN201310589606 A CN 201310589606A CN 103569961 A CN103569961 A CN 103569961A
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Abstract
The invention discloses a preparation method for a silver nanoparticle chain under inducement of a silicon nanowire. The method comprises the following steps of removing a surface oxidation layer of the silicon nanowire, and dispersing the silicon nanowire into ethanol solution; preheating etchant containing silver ions and hydrofluoric acid to a certain temperature, pouring the etchant into silicon nanowire dispersion liquid, constantly mixing the mixture, and after reacting the mixture for a certain period of time, centrifuging reacted liquid, and conducting collection and sedimentation to obtain the silver nanoparticle chain. The preparation method for the silver nanoparticle chain under inducement of the silicon nanowire is fast, convenient, and low in equipment price, preparation can be conducted at low temperature, the length and the trend of the silver nanoparticle chain can be adjusted according to the length and the arrangement manner of the silicon nanowire, the size of metal particles in the silver nanoparticle chain ranges from 50-100m, the space between adjacent particles is smaller than 10 nanometers, and large quantity of samples can be prepared to meet different requirements for application, particularly meet the requirement of an ultra-sensitive SERS substrate.
Description
Technical field
The original position preparation that the present invention relates to a kind of One Dimension Silicon nano wire induction detects the preparation method of the silver nanoparticle chain of substrate as hypersensitive SERS.
Background technology
Raman spectral information is abundant, chemical constitution is had to fingerprint recognition effect, and the required amount of samples of Raman detection technology based on Raman spectrum is few, analysis efficiency is high and do not destroy sample, is therefore more and more subject to extensive concern.
Surface-enhanced Raman (Surface enhanced raman scattering, SERS) effect refers in some metal surfaces or colloidal sol of special preparation (as coarse gold, silver or copper), while adding detected sample, in excitation area, the magnetic field of sample surfaces or nearly surface significantly strengthens, the phenomenon that causes the Raman scattering intensity of the sample molecule that is adsorbed greatly to strengthen.At present, this technology has reached high sensitivity, even Single Molecule Detection rank.Wherein, because silver nano-grain has the preparation of being easy to and strengthens remarkably productive advantage and widely used.Theoretical modeling calculates and to show, if silver nano-grain is assembled, and while making grain spacing≤10nm, can form " focus " at particle gap location, and surface-enhanced Raman signal is now the most obvious.
The extensive use of current highly sensitive SERS technology is subject to the restriction of substrate, is difficult to obtain repeatably testing result.This is mainly because generally adopt silver nano-grain and aggregation thereof as SERS substrate at present.In these substrate preparation process, be random arrangement, be difficult to guarantee the repeatability of substrate pattern, and SERS depend on substrate pattern to heavens.In addition, because silver nano-grain has the character of photic distortion, this likely causes pattern in testing process to change, thereby affects the authenticity of SERS signal.
For obtain providing can repeating signal SERS substrate, there are bibliographical information application BL method, photoetching ranking method that the materials such as gold, silver are made to structurally ordered micro-structural (Andrea Tao, Franklin Kim, Christian Hess, Joshua Goldberger, Rongrui He, Yugang Sun, Younan Xia, Peidong Yang Nano Lett., 2003,3,9and Jesse Theiss, Prathamesh Pavaskar, Pierre M.Echternach, Richard E.Muller, Stephen B.Cronin, Nano Lett., 2010,10,2749).Although but the structure that this method obtains has repeatability, but still it is unstable to overcome silver nano-grain, easily distortion, the difficulty of reuniting.Therefore sensitivity and repeatability are bad.In addition, the desired equipment of photoetching technique is complicated, sample preparation speed is slow, cost is very high.Also there is bibliographical information by finishing, to improve stability (the Ping Ji Huang of silver nano-grain, Lai-Kwan Chau, Tzyy Schiuan Yang, Li Lin Tay, Tai Tsung Lin, Adv.Funct.Mater., 2009,19,242), but finishing meeting affects the Surface Contact of detected material and silver nano-grain, reduce detection sensitivity, in detection, may introduce Interference Peaks simultaneously.Therefore, find a kind of method of preparing silver nano-grain package assembly, the substrate that stable to prepare, highly sensitive SERS detects remains the focus that researchers pay close attention to.
