CN104949959A - Quick preparing method for large-area surface Raman spectrum enhancing monocrystalline silicon substrate - Google Patents
Quick preparing method for large-area surface Raman spectrum enhancing monocrystalline silicon substrate Download PDFInfo
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- CN104949959A CN104949959A CN201510406413.4A CN201510406413A CN104949959A CN 104949959 A CN104949959 A CN 104949959A CN 201510406413 A CN201510406413 A CN 201510406413A CN 104949959 A CN104949959 A CN 104949959A
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Abstract
The invention relates to a quick preparing method for a large-area surface Raman spectrum enhancing monocrystalline silicon substrate and belongs to the field of SERS substrate preparing. The quick preparing method comprises the steps that the surface of monocrystalline silicon is covered with a microballoon array which is periodically and densely arranged; microballoon left on the surface is removed through laser scanning or irradiating; the monocrystalline silicon is immersed into a sodium hydroxide water solution including alcohol, corrosion is carried out for 10-30 s in the environment with the water bath temperature ranging from 70 DEG C to 80 DEG C, the monocrystalline silicon is taken out and cleaned with deionized water, and the monocrystalline silicon with the microstructure array is obtained, wherein in the water solution, the sodium hydroxide accounts for 5%-10% by mass, and alcohol accounts for 8%-10% by mass; silver film deposition is carried out on the surface of the corroded monocrystalline silicon through magnetron sputtering, and the deposition thickness ranges from 50 nm to 200 nm. By means of the quick preparing method, the periodic and uniform microstructure array can be quickly, easily and conveniently prepared, and the performance of an SERS substrate can be controlled by controlling the morphology dimension feature of the microstructure array and the thickness of a silver film. Meanwhile, the method is high in reproducibility and low in cost, and prepared SERS substrate is stable in performance and capable of being repeatedly used.
Description
Technical field
The invention belongs to surface Raman enhancement spectrum substrate preparation field.
Background technology
Surface Raman enhancement spectrum (SERS), since being found, having obtained as a kind of powerful detection analysis tool and has paid close attention to widely.Compared to common Raman signal, in theory, when target molecule to be measured is between the gap of metal nanoparticle, the enhancer of its SERS signal can reach 10
14doubly.This enhancing can make faint Raman signal originally become detectable, even also can obtain Raman dactylogram clearly at single molecules level.And the strong anti-interference ability that Raman scattering itself has, in conjunction with SERS technology, it can be applied in complex environment of all kinds.The preparation of SERS substrate is normally by chemosynthesis or self assembly effect depositing metallic nanoparticles in solid substrate, and this method can obtain stronger enhancer.But the stability of its homogeneity and metallic particles limits its application extension detected in large area.Therefore, people propose on SERS substrate, to prepare micro-nano structure to improve its homogeneity and stability.By the method for focused-ion-beam lithography (FIB) or electron beam lithography, accurately can control pattern and the size of micro-nano structure, and there is good repeatability.Meanwhile, these methods also there is preparation expense and environmental requirement higher, the shortcomings such as preparation efficiency is lower.The Fang Feng continent group of University Of Tianjin utilizes the method for FIB to obtain at silicon face the elliptical array that minimum spacing is 15nm, and on its plated surface the gold grain film of 10-70nm, obtain good SERS effect.Simultaneously, its maximum area of preparing is 9.6 μm × 9.6 μm (" High Performance Surface-enhanced Raman Scattering Substrate of Si-based Au Film Developed by Focused Ion Beam Nanofabrication " .Nanoscale research letters.20127.Tingting Gao, et al).
