CN105197882A - Silicon nano cone array coated with gold film as well as preparation method and application thereof - Google Patents
Silicon nano cone array coated with gold film as well as preparation method and application thereof Download PDFInfo
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- CN105197882A CN105197882A CN201510496122.9A CN201510496122A CN105197882A CN 105197882 A CN105197882 A CN 105197882A CN 201510496122 A CN201510496122 A CN 201510496122A CN 105197882 A CN105197882 A CN 105197882A
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Abstract
The invention discloses a silicon nano cone array coated with a gold film as well as a preparation method and an application thereof. The array is a silicon nano cone sequence array with a surface coated with a gold film, wherein the conical bottom diameter of silicon nano cones forming the silicon nano cone sequence array is 180nm to 220nm, the cone height is 450nm to 550nm, the cone period is 250nm to 350nm, and the thickness of the gold film is 15nm to 25nm. The preparation method comprises the following steps: first synthesizing polystyrene colloidal spheres on a silicon substrate to form a single-layer colloidal crystal template by virtue of a gas-liquid interface self-assembling technology, placing the silicon substrate with the single-layer colloidal crystal template in a sulfur hexafluoride atmosphere, etching the silicon substrate by virtue of plasma to obtain the silicon substrate with silicon nano cone sequence array, and depositing the gold film on the silicon substrate with the silicon nano cone sequence array by utilizing an ion beam sputtering technology or thermal evaporation deposition technology to obtain a target product. The silicon nano cone array can be used as an active substrate of surface enhanced raman scattering to measure the content of clenbuterol hydrochloride attached thereon.
Description
Technical field
The present invention relates to a kind of nano-cone array and preparation method and purposes, silicon nanorods array of especially a kind of coated golden film and its production and use.
Background technology
Molecular structural formula is
clenobuterol hydrochloride, be commonly called as clenbuterol hydrochloride.If use clenobuterol hydrochloride in the process of artificial feeding animal, though the formation of animal tallow can be reduced, improve the transformation efficiency of lean meat, can cause clenobuterol hydrochloride molecule extended residual in animal body.If after people have eaten the meat containing clenobuterol hydrochloride, then the poisoning symptoms such as dizziness, palpitaition, finger be numb are there will be.At present, detecting the common method of clenobuterol hydrochloride has gas chromatography-mass spectrum to be used in conjunction method, high performance liquid chromatography, mould labelled immune adsorption measurement, capillary electrophoresis etc., so its all also exist that detectable limit is high, complicated operation, easily misrepresent deliberately, the defect such as wrong report.
In recent years, nanometer technology obtains significant progress, numerous nano material of the different material that people develop has achieved in magnetic recording, sensor to be applied widely, as being entitled as " size and pattern control based on the height ordered nanometer silica array of direct nanosphere lithography technology ", " Acta Physica Sinica " the 56th volume the 7th phase 4242nd ~ 5 pages, the article in July, 2007.The product mentioned in this article is sequential 2 D silicon nano column array; First its preparation method makes the two-dimensional ordered array of individual layer polystyrene (PS) colloidal spheres at silicon face by self-assembly method, re-use this two-dimensional ordered array of oxygen plasma etch, obtain the orderly monolayer array of the PS colloid bead of different size, then, be after source of the gas etches this orderly monolayer array with carbon tetrafluoride, high annealing removes colloidal spheres, obtains product.But, no matter be product, or its preparation method, all there is weak point, first, product can not be used for detecting clenobuterol hydrochloride; Secondly, preparation method is more loaded down with trivial details, and can not obtain the product for detecting clenobuterol hydrochloride.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming weak point of the prior art, provides a kind of rational in infrastructure, for detecting the silicon nanorods array of the coated golden film of trace clenobuterol hydrochloride.
Another technical problem that the present invention will solve is for providing a kind of preparation method of silicon nanorods array of above-mentioned coated golden film.
Another technical problem that the present invention will solve is for providing a kind of purposes of silicon nanorods array of above-mentioned coated golden film.