Summary of the invention
First technical problem that the present invention will solve is to provide a kind of preparation method of silver nanoparticle chain of One Dimension Silicon nano wire induction.
For solving above-mentioned first technical problem, the present invention adopts following technical proposals:
A preparation method for the silver nanoparticle chain of nano wire induction, the method comprises the steps:
1) silicon nanowires is scattered in and in absolute ethyl alcohol, forms silicon nanowires dispersion liquid;
2) etching liquid of silver ion and hydrofluoric acid is carried out to preheating;
3) etching liquid after preheating poured in dispersion liquid and continued to stir;
4) after stirring, mixed liquor is carried out centrifugal, collecting precipitation, obtains silver nanoparticle chain;
Preferably, step 1) diameter of described silicon nanowires is about 100-500nm.
Preferably, step 1) described silicon nanowires is the silicon nanowires of removing surface oxide layer, and described dispersion refers to that the silicon nanowires of removing surface oxide layer is scattered in absolute ethyl alcohol completely; The described silicon nanowires of removing surface oxide layer refers to, the silicon nanowires of surface coverage oxide layer is soaked in to ultrasonic dispersion in the hydrofluoric acid solution that mass concentration is 5%-10%, place after 20-30min, centrifugation, collecting precipitation, and rinse with deionized water, absolute ethyl alcohol, collect the precipitation obtaining and be the silicon nanowires of removing surface oxide layer; The silicon nanowires of described surface coverage oxide layer is to make catalyst with glass putty, and thermal evaporation silicon monoxide powder preparation obtains; Or take silicon chip as raw material, etching method obtains.
Preferably, described in step 1), in silicon nanowires dispersion liquid, the content of silicon nanowires is 0.5-1mg/ml
Preferably, step 2) described etching liquid is selected from the mixed solution of liquor argenti nitratis ophthalmicus and hydrofluoric acid solution or the mixed solution of silver acetate solution and hydrofluoric acid solution, and the mixed solution of described liquor argenti nitratis ophthalmicus and hydrofluoric acid solution refers to the mixed aqueous solution of 0.5-2mmol/L liquor argenti nitratis ophthalmicus and 3-6mol/L hydrofluoric acid solution.
Preferably, described etching liquid is selected from the mixed aqueous solution of 1-1.5mmol/L liquor argenti nitratis ophthalmicus and 4-5mol/L hydrofluoric acid solution; More preferably, described etching liquid is selected from the mixed aqueous solution of mixed aqueous solution, 1mmol/L liquor argenti nitratis ophthalmicus and 4.5mom/L hydrofluoric acid solution or the mixed aqueous solution of 1.5mmol/L liquor argenti nitratis ophthalmicus and 5.0mom/L hydrofluoric acid solution of 0.5mmol/L liquor argenti nitratis ophthalmicus and 4.0mom/L hydrofluoric acid solution.
Preferably, step 3) described preheat temperature is 30-60 ℃; Preferably, described preheat temperature is 40-50 ℃; More electedly, described preheat temperature is 40 ℃, 45 ℃ or 50 ℃.
Preferably, step 3) described whipping temp is 15 ℃-25 ℃; Mixing time is 1min-5min; Described mixing time is 2-3min.
Preferably, step 4) described mixed liquor centrifugal condition is, by mixed liquor centrifugal 3min under 8000r/min rotating speed, silver nanoparticle chain to be separated from solution system.Then silver nanoparticle chain is used to deionized water ultrasonic irrigation 3 times successively, use again absolute ethyl alcohol ultrasonic irrigation 3 times, each all centrifugal 5min under 8000r/min rotating speed of rear solution that rinse, collect each centrifugal solid product obtaining, and obtain the silver nanoparticle chain of One Dimension Silicon nano wire induction.
Preferably, the described silver nanoparticle chain length preparing and trend can be adjusted according to the length of silicon nanowires and arrangement mode, its width is 100-200nm, and the metallic particles in silver nanoparticle chain is of a size of 50-100nm, adjacent particle spacing <10nm.
