CN103257132A - Silver nanoparticle cap array surface-enhanced raman activity substrate and preparation method thereof - Google Patents
Silver nanoparticle cap array surface-enhanced raman activity substrate and preparation method thereof Download PDFInfo
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- CN103257132A CN103257132A CN2013101311200A CN201310131120A CN103257132A CN 103257132 A CN103257132 A CN 103257132A CN 2013101311200 A CN2013101311200 A CN 2013101311200A CN 201310131120 A CN201310131120 A CN 201310131120A CN 103257132 A CN103257132 A CN 103257132A
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Abstract
The invention discloses a silver nanoparticle cap array surface-enhanced raman activity substrate and a preparation method thereof. The substrate is formed in a way that a silver film with an order nanoparticle cap array structure adhered to a silicon single crystal underlayer, the thickness of the silver film is 80-150mm, silver nanoparticle caps are in raised foam-shaped structures the centers of which are provided with holes, the diameters of the silver nanoparticle caps are 30-95nm, and center distance of the adjacent two adjacent nanometer caps is 100-110nm. The silver nanoparticle cap array surface-enhanced raman activity substrate provided by the invention has the advantages that the morphology is uniform, the structure is controlled, the prominent surface raman enhancing effects can be realized on analytes with different densities, the enhancing factor can achieve 109, and an enhancing signal is uniform and stable. A method provided by the invention has the advantages that structure parameters and morphologies of the silver nanoparticle caps are adjusted according to structure parameters of an ultrathin alumina template and a metal sedimentation process, and parameters of the silver nanoparticle cap array substrate can adjust and control the surface raman enhancing effect, the operation is simple, the cost is low, the volume production is easy, and the repeatability of products among different batches is high.
Description
Technical field
The present invention relates to a kind of surface reinforced Raman active substrate and preparation method thereof, particularly a kind of silver nanoparticle cap array surface strengthens Raman active substrate and preparation method thereof.
Background technology
Since Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering, SERS) be found in 1974 after, be widely used in fields such as surface interface science, analysis science and biomedicines very soon, for the structure that deeply characterizes various surface/interface and process provide information on the molecular level.Through constantly development and research, it has shown great potentiality in life science and nano science field, because it has very high sensitivity, can detect the unimolecular layer that is adsorbed on the metal surface and the molecule of inferior unimolecular layer, can provide the structural information of surface molecular again, be considered to the instrument of a kind of very effective detection interfacial characteristics and intermolecular interaction, sign surface molecular absorption behavior and molecular structure.
In view of the SERS technology has a wide range of applications, become key component at the bottom of preparing the SERS active group that a kind of stability is high, enhancing is effective, reappearance is strong.A lot of at the bottom of traditional SERS active group of using always at present, as: the noble metal active electrode basement of electrochemical rougheningization, at the bottom of the noble metal colloidal sol active group, at the bottom of the active group of the film activity substrate of vacuum evaporation noble metal island, the substrate of noble metal dendrite and chemical etching and chemogenic deposit noble metal, yet the surfaceness that provides at the bottom of these self assembly active groups is difficult to control thereby influenced stability, homogeneity and the repeatability of absorbing molecules spectrum.The shortcomings and limitations that the method for the orderly surface nano-structure of preparation that Recent study is more has some preparations and uses, for example: use the area of the prepared surface nano-structure of beamwriter lithography and scan-probe method very little, productive rate is low, apparatus expensive; For self-organizing growth method and nano impression method, usually than the difficult structural parameters of regulating surface nano-structure.And because its preparation procedure is loaded down with trivial details, preparation cost height and preparation efficiency are low etc., and reason limits its development.Therefore it is a kind of efficient, flexible, low-cost to be badly in need of exploitation, can prepare high sensitivity, can repeat, the method for the surface nano-structure SERS substrate of stable homogeneous.