For solving technical problem of the present invention, the technical scheme adopted is: the silicon nanorods array of coated golden film comprises the sequential 2 D nano-silicon array be placed on silicon substrate, particularly,
Described sequential 2 D nano-silicon array is silicon nanorods oldered array, and the surface of described silicon nanorods oldered array is covered with golden film;
The cone bottom diameter of the silicon nanorods of described composition silicon nanorods oldered array is 180 ~ 220nm, bore the high 450 ~ 550nm of being, the cone cycle is 250 ~ 350nm;
The thickness of described golden film is 15 ~ 25nm.
Further improvement as the silicon nanorods array of coated golden film:
Preferably, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of the silicon nanorods array of above-mentioned coated golden film comprises the making of colloid monolayer crystal template, and particularly completing steps is as follows:
Step 1, the polystyrene colloid ball being first 250 ~ 350nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate, then to have the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it be 30 ~ 40cm
3/ min, pressure are plasma etching 3 ~ 4min in the sulfur hexafluoride atmosphere of 3 ~ 3.4Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array;
Step 2, uses ion beam sputter depositing technology or thermal evaporation deposition technology, deposited gold film on the silicon substrate being equipped with silicon nanorods oldered array thereon, the silicon nanorods array of obtained coated golden film.
Further improvement as the preparation method of the silicon nanorods array of coated golden film:
Preferably, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).
Preferably, the power of plasma etching is 180 ~ 220W.
Preferably, deposition current during ion beam sputter depositing gold film is 18 ~ 22mA, the time is 3 ~ 5min.
For solving another technical problem of the present invention, another technical scheme adopted is: the purposes of the silicon nanorods array of above-mentioned coated golden film is,
Using the active substrate of the silicon nanorods array of coated golden film as SERS (SERS), laser Raman spectrometer is used to measure the content of the clenobuterol hydrochloride of attachment on it.
Further improvement as the purposes of the silicon nanorods array of coated golden film:
Preferably, the excitation wavelength of laser Raman spectrometer is 532nm or 785nm, power output is 4 ~ 6mW, the time of integration is 8 ~ 12s; Particularly wavelength is that the exciting light of 785nm belongs to near-infrared light source, and be easy to the coupling realizing optical fiber, pole is beneficial to the trace detection of portability clenobuterol hydrochloride.
Relative to the beneficial effect of prior art be:
One, use ESEM and X-ray diffractometer to characterize respectively to obtained object product, from its result, object product is that the surface of silicon nanorods oldered array is covered with golden film; Wherein, the cone bottom diameter of the silicon nanorods of composition silicon nanorods oldered array is 180 ~ 220nm, bore the high 450 ~ 550nm of being, the cone cycle is 250 ~ 350nm, and the thickness of golden film is 15 ~ 25nm.The object product that this golden film be covered with by silicon nanorods oldered array and its surface is assembled into, both because silicon nanorods oldered array is the small-size effect that sequential 2 D nano-array makes it have nano material, make because of the existence of ordered nano taper gold the SERS focus creating Electromagnetic enhancement between cone point again, more make due to silicon nanorods oldered array and golden effectively integrating of film object product be provided with high SERS active.
Its two, using obtained object product as SERS active-substrate, through carrying out the tests of the repeatedly many batches under variable concentrations to clenobuterol hydrochloride, when the concentration of measured object clenobuterol hydrochloride is low to moderate 10
-8during mol/L, still it can be detected effectively, and its uniformity detected and the multiple spot of repeatability on object product and any point all very good.
Its three, preparation method is simple, science, efficient.Not only to obtain rational in infrastructure, for detecting the object product of trace clenobuterol hydrochloride---the silicon nanorods array of coated golden film, also make it have higher SERS active, and overcome that existing method detects that the detectable limit of clenobuterol hydrochloride is high, complicated operation, easily misrepresent deliberately, the defect such as wrong report, more have the simple and convenient feature that makes; And then make object product very easily in commercial applications in detection clenobuterol hydrochloride.
Accompanying drawing explanation
Fig. 1 is to one of result that obtained object product uses ESEM (SEM) to characterize.The pattern that SEM image demonstrates object product is nanocone oldered array.