In recent years, people be devoted to explore can more low cost and prepare the method for SERS substrate more efficiently.The Hai Pang Chiang group in Taiwan is by dripping painting polystyrene sphere on a glass substrate, its self assembly effect is utilized to obtain the micro-sphere array of solid matter, these micro-sphere arrays, after deposited Argent grain film, show good SERS effect (" Size Dependence of Nanoparticle-SERS Enhancement from Silver Film over Nanosphere (AgFON) Substrate " .Plasmonics (2011) 6:201 – 206.Wenchi Lin et al.).The Zhida Xu group of University of Illinois of the U.S. utilizes the silicon Template preparation of inverted pyramid to have the high molecular polymer substrate of positive pyramid and inverted pyramid array, deposited the gold grain film of 200nm above simultaneously, thus obtain the different SERS substrate (" Nanoreplicated positive and inverted submicrometer polymer pyramid array for surface-enhanced Raman spectroscopy " .Journal of Nanophotonics Vol.5,2011.Xu et al.) strengthening effect.
Therefore, improve homogeneity and the stability of SERS substrate, ensure high efficiency and low cost, be that SERS substrate prepares institute's problems faced now simultaneously.
Laser has that energy is high, easy to operate, controllability is good and noncontact irradiated heat not easily introduces the features such as pollution, and laser irradiation monocrystalline silicon can form microstructure to its modifying surface.The present invention proposes the fast preparation method that a kind of wide area surface strengthens Raman spectrum monocrystal silicon substrate, first micro structure array preparation is carried out at monocrystalline silicon surface, this monocrystalline substrate with micro structure array, after carrying out magnetron sputtering surface deposition silver nanoparticle film, shows good SERS effect.By the adjustment to microstructure appearance size characteristic and silver film thickness, the regulation and control of the SERS effect to substrate can be realized.
Summary of the invention
A kind of wide area surface is the object of the present invention is to provide to strengthen the fast preparation method of Raman spectrum monocrystal silicon substrate.
The object of the invention is to be achieved through the following technical solutions:
1, wide area surface strengthens a fast preparation method for Raman spectrum monocrystal silicon substrate, it is characterized in that, comprises the following steps:
1) adopt direct drop-coating arrange on cleaned monocrystalline silicon piece sample surfaces individual layer Hexagonal Close-packed distribution SiO
2micro-sphere array;
2) by through 1) monocrystal silicon sample that processed is positioned on target platform, and adjustment light path, adopts the ultrashort pulse laser of ultraviolet wavelength to carry out irradiation or scanning;
3) by through 2) monocrystal silicon sample that processed carries out ultrasonic cleaning and removes microballoon, immerse in the sodium hydrate aqueous solution containing ethanol, be in the environment of 70-80 DEG C at bath temperature, corrosion 10-30s, take out after corrosion and use deionized water rinsing, obtain the monocrystalline silicon piece with micro structure array; In described aqueous solution, the mass percent of NaOH is 5%-10%, and the mass percent of ethanol is 8%-10%;
4) by through 3) monocrystalline substrate that processes carries out magnetron sputtering deposition silverskin, and the magnetron sputtering time is 5-15min, and silver-plated thickness is 50-200nm.
When laser instrument adopts scanning, adopt pulsewidth≤10
-11the positive out of focus single line scan of ultrashort pulse of the ultraviolet wavelength of s, sweep spacing is laser facula size, and repetition frequency is 200-400kHz, and sweep velocity is 800-1200mm/s, and power density is 5-25W/mm
2.
When laser instrument adopts irradiation, by through 1) monocrystal silicon sample that process is positioned on target platform, adjusts light path, makes all to restraint hot spot and sample size adapts, and carries out monopulse irradiation, the excimer laser of laser instrument to be wavelength be 248nm; Adopt pulse energy density 100mJ/cm
2-400mJ/cm
2, frequency is 1-3Hz.
Further, regulated and controled by the size or the SERS effect of pattern to substrate changing micro structure array, when the interval of micro structure array reduces, the SERS effect of substrate strengthens; When the size of micro structure array increases, substrate S ERS effect strengthens.
Further, regulated and controled by the SERS effect of thickness to substrate changing Ag films, when silver film thickness is between 50-160nm, the SERS effect of substrate increases with the increase of thickness, when silver film thickness is between 160-200nm, the SERS effect of substrate reduces with the increase of thickness.