Film substrate is a kind of stable SERS substrate, refers to cover nanoscale, rough surface, satisfy the metallic diaphragm that surface plasma excites at solid carrier surface.The surface geometry form of metal film will be to determine the analyte Raman signal to strengthen the key of effect in the solid-state SERS substrate.Novel UTAM(Ultra-Thin Alumina Mask, ultrathin alumina template) the nano surface technology of preparing provides the method for the controlled surface nano-structure of a kind of effective preparation large tracts of land and structure.UTAM nano surface technology of preparing has lot of advantages, comprise that structural parameters are adjustable, large-area preparation, performance are controlled, high density, fast and high production, equipment drop into lowly, these advantages make UTAM nano surface technology of preparing become a very promising research direction in the Surface Nano-Patterning research field and have been subjected to paying close attention to widely.
Summary of the invention
One of purpose of the present invention is to provide a kind of silver nanoparticle cap array surface to strengthen Raman active substrate.
It is a kind of based on UTAM(Ultra-Thin Alumina Mask that two of purpose of the present invention is to provide, the ultrathin alumina template) the silver nanoparticle cap array surface of nano surface technology of preparing strengthens the preparation method of Raman active substrate, to be used for that trace compound and biomolecule are detected analysis.
For achieving the above object, the present invention is by the following technical solutions:
A kind of silver nanoparticle cap array surface strengthens Raman active substrate, it is characterized in that this substrate is to be stained with the silver-colored film that one deck has orderly silver nanoparticle cap array structure in silicon monocrystalline substrate: the thickness of this silver film is 80 ~ 150 nm, described silver nanoparticle cap is the center balloon-shaped structure with holes of protuberance, diameter is 30～95 nm, and adjacent two nanometer cap centre distance are 100～110 nm.
A kind of method for preparing above-mentioned silver nanoparticle cap array surface enhancing Raman active substrate is characterized in that the concrete steps of this method are,
A. ultrathin alumina template UTAM preparation;
B. step a gained UTAM is carried out aperture adjustment;
C. step b gained UTAM is transferred on the Si substrate;
D. with step c gained UTAM/Si sample, be 8 * 10 in vacuum tightness
-4Pa, under evaporation rate 0.3～0.5 nm/s condition, evaporation silver powder 200～300 s; Remove UTAM and Si substrate then, the surface that will have an orderly silver nanoparticle cap array is transferred in the deionized water up and is cleaned, and it is gone to after the cleaning to stick in the acetone on the single crystalline Si substrate again, namely gets the silver nanoparticle cap surface and strengthen Raman active substrate after solidifying.
The concrete steps of above-mentioned ultrathin alumina template UTAM are:
A_1. the pre-service of aluminium flake: with high-purity aluminium flake ultrasonic cleaning 30 min in acetone of 0.2 mm thick 99.999%, 450～550 ℃ of annealing under the nitrogen protection, in the mixed liquor of the ethanol of 0 ℃ of temperature and perchloric acid, carry out electrochemical polish under the 750 mA constant current conditions then;
A_2. anodic oxidation: be electrolytic solution with the aluminium flake after step a_1 handles with 0.3 M oxalic acid solution, after carrying out the anodized first time under the 40 V constant voltages, the time is 7～12 h; Soaking 10 h then under 60 ℃ of conditions of temperature in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, is electrolytic solution with 0.3 M oxalic acid solution again, carries out the anodic oxidation second time 3～5 min under 40 V constant voltages;
A_3. the removal of unreacted aluminium substrate: step a_2 gained alumina formwork is immersed in CuCl
2In the mixed liquor of HCl, unoxidized aluminium substrate is dissolved away fully, to obtain pure ultrathin alumina template.
Above-mentioned UTAM aperture adjustment concrete steps are: the barrier layer of alumina formwork is swum in 30 ℃ down, and mass percent is in 5% the dilute phosphoric acid solution, and reaming times 45～60 min obtains the UTAM in different apertures.
The concrete steps that above-mentioned UTAM transfers on the Si substrate are: will swim in the acetone soln with the UTAM sample of photoresist through after the reaming and surface, the photoresist for the treatment of the surface all after the dissolving, is transferred to UTAM on the clean Si substrate.