Silicon nanowires used in the present invention can prepare by following two kinds of methods: (1), chemical vapour deposition technique CVD method: using glass putty as catalyst, in tube type vacuum stove, thermal evaporation silicon monoxide SiO powder makes silicon nanowires, and the surface of silicon nanowires of preparation is coated with layer of silicon dioxide SiO by this method
2oxide layer, the diameter of this nano wire is about 100-500nm.Preparation thick product in absolute ethyl alcohol after ultrasonic dispersion through multiple times of filtration, can use; (2), etching method: the single-sided polishing silicon chip of having bought is cut into small pieces, after cleaning up, is containing silver nitrate (AgNO
3) and the etching liquid of hydrofluoric acid (HF) in heat etching, afterwards, with blade, silicon nanowires is scraped off stand-by.
The silicon nanowires that the present invention be take after hydrofluoric acid treatment is prepared silver nanoparticle chain as template, this surface of silicon nanowires has special reproducibility, metal ion in solution can be reduced into simple substance and be deposited on surface of silicon nanowires, surface of silicon nanowires is oxidized to silica (SiO simultaneously
2), the hydrofluoric acid in solution (HF) is with being about to its dissolving.Therefore, by the method, silicon nanowires is to the generation of silver nano-grain and grow up and guide, and makes silver nanoparticle chain simultaneously.
Beneficial effect of the present invention is as follows:
Preparation method's simple and fast of the present invention, equipment is cheap, can carry out at low temperatures, the silver nanoparticle chain length making and trend can be adjusted according to the length of silicon nanowires and arrangement mode, metallic particles in silver nanoparticle chain is of a size of 50-100nm, and adjacent particle spacing <10nm can prepare sample in a large number, to meet the needs of different application, especially meet the needs for overdelicate SERS substrate.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail;
Fig. 1 a is transmission electron microscope (TEM) photo of the silver nanoparticle chain of the One Dimension Silicon nano wire induction for preparing of embodiment 1;
Fig. 1 b is that the silver nanoparticle chain of the One Dimension Silicon nano wire induction for preparing of embodiment 1 is for rhodamine 6G Raman detection spectrogram;
Fig. 2 a is SEM (SEM) photo of the silver nanoparticle chain of the One Dimension Silicon nano wire induction for preparing of embodiment 2;
Fig. 2 b be the One Dimension Silicon nano wire induction for preparing of embodiment 2 silver nanoparticle chain for rhodamine 6G Raman detection spectrogram.
The specific embodiment
For understanding better the present invention, will further illustrate the solution of the present invention by specific embodiment below, protection scope of the present invention should comprise the full content of claim, but is not limited to this.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
The silver nitrate using in embodiment, hydrofluoric acid (mass concentration is 40%), is all purchased from Beijing chemical reagents corporation; Silicon chip (N-type, 0.01～0.02 Ω/cm) is purchased from Tianjin semiconductor institute, before use, is not all for further processing.
Embodiment 1, the silver nanoparticle chain of preparing One Dimension Silicon nano wire induction detect substrate as hypersensitive SERS
Prepare silicon nanowires: using glass putty as catalyst, thermal evaporation silicon monoxide powder obtains; Specific as follows: to take the silicon monoxide powder of 1.0g and the glass putty of 3.0g, be placed on respectively in different porcelain boats, the porcelain boat that glass putty is housed is put in to the high-temperature region of vacuum tube furnace, the porcelain boat that silicon monoxide powder is housed is put in to distance high-temperature district 5cm near the position of tube furnace outlet, sealing vacuum tube furnace; Be pumped to pressure to 5 * 10 in furnace chamber
-2after mbar, with the speed of 40 ℃/min, furnace high-temperature district is heated to 1360 ℃, after insulation 7-8h, is cooled to room temperature.The silicon nanowires diameter of preparation is about 100-500 nanometer, the oxide layer of the coated one deck silicon in surface.The first ultrasonic dispersion in ethanolic solution of the thick product of silicon nanowires of experiment preparation could be used after multiple times of filtration.
Take the above-mentioned silicon nanowires of about 1mg and be put in centrifuge tube, adding wherein 2-5ml mass fraction is 10% hydrofluoric acid solution, after ultrasonic dispersion number minute, places and removes surface oxide layer in 15 minutes, centrifugation, the silicon nanowires of the surface oxide layer that is removed.