A kind of wide area surface that the present invention proposes strengthens the fast preparation method of Raman spectrum monocrystal silicon substrate, has the following advantages:
1, in the inventive method, the processing of laser irradiation microballoon can carry out precise positioning to the position that microstructure is formed, and the size that only need change microballoon just accurately can control the density degree of micro structure array, and ensures good periodicity and homogeneity.
2, in the inventive method, by the adjustment of effects on surface microstructure appearance size characteristic and silver film thickness, the adjustment of Raman enhancement effect can be realized, there is higher controllability.
3, in the inventive method, the prepared monocrystalline silicon SERS substrate stability with micro structure array is better, can reuse.
4, in the inventive method, the laser power that UV ultrashort laser device adopts is less, and technique is simple, and can realize large area processing; The time of alkaline etching is 10-30s, and the magnetron sputtering time is 5-15min, and overall manufacturing cycle is short; Meanwhile, equipment cost is lower, and structure reappearance is high, raw materials used cheap, has higher practicality.
Accompanying drawing explanation
Fig. 1 is micro structure array figure prepared by embodiment 1;
Fig. 2 is micro structure array figure prepared by embodiment 2;
Fig. 3 is micro structure array figure prepared by embodiment 3;
Fig. 4 is the Raman collection of illustrative plates of sample prepared by different parameters.
Embodiment
The cleaning of following examples is specially: monocrystalline silicon is immersed acetone soln ultrasonic cleaning 6-10 minute; 6-10 minute is soaked in the HF solution of massfraction 5%-20%; Immerse ethanolic solution ultrasonic cleaning 6-10 minute, rinse, dry; But be not limited to this cleaning way.
Embodiment 1:
Adopt direct drop-coating arrange on cleaned monocrystalline silicon piece sample surfaces individual layer Hexagonal Close-packed distribution SiO
2microballoon, Microsphere Size used is 1.5 μm; Monocrystal silicon sample is placed on target platform, adjustment light path, adopts ultrashort pulse (10ps) laser instrument of ultraviolet wavelength to carry out positive out of focus single line scan, sweep spacing is laser facula size, repetition frequency is 400kHz, and sweep velocity is 1200mm/s, and power density is 5W/mm
2; Cleaned monocrystal silicon sample is immersed in the sodium hydrate aqueous solution containing ethanol, be in the environment of 75 DEG C at bath temperature, corrosion 10s, take out and use deionized water rinsing, obtain the monocrystalline silicon piece with micro structure array, in described aqueous solution, the mass percent of NaOH is 10%, and the mass percent of ethanol is 8%; The monocrystalline silicon piece utilizing magnetron sputtering effects on surface to have micro structure array carries out silver nanoparticle thin film deposition, and sedimentation time is 8min, and acquisition thickness is 100nm.
Structure prepared is as can be seen from Figure 1 poroid shape, has periodicity and homogeneity preferably.
Embodiment 2:
Adopt direct drop-coating arrange on cleaned monocrystalline silicon piece sample surfaces individual layer Hexagonal Close-packed distribution SiO
2microballoon, Microsphere Size used is 1 μm; Monocrystal silicon sample is placed on target platform, adjustment light path, adopts ultrashort pulse (10ps) laser instrument of ultraviolet wavelength to carry out positive out of focus single line scan, sweep spacing is laser facula size, repetition frequency is 200kHz, and sweep velocity is 1000mm/s, and power density is 20W/mm
2; Cleaned monocrystal silicon sample is immersed in the sodium hydrate aqueous solution containing ethanol, be in the environment of 75 DEG C at bath temperature, corrosion 30s, take out and use deionized water rinsing, obtain the monocrystalline silicon piece with micro structure array, in described aqueous solution, the mass percent of NaOH is 10%, and the mass percent of ethanol is 10%; The monocrystalline silicon piece utilizing magnetron sputtering effects on surface to have micro structure array carries out silver nanoparticle thin film deposition, and sedimentation time is 12min, and acquisition thickness is 160nm.