The concrete steps that above-mentioned UTAM removes are: the UTAM/Si sample that will evaporate certain thickness silver film is immersed in the NaOH solution of 0.1M, this moment, silicon base was separated with UTAM, continue to soak 20 min, UTAM is dissolved fully, the silver-colored film of individualism forwarded in the deionized water clean, again it is gone to after the cleaning and stick in the acetone on the single crystalline Si substrate that is coated with UV glue, after solidifying, namely get the silver nanoparticle cap surface and strengthen Raman active substrate.
Advantage of the present invention and effect are: the present invention has the following advantages compared with prior art:
1) the silver nanoparticle cap array surface of UTAM method provided by the invention preparation strengthens Raman active substrate pattern homogeneous, and structure is controlled, has significant surface Raman enhancement effect for the analyte of variable concentrations, and strengthens the signal stable homogeneous.
2) large tracts of land high-sequential provided by the invention, the controlled silver nanoparticle cap array surface of structure strengthen the preparation method of Raman active substrate, can regulate structural parameters and the pattern of porous order thin film according to the structural parameters of ultrathin alumina template, realize that silver nanoparticle cap array substrate strengthens the Different Effects of effect to Raman surface.
3) preparation method of the surface reinforced Raman active substrate of large tracts of land high-sequential provided by the invention, the controlled silver nanoparticle cap of structure array can realize preparing the surface nano-structure based on different substrates and metal material large tracts of land high-sequential.
4) the present invention adopts with the method for UTAM as mask thermal evaporation physical vapour deposition (PVD) noble metal nano cap, has simple to operately, and cost is low, is easy to produce in batches repeatable high advantage between different batches.
Description of drawings
Fig. 1 is the SEM figure that adopts the UTAM of two-step oxidation method preparation.
Fig. 2 is the SEM figure that has deposited the part UTAM sample of Ag film.
Fig. 3 is the SEM figure that utilizes the silver nanoparticle cap array of UTAM preparation, and wherein illustration is the SEM figure of the local silver nanoparticle cap array that amplifies.
Fig. 4 is the Raman spectrogram at the bottom of the deposition gained silver nanoparticle cap array SERS active group among the UTAM that makes according to the different reaming time (being followed successively by 45,50,55 and 60 min from bottom to top), is 1 * 10 with concentration
-6The rhodamine 6G of M (R6G) solution is probe molecule.
Fig. 5 is the homogeneity for specimen SERS signal, adopts 10 some test gained SERS spectrograms at random at sample surfaces, and probe molecule is concentration 1 * 10
-6The R6G solution of M.
Embodiment
Embodiment 1: present embodiment is at the UTAM upper surface, and deposition is prepared Ag nanometer cap array structure large-area ordered, homogeneous.And with 1 * 10
-6(rhodamine 6G R6G) is probe molecule to the rhodamine of M, carries out the test of surperficial Raman spectrum.At first with aluminium flake acetone ultrasonic cleaning 30 min of 0.2 mm thick 99.999%; under the nitrogen protection after 450 ~ 550 ℃ of annealing; in the mixed liquor (volume ratio 1:9) of the ethanol of 0 ℃ of temperature and perchloric acid, electrochemical polish under constant current (750 mA) condition makes standby aluminium flake.With pretreated standby aluminium flake 40 V voltages, 4 ℃ of following oxidation 12 h in 0.3 M oxalic acid, take out, put into volume ratio and be the mixed solution of the phosphoric acid of the 1.8w% chromic acid of 1:1 and 6w%, corrosion 10 h under 60 ℃ the temperature; After washing repeatedly with deionized water, put into electrolytic tank again, adopt with once oxidation the same terms and carry out secondary oxidation 5 min.After the taking-up, the surface-coated photoresist immerses CuCl behind the baking molding
2In the mixed liquor of HCl, moltenly remove unoxidized aluminium substrate, to obtain purer UTAM sample.The UTAM sample barrier layer of removing aluminium substrate is swum in 30 ℃ of 5% dilute phosphoric acid solution of constant temperature down, to remove bottom thicker barrier layer and adjustment aperture size.Regulate the reaming time according to the experiment needs, obtain the bilateral UTAM in different apertures, the reaming time of adopting in this example is 45 ~ 60 min, and corresponding aperture is 45 ~ 60 nm.At last UTAM is dipped in the molten photoresist that goes in the acetone soln, transfers on the Si substrate, dry, standby, as shown in Figure 1.The UTAM/Si sample is placed evaporating and coating equipment, and vacuum tightness is 8 * 10