Fig. 2 is to one of result that obtained object product uses X-ray diffraction (XRD) instrument to characterize.XRD spectra confirms that object product is made up of silicon and gold.
Fig. 3 is to one of result that the object product containing variable concentrations clenobuterol hydrochloride uses the laser Raman spectrometer that excitation wavelength is 532nm to characterize.Which confirms using object product as SERS active-substrate, the trace clenobuterol hydrochloride of attachment on it can be detected.
Fig. 4 is to one of result that the object product containing variable concentrations clenobuterol hydrochloride uses the laser Raman spectrometer that excitation wavelength is 785nm to characterize.Which confirms using object product as SERS active-substrate, the trace clenobuterol hydrochloride of attachment on it can be detected.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
First buy from market or obtain voluntarily:
Crystal face is the monocrystalline silicon piece of (100); Bulb diameter is the polystyrene colloid ball of 250 ~ 350nm.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, the polystyrene colloid ball being first 250nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate; Wherein, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).Having the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it is again 30cm
3/ min, pressure are plasma etching 3min in the sulfur hexafluoride atmosphere of 3.4Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array; Wherein, the power of plasma etching is 220W.
Step 2, uses ion beam sputter depositing (or thermal evaporation deposition) technology, and on the silicon substrate being equipped with silicon nanorods oldered array thereon, deposit thickness is the golden film of 15nm; Wherein, deposition current during ion beam sputter depositing gold film is 18mA, the time is 5min, is obtainedly similar to shown in Fig. 1, and the silicon nanorods array of coated golden film as shown in the spectral line in Fig. 2.
Embodiment 2
The concrete steps of preparation are:
Step 1, the polystyrene colloid ball being first 280nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate; Wherein, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).Having the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it is again 33cm
3/ min, pressure are plasma etching 3.3min in the sulfur hexafluoride atmosphere of 3.3Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array; Wherein, the power of plasma etching is 210W.
Step 2, uses ion beam sputter depositing (or thermal evaporation deposition) technology, and on the silicon substrate being equipped with silicon nanorods oldered array thereon, deposit thickness is the golden film of 18nm; Wherein, deposition current during ion beam sputter depositing gold film is 19mA, the time is 4.5min, is obtainedly similar to shown in Fig. 1, and the silicon nanorods array of coated golden film as shown in the spectral line in Fig. 2.
Embodiment 3
The concrete steps of preparation are:
Step 1, the polystyrene colloid ball being first 300nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate; Wherein, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).Having the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it is again 35cm
3/ min, pressure are plasma etching 3.5min in the sulfur hexafluoride atmosphere of 3.2Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array; Wherein, the power of plasma etching is 200W.
Step 2, uses ion beam sputter depositing (or thermal evaporation deposition) technology, and on the silicon substrate being equipped with silicon nanorods oldered array thereon, deposit thickness is the golden film of 20nm; Wherein, deposition current during ion beam sputter depositing gold film is 20mA, the time is 4min, obtained as shown in Figure 1, and the silicon nanorods array of coated golden film as shown in the spectral line in Fig. 2.
Embodiment 4
The concrete steps of preparation are:
Step 1, the polystyrene colloid ball being first 330nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate; Wherein, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).Having the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it is again 38cm
3/ min, pressure are plasma etching 3.8min in the sulfur hexafluoride atmosphere of 3.1Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array; Wherein, the power of plasma etching is 190W.
Step 2, uses ion beam sputter depositing (or thermal evaporation deposition) technology, and on the silicon substrate being equipped with silicon nanorods oldered array thereon, deposit thickness is the golden film of 23nm; Wherein, deposition current during ion beam sputter depositing gold film is 21mA, the time is 3.5min, is obtainedly similar to shown in Fig. 1, and the silicon nanorods array of coated golden film as shown in the spectral line in Fig. 2.
Embodiment 5
The concrete steps of preparation are:
Step 1, the polystyrene colloid ball being first 350nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate; Wherein, silicon substrate for its crystal face be the monocrystalline silicon piece of (100).Having the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it is again 40cm
3/ min, pressure are plasma etching 4min in the sulfur hexafluoride atmosphere of 3Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array; Wherein, the power of plasma etching is 180W.
