CN102590179A - Silver nano lattice surface enhanced raman active substrate and preparation method thereof - Google Patents
Silver nano lattice surface enhanced raman active substrate and preparation method thereof Download PDFInfo
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- CN102590179A CN102590179A CN2012100846764A CN201210084676A CN102590179A CN 102590179 A CN102590179 A CN 102590179A CN 2012100846764 A CN2012100846764 A CN 2012100846764A CN 201210084676 A CN201210084676 A CN 201210084676A CN 102590179 A CN102590179 A CN 102590179A
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Abstract
The invention discloses a silver nano lattice surface enhanced raman active substrate and a preparation method thereof. According to the substrate, silicon single crystal is used as an underlay; a silver nanoparticle array structure is deposited on the silicon surface; the particle size of the silver nanoparticles is 30-90 nm; and the center distance of the particles is 99-111 nm. The silver nano lattice surface enhanced raman active substrate provided by the invention has a uniform shape and a controllable structure, and has an obvious surface raman enhancement effect on analytes of different concentrations, and an enhancement signal is uniform and stable. According to the method, the structural parameters and the shape of a silver nano lattice can be adjusted according to structural parameters of an ultra-thin aluminum oxide template, so that different influences of different metal nano lattice substrates on a raman surface enhancement effect are realized. The substrate and the method have the advantages of easiness for operation, low cost and easiness for industrial production.
Description
Technical field
The present invention relates to a kind of silver-colored nano-dot matrix surface reinforced Raman active substrate and preparation method thereof; Particularly a kind of silver-colored nano-dot matrix surface reinforced Raman active substrate based on UTAM (Ultra-Thin Alumina Mask, ultrathin alumina template) nano surface technology of preparing and preparation method thereof.
Background technology
SERS (Surface-enhanced Raman Scattering; SERS) since 1974 come to light; Just caused that everybody pays close attention to widely,, can detect the unimolecular layer that is adsorbed on the metal surface and the molecule of inferior unimolecular layer because of it has very high sensitivity; 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.The SERS technology becomes Surface Science and the strong research means of electrochemical field gradually; And in trace analysis and even Single Molecule Detection, chemistry and industry, environmental science, biomedical system; Obtain widespread use in the research of aspect such as nano material and sensor, even the coupling of Raman technology and other technologies occurred.
Have a wide range of applications in view of the SERS technology, become key component at the bottom of prepare a kind of stability height, reinforced effects is good, reappearance is strong SERS active group.A lot of at the bottom of traditional SERS active group commonly used 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 film activity substrate of vacuum evaporation noble metal island 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.Shortcoming and limitation that the method for the orderly surface nano-structure of preparation that Recent study is more all has some preparations and uses, for example: the area with the prepared surface nano-structure of beamwriter lithography and scan-probe method is very little, and productive rate is low, apparatus expensive; For self-organizing growth method and nano impression method, the difficult usually 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.And template has superior condition for the particle diameter of realizing particle in the nano particle assembly system and the controllability and the homogeneity of distribution thereof.Especially on AAO (Anodic Aluminum Oxide) template basis, develop and next UTAM, more provided the method for the surface nano-structure SERS substrate of a kind of effective preparation large tracts of land and controllable structure.UTAM nano surface technology of preparing has lot of advantages; Comprise that adjustable structural parameters (size, spacing, pattern, arrangement, crystal structure), large-area preparation, controlled performance, high density, fast and high production, low equipment input, these advantages make UTAM nano surface preparation method become a very promising research direction in the Surface Nano-Patterning research field and received widely and paying close attention to.
Summary of the invention
One of the object of the invention is to provide the substrate of a kind of silver-colored nano-dot matrix surface reinforced Raman active.
It is a kind of based on UTAM (Ultra-Thin Alumina Mask that two of the object of the invention is to provide; The ultrathin alumina template) preparation method of the silver-colored nano-dot matrix surface reinforced Raman active substrate of nano surface technology of preparing is to be used for that trace compound and biomolecule are carried out check and analysis.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The substrate of a kind of silver-colored nano-dot matrix surface reinforced Raman active is characterized in that this substrate is substrate with the silicon single crystal, at silicon face depositing silver nanoparticle array structure; The particle diameter of