-4Under Pa, evaporation rate 0.3 ~ 0.5 nm/s condition, 100 nm are thick for evaporation silver powder, obtain structure as shown in Figure 2, use the NaOH solution removal UTAM of 0.1M then, and gained silverskin upset shifted be fixed on the substrate, make arrange on the silicon base as shown in Figure 3 in order, the silver nanoparticle cap array of structure and morphology homogeneous.Structural parameters according to UTAM are regulated, and the argent nanometer cap array surface that can prepare a series of different parameters (hole diameter at silver nanoparticle center is 12 ~ 35 nm) strengthens Raman active substrate.It is 1 * 10 that the above-mentioned sample that obtains is dipped in concentration
-6Take out behind 30 min in the solution of M rhodamine 6G, nitrogen dries up, and tests with the laser capture microdissection Raman spectrometer.Fig. 4 is the Raman spectrogram at the bottom of the deposition gained silver nanoparticle cap array SERS active group among the UTAM that makes the different reaming times (being followed successively by 45,50,55 and 60 min from bottom to top).It is all fine to see that SERS signal at the bottom of the different reaming time silver nanoparticle cap array active groups strengthens effect, especially strengthens the most significantly with Raman at the bottom of the active group of the gained of reaming times 60 min, and enhancer can reach 0.98 * 10
9For the homogeneity at the bottom of the active group of investigating preparation, get 10 points at random at sample surfaces and survey its SERS, the gained result as shown in Figure 5, three principal character peak 1362cm
-1, 1509cm
-1, 1650cm
-1Relative standard deviation be respectively 6.2%, 6.5%, 6.6%, according to bibliographical information, at the bottom of the SERS active group, the relative standard deviation at its characteristic peak place is wanted＜20 %, Raman signal relative standard deviation＜7% of the silver nanoparticle cap array for preparing by UTAM in this example, the surface-enhanced Raman basal signal stable homogeneous that this method makes is described, favorable repeatability can be used for the detection of trace compound or biomolecule.
Claims (6)
1. a silver nanoparticle cap array surface strengthens Raman active substrate, it is characterized in that this substrate is to be stained with the silver-colored film that one deck has orderly silver nanoparticle cap array structure in silicon monocrystalline substrate; The thickness of this silver film is: 80～150 nm; Described silver nanoparticle cap is the center balloon-shaped structure with holes of protuberance, and diameter is 30～95 nm, and adjacent two nanometer cap centre distance are 100～110 nm.
2. one kind prepares the method that silver nanoparticle cap array surface according to claim 1 strengthens Raman active substrate, it is characterized in that the concrete steps of this method are,
A. ultrathin alumina template UTAM preparation;
B. step a gained UTAM is carried out aperture adjustment;
C. step b gained UTAM is transferred on the Si substrate;
D. with step c gained UTAM/Si sample, be 8 * 10 in vacuum tightness
-4Pa, under evaporation rate 0.3～0.5 nm/s condition, evaporation silver powder 200～300 s; Remove UTAM and Si substrate then, the surface that will have an orderly silver nanoparticle cap array is transferred in the deionized water up and is cleaned, and it is gone to after the cleaning to stick in the acetone on the single crystalline Si substrate again, namely gets the silver nanoparticle cap surface and strengthen Raman active substrate after solidifying.
3. method according to claim 2 is characterized in that the concrete steps that prepare described ultrathin alumina template UTAM are:
A_1. the pre-service of aluminium flake: with high-purity aluminium flake ultrasonic cleaning 30 min in acetone of 0.2 mm thick 99.999%, 450～550 ℃ of annealing under the nitrogen protection, in the mixed liquor of the ethanol of 0 ℃ of temperature and perchloric acid, carry out electrochemical polish under the 750 mA constant current conditions then;
A_2. anodic oxidation: be electrolytic solution with the aluminium flake after step a_1 handles with 0.3 M oxalic acid solution, after carrying out the anodized first time under the 40 V constant voltages, the time is 7～12 h; Soaking 10 h then under 60 ℃ of conditions of temperature in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, is electrolytic solution with 0.3 M oxalic acid solution again, carries out the anodic oxidation second time 3～5 min under 40 V constant voltages;
A_3. the removal of unreacted aluminium substrate: step a_2 gained alumina formwork is immersed in CuCl
2In the mixed liquor of HCl, unoxidized aluminium substrate is dissolved away fully, to obtain pure ultrathin alumina template.