Step 2, uses ion beam sputter depositing (or thermal evaporation deposition) technology, and on the silicon substrate being equipped with silicon nanorods oldered array thereon, deposit thickness is the golden film of 25nm; Wherein, deposition current during ion beam sputter depositing gold film is 22mA, the time is 3min, is obtainedly similar to shown in Fig. 1, and the silicon nanorods array of coated golden film as shown in the spectral line in Fig. 2.
The purposes of the silicon nanorods array of coated golden film is,
Using the active substrate of the silicon nanorods array of coated golden film as SERS, use laser Raman spectrometer to measure the content of the clenobuterol hydrochloride of attachment on it, obtain as or be similar to the result shown in Fig. 3 or Fig. 4; Wherein, the excitation wavelength of laser Raman spectrometer is 532nm or 785nm, power output is 4 ~ 6mW, the time of integration is 8 ~ 12s.
Obviously, those skilled in the art can carry out various change and modification to silicon nanorods array of coated golden film of the present invention and its production and use and not depart from the spirit and scope of the present invention.Like this, if belong within the scope of the claims in the present invention and equivalent technologies thereof to these amendments of the present invention and modification, then the present invention is also intended to comprise these change and modification.
Claims (8)
1. a silicon nanorods array for coated golden film, comprises the sequential 2 D nano-silicon array be placed on silicon substrate, it is characterized in that:
Described sequential 2 D nano-silicon array is silicon nanorods oldered array, and the surface of described silicon nanorods oldered array is covered with golden film;
The cone bottom diameter of the silicon nanorods of described composition silicon nanorods oldered array is 180 ~ 220nm, bore the high 450 ~ 550nm of being, the cone cycle is 250 ~ 350nm;
The thickness of described golden film is 15 ~ 25nm.
2. the silicon nanorods array of coated golden film according to claim 1, is characterized in that the silicon substrate monocrystalline silicon piece that to be its crystal face be (100).
3. a preparation method for the silicon nanorods array of coated golden film described in claim 1, comprises the making of colloid monolayer crystal template, it is characterized in that completing steps is as follows:
Step 1, the polystyrene colloid ball being first 250 ~ 350nm by bulb diameter by liquid-vapor interface self-assembling technique synthesizes colloid monolayer crystal template on silicon substrate, then to have the silicon substrate of colloid monolayer crystal template to be placed in flow synthesis on it be 30 ~ 40cm
3/ min, pressure are plasma etching 3 ~ 4min in the sulfur hexafluoride atmosphere of 3 ~ 3.4Pa, obtain the silicon substrate it being equipped with silicon nanorods oldered array;
Step 2, uses ion beam sputter depositing technology or thermal evaporation deposition technology, deposited gold film on the silicon substrate being equipped with silicon nanorods oldered array thereon, the silicon nanorods array of obtained coated golden film.
4. the preparation method of the silicon nanorods array of coated golden film according to claim 3, is characterized in that the silicon substrate monocrystalline silicon piece that to be its crystal face be (100).
5. the preparation method of the silicon nanorods array of coated golden film according to claim 3, is characterized in that the power of plasma etching is 180 ~ 220W.
6. the preparation method of the silicon nanorods array of coated golden film according to claim 3, deposition current when it is characterized in that ion beam sputter depositing gold film is 18 ~ 22mA, the time is 3 ~ 5min.
7. a purposes for the silicon nanorods array of coated golden film described in claim 1, is characterized in that:
Using the active substrate of the silicon nanorods array of coated golden film as SERS, laser Raman spectrometer is used to measure the content of the clenobuterol hydrochloride of attachment on it.
8. the purposes of the silicon nanorods array of coated golden film according to claim 7, is characterized in that the excitation wavelength of laser Raman spectrometer is 532nm or 785nm, power output is 4 ~ 6mW, the time of integration is 8 ~ 12s.
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| CN107101988A (en) * | 2017-03-16 | 2017-08-29 | 中国科学院合肥物质科学研究院 | A kind of high density nanometer pinpoint array of golden film covering and its application |
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