Structure prepared is as can be seen from Figure 2 mound shape structure, has periodicity and homogeneity preferably.
Embodiment 3:
Adopt direct drop-coating arrange on cleaned monocrystalline silicon piece sample surfaces individual layer Hexagonal Close-packed distribution SiO
2microballoon, Microsphere Size used is 0.5 μm; Monocrystal silicon sample is placed on target platform, adjustment light path, adopts ultrashort pulse (10ps) laser instrument of ultraviolet wavelength to carry out positive out of focus single line scan, sweep spacing is laser facula size, repetition frequency is 200kHz, and sweep velocity is 1200mm/s, and power density is 25W/mm
2; Cleaned monocrystal silicon sample is immersed in the sodium hydrate aqueous solution containing ethanol, be in the environment of 70 DEG C at bath temperature, corrosion 30s, take out and use deionized water rinsing, obtain the monocrystalline silicon piece with micro structure array, in described aqueous solution, the mass percent of NaOH is 10%, and the mass percent of ethanol is 10%; The monocrystalline silicon piece utilizing magnetron sputtering effects on surface to have micro structure array carries out silver nanoparticle thin film deposition, and sedimentation time is 12min, and acquisition thickness is 160nm;
The structure prepared as can be seen from Figure 3 is bulk structure, has periodicity and homogeneity preferably.
Fig. 4, for utilizing the SERS substrate Raman collection of illustrative plates prepared by different Microsphere Size and etching time, can find out, pattern and the size of the enhancing effect adopting the SERS substrate prepared of the method to show and micro structure array are relevant.
Claims (5)
1. wide area surface strengthens a fast preparation method for Raman spectrum monocrystal silicon substrate, it is characterized in that, comprises the following steps:
1) adopt direct drop-coating arrange on cleaned monocrystalline silicon piece sample surfaces individual layer Hexagonal Close-packed distribution SiO
2micro-sphere array;
2) by through 1) monocrystal silicon sample that processed is positioned on target platform, and adjustment light path, adopts the ultrashort pulse laser of ultraviolet wavelength to carry out irradiation or scanning;
3) by through 2) monocrystal silicon sample that processed carries out ultrasonic cleaning and removes microballoon, immerse in the sodium hydrate aqueous solution containing ethanol, be in the environment of 70-80 DEG C at bath temperature, corrosion 10-30s, take out after corrosion and use deionized water rinsing, obtain the monocrystalline silicon piece with micro structure array; In described aqueous solution, the mass percent of NaOH is 5%-10%, and the mass percent of ethanol is 8%-10%;
4) by through 3) monocrystalline substrate that processes carries out magnetron sputtering deposition silverskin, and the magnetron sputtering time is 5-15min, and silver-plated thickness is 50-200nm.
2. method according to claim 1, is characterized in that:
When laser instrument adopts scanning, adopt pulsewidth≤10
-11the positive out of focus single line scan of ultrashort pulse of the ultraviolet wavelength of s, sweep spacing is laser facula size, and repetition frequency is 200-400kHz, and sweep velocity is 800-1200mm/s, and power density is 5-25W/mm
2.
3. method according to claim 1, is characterized in that:
When laser instrument adopts irradiation, by through 1) monocrystal silicon sample that process is positioned on target platform, adjusts light path, makes all to restraint hot spot and sample size adapts, and carries out monopulse irradiation, the excimer laser of laser instrument to be wavelength be 248nm; Adopt pulse energy density 100mJ/cm
2-400mJ/cm
2, frequency is 1-3Hz.
4. wide area surface strengthens the fast preparation method of Raman spectrum monocrystal silicon substrate according to claim 1, it is characterized in that: regulated and controled by the size or the SERS effect of pattern to substrate that change micro structure array, when the interval of micro structure array reduces, the SERS effect of substrate strengthens; When the size of micro structure array increases, substrate S ERS effect strengthens.