The silicon nanowires of removing surface oxide layer is dispersed in ethanolic solution, silicon nanowires is disperseed.The etching liquid 5ml being mixed into of the hydrofluoric acid solution of the liquor argenti nitratis ophthalmicus by 1m mol/L and 4.5mol/L is preheated to 40-50 ℃ in lighttight cleansing bath tub.Get silicon nanowires dispersion liquid 1mL, at room temperature after stirred for several minute, use disposable syringe to add rapidly wherein the preheated etching liquid of 5mL, under room temperature condition, continue stirring reaction 1min, after finishing, reaction by final solution centrifugal 3min under 8000r/min rotating speed, product is separated from solution system.Then by product with deionized water ultrasonic irrigation 3 times, use again absolute ethyl alcohol ultrasonic irrigation 3 times, each all centrifugal 5min under 8000r/min rotating speed of rear solution that rinse, collect each centrifugal solid product obtaining, the silver nanoparticle chain that obtains the induction of One Dimension Silicon nano wire, is finally dispersed in absolute ethyl alcohol stand-by by the silver nanoparticle chain of preparation.
The alcohol dispersion liquid of silver nanoparticle chain is dropped on copper mesh, after ethanol evaporation at the pattern of transmission electron microscope (TEM) Microscopic observation silver nanoparticle chain.In order to check the material of preparation whether to have hypersensitive Raman, strengthen ability, we adopt Raman spectrometer (Renishaw Raman Invia Reflex Spectroscopy) at super low concentration (5 * 10
-12mol/L) under testing conditions, collect the raman spectral signal of dye molecule rhodamine 6G.
The pattern of the silver nanoparticle chain of resulting One Dimension Silicon nano wire induction as shown in Figure 2 a.Average grain diameter by the known silver nano-grain of Fig. 1 a is about 55nm, and adjacent particle spacing is about 4nm; The test super low concentration (5 * 10 of this sample
-12mol/L) rhodamine 6G SERS as shown in Figure 1 b, can find out that by Fig. 1 b sample has the ability that super low concentration detects.
Embodiment 2, the silver nanoparticle chain of preparing One Dimension Silicon nano wire induction detect substrate as hypersensitive SERS
The silver nanoparticle chain of preparing the induction of One Dimension Silicon nano wire according to the method for embodiment 1, difference is that the silicon nanowires using in the present embodiment is for to be made by chemical etching method.
Prepare silicon nanowires: silicon chip is cut into 1cm * 2cm size, after cleaning in deionized water, in ethanolic solution, clean again, clean after 3 times, silicon chip is put into and contained the solution that the concentrated sulfuric acid (97%) and hydrogen peroxide (35%), volume ratio are 3:1, soak 10 minutes, to remove the organic matter of silicon chip surface.Silicon chip immerses in the mixed liquor of the liquor argenti nitratis ophthalmicus of 18mmol/L and the hydrofluoric acid solution of 4.8mol/L, under 50 ℃ of water bath condition, reaction 15mins, after silicon chip is taken out, water washes out the floccule adhering to, and put it into and in chloroazotic acid, soak 30mins, except the silver-colored particle of attachment removal, with deionized water, absolute ethyl alcohol, rinse well afterwards.With blade, silicon nanometer is hung from silicon chip, put into plastic tube standby.
The further processing of silicon nanowires and the preparation of silver nanoparticle chain all adopt the method in embodiment 1.The alcohol dispersion liquid of silver nanoparticle chain is dropped on the silicon chip of polishing, after taking alcohol evaporation, under SEM (SEM), observe the pattern of silver nanoparticle chain.The pattern of the silver nanoparticle chain of resulting One Dimension Silicon nano wire induction as shown in Figure 2 a.Average grain diameter by the known silver nano-grain of Fig. 2 a is about 40nm, and adjacent particle spacing is about 5nm; The test super low concentration (5 * 10 of this sample
-12mol/L) rhodamine 6G SERS as shown in Figure 2 b, can find out that by Fig. 2 b sample has the ability that super low concentration detects.
Embodiment 3, the silver nanoparticle chain of preparing One Dimension Silicon nano wire induction detect substrate as hypersensitive SERS
According to the method for embodiment 1, prepare silver nanoparticle chain, what difference was to use in the present embodiment is that silver acetate replaces silver nitrate.