4. method according to claim 2, it is characterized in that described UTAM aperture adjustment concrete steps are: the barrier layer of alumina formwork is swum in 30 ℃ down, mass percent is in 5% the dilute phosphoric acid solution, and reaming times 45～60 min obtains the UTAM in different apertures.
5. method according to claim 2, it is characterized in that the concrete steps that described UTAM transfers on the Si substrate are: will swim in the acetone soln through the UTAM sample of after the reaming and surface with photoresist, after treating the whole dissolvings of photoresist on surface, UTAM is transferred on the clean Si substrate.
6. method according to claim 2, it is characterized in that the concrete steps that described UTAM removes are: the UTAM/Si sample that will evaporate certain thickness silver film is immersed in the NaOH solution of 0.1M, this moment, silicon base was separated with UTAM, continue to soak 20 min, UTAM is dissolved fully, the silver-colored film of individualism forwarded in the deionized water clean, again it is gone to after the cleaning and stick in the acetone on the single crystalline Si substrate that is coated with UV glue, after solidifying, namely get the silver nanoparticle cap surface and strengthen Raman active substrate.
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| CN105316743A (en) * | 2015-12-08 | 2016-02-10 | 郭秋泉 | Preparation method for large-area ultrathin porous anodized alumina membranes |
| CN105954253A (en) * | 2016-04-23 | 2016-09-21 | 上海大学 | Glucose SERS detection substrate based on Ag@Ag nanodot hierarchical galaxy array and preparation method thereof |
| CN106645077A (en) * | 2015-10-28 | 2017-05-10 | 上海大学 | A preparing method of an SERS active substrate having a 'hot spot' dimension of less than 5 nm based on a novel high- and low-temperature counterboring process with a step core drill |
| CN108374153A (en) * | 2018-01-17 | 2018-08-07 | 南京大学 | A kind of Grown by Magnetron Sputtering large area, the method for high-sequential nano particle |
| CN113185144A (en) * | 2021-04-29 | 2021-07-30 | 安徽师范大学 | Preparation method of echinoid ordered micro-nano array structure |
| CN114018897A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
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| CN106645077A (en) * | 2015-10-28 | 2017-05-10 | 上海大学 | A preparing method of an SERS active substrate having a 'hot spot' dimension of less than 5 nm based on a novel high- and low-temperature counterboring process with a step core drill |
| CN106645077B (en) * | 2015-10-28 | 2019-06-25 | 上海大学 | The preparation method of SERS active-substrate of the spot size less than 5nm |
| CN105316743A (en) * | 2015-12-08 | 2016-02-10 | 郭秋泉 | Preparation method for large-area ultrathin porous anodized alumina membranes |
| CN105954253A (en) * | 2016-04-23 | 2016-09-21 | 上海大学 | Glucose SERS detection substrate based on Ag@Ag nanodot hierarchical galaxy array and preparation method thereof |
| CN105954253B (en) * | 2016-04-23 | 2019-02-22 | 上海大学 | Glucose SERS detection substrate and preparation method thereof based on Ag@Ag nano dot classification galaxy array |
| CN108374153A (en) * | 2018-01-17 | 2018-08-07 | 南京大学 | A kind of Grown by Magnetron Sputtering large area, the method for high-sequential nano particle |
| CN113185144A (en) * | 2021-04-29 | 2021-07-30 | 安徽师范大学 | Preparation method of echinoid ordered micro-nano array structure |
| CN113185144B (en) * | 2021-04-29 | 2022-06-21 | 安徽师范大学 | Preparation method of echinoid ordered micro-nano array structure |
| CN114018897A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
| CN114018897B (en) * | 2021-10-21 | 2023-04-07 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
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