5. wide area surface strengthens the fast preparation method of Raman spectrum monocrystal silicon substrate according to claim 1, it is characterized in that: regulated and controled by the SERS effect of thickness to substrate changing Ag films, when silver film thickness is between 50-160nm, the SERS effect of substrate increases with the increase of thickness, when silver film thickness is between 160-200nm, the SERS effect of substrate reduces with the increase of thickness.
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| PCT/CN2015/084989 WO2016015599A1 (en) | 2014-07-27 | 2015-07-24 | Fast preparation method for large area monocrystalline silicon substrate with surface-enhanced raman spectrum |
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Cited By (8)
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| WO2016015599A1 (en) * | 2014-07-27 | 2016-02-04 | 北京工业大学 | Fast preparation method for large area monocrystalline silicon substrate with surface-enhanced raman spectrum |
| CN105562936A (en) * | 2015-12-22 | 2016-05-11 | 天津大学 | Preparation method of aluminum nanometer structure for surface enhancement of Raman scattering |
| CN106324073A (en) * | 2016-09-12 | 2017-01-11 | 东南大学 | Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry |
| CN107462565A (en) * | 2017-07-21 | 2017-12-12 | 山东师范大学 | Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation method |
| CN108226123A (en) * | 2017-12-12 | 2018-06-29 | 华南师范大学 | A kind of method that femtosecond laser prepares surface enhanced Raman scattering substrate |
| CN111175284A (en) * | 2020-03-19 | 2020-05-19 | 西南科技大学 | Preparation method of surface enhanced Raman substrate with layered micro/nano structure |
| CN111175285A (en) * | 2020-03-19 | 2020-05-19 | 西南科技大学 | Surface enhanced Raman substrate with layered micro/nano structure and detection method thereof |
| CN112014375A (en) * | 2020-09-03 | 2020-12-01 | 鲁东大学 | Metal circular ring inner hexagram trimer nano array and preparation method and application thereof |
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Cited By (13)
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|---|---|---|---|---|
| WO2016015599A1 (en) * | 2014-07-27 | 2016-02-04 | 北京工业大学 | Fast preparation method for large area monocrystalline silicon substrate with surface-enhanced raman spectrum |
| CN105562936A (en) * | 2015-12-22 | 2016-05-11 | 天津大学 | Preparation method of aluminum nanometer structure for surface enhancement of Raman scattering |
| CN105562936B (en) * | 2015-12-22 | 2017-03-29 | 天津大学 | A kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy |
| CN106324073A (en) * | 2016-09-12 | 2017-01-11 | 东南大学 | Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry |
| CN107462565A (en) * | 2017-07-21 | 2017-12-12 | 山东师范大学 | Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation method |
| CN108226123B (en) * | 2017-12-12 | 2021-02-23 | 华南师范大学 | Method for preparing surface enhanced Raman scattering substrate by femtosecond laser |
| CN108226123A (en) * | 2017-12-12 | 2018-06-29 | 华南师范大学 | A kind of method that femtosecond laser prepares surface enhanced Raman scattering substrate |
| CN111175284A (en) * | 2020-03-19 | 2020-05-19 | 西南科技大学 | Preparation method of surface enhanced Raman substrate with layered micro/nano structure |
| CN111175285A (en) * | 2020-03-19 | 2020-05-19 | 西南科技大学 | Surface enhanced Raman substrate with layered micro/nano structure and detection method thereof |
| CN111175284B (en) * | 2020-03-19 | 2022-06-07 | 西南科技大学 | Preparation method of surface enhanced Raman substrate with layered micro/nano structure |
| CN111175285B (en) * | 2020-03-19 | 2022-06-07 | 西南科技大学 | Surface enhanced Raman substrate with layered micro/nano structure and detection method thereof |
| CN112014375A (en) * | 2020-09-03 | 2020-12-01 | 鲁东大学 | Metal circular ring inner hexagram trimer nano array and preparation method and application thereof |
| CN112014375B (en) * | 2020-09-03 | 2023-06-16 | 鲁东大学 | Metal ring inner hexagon trimer nano-array and preparation method and application thereof |
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