Embodiment 4, the silver nanoparticle chain of preparing One Dimension Silicon nano wire induction detect substrate as hypersensitive SERS
According to the method for embodiment 2, prepare silver nanoparticle chain, what difference was to use in the present embodiment is that silver acetate replaces silver nitrate.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give all embodiments exhaustive, every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (10)
1. a preparation method for the silver nanoparticle chain of One Dimension Silicon nano wire induction, is characterized in that, comprises the steps:
1) silicon nanowires is scattered in and in absolute ethyl alcohol, forms silicon nanowires dispersion liquid;
2) etching liquid of silver ion and hydrofluoric acid is carried out to preheating;
3) etching liquid after preheating poured in dispersion liquid and continued to stir;
4) after stirring, mixed liquor is carried out centrifugal, collecting precipitation, obtains silver nanoparticle chain.
2. preparation method according to claim 1, is characterized in that: step 1) diameter of described silicon nanowires is about 100-500nm.
3. preparation method according to claim 1, is characterized in that: step 1) described silicon nanowires is the silicon nanowires of removing surface oxide layer, described dispersion refers to that the silicon nanowires of removing surface oxide layer is scattered in absolute ethyl alcohol completely; The described silicon nanowires of removing surface oxide layer refers to, the silicon nanowires of surface coverage oxide layer is soaked in to ultrasonic dispersion in the hydrofluoric acid solution that mass concentration is 5%-10%, place after 20-30min, centrifugation, collecting precipitation, and rinse with deionized water, absolute ethyl alcohol, collect the precipitation obtaining and be the silicon nanowires of removing surface oxide layer; The silicon nanowires of described surface coverage oxide layer is to make catalyst with glass putty, and thermal evaporation silicon monoxide powder preparation obtains; Or take silicon chip as raw material, etching method obtains.
4. preparation method according to claim 1, is characterized in that: described in step 1), in silicon nanowires dispersion liquid, the content of silicon nanowires is 0.5-1mg/ml.
5. preparation method according to claim 1, it is characterized in that: step 2) described etching liquid is selected from the mixed solution of liquor argenti nitratis ophthalmicus and hydrofluoric acid solution or the mixed solution of silver acetate solution and hydrofluoric acid solution, and the mixed solution of described liquor argenti nitratis ophthalmicus and hydrofluoric acid solution refers to the mixed aqueous solution of 0.5-2mmol/L liquor argenti nitratis ophthalmicus and 3-6mol/L hydrofluoric acid solution.
6. preparation method according to claim 5, is characterized in that: described etching liquid is selected from the mixed aqueous solution of 1-1.5mmol/L liquor argenti nitratis ophthalmicus and 4-5mol/L hydrofluoric acid solution; More preferably, described etching liquid is selected from the mixed aqueous solution of mixed aqueous solution, 1mmol/L liquor argenti nitratis ophthalmicus and 4.5mom/L hydrofluoric acid solution or the mixed aqueous solution of 1.5mmol/L liquor argenti nitratis ophthalmicus and 5.0mom/L hydrofluoric acid solution of 0.5mmol/L liquor argenti nitratis ophthalmicus and 4.0mom/L hydrofluoric acid solution.
7. preparation method according to claim 1, is characterized in that: step 3) described preheat temperature is 30-60 ℃; Preferably, described preheat temperature is 40-50 ℃; More electedly, described preheat temperature is 40 ℃, 45 ℃ or 50 ℃.
8. preparation method according to claim 1, is characterized in that: step 3) described whipping temp is 15 ℃-25 ℃; Mixing time is 1min-5min; Described mixing time is 2-3min.
9. preparation method according to claim 1, is characterized in that: step 4) described mixed liquor centrifugal condition is, by mixed liquor centrifugal 3min under 8000r/min rotating speed, silver nanoparticle chain to be separated from solution system.Then silver nanoparticle chain is used to deionized water ultrasonic irrigation 3 times successively, use again absolute ethyl alcohol ultrasonic irrigation 3 times, each all centrifugal 5min under 8000r/min rotating speed of rear solution that rinse, collect each centrifugal solid product obtaining, and obtain the silver nanoparticle chain of One Dimension Silicon nano wire induction.
10. according to the preparation method described in claim 1-9 any one, it is characterized in that: described in the silver nanoparticle chain length for preparing and trend can adjust according to the length of silicon nanowires and arrangement mode, its width is 100-200nm, metallic particles in silver nanoparticle chain is of a size of 50-100nm, adjacent particle spacing <10nm.
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Application publication date: 20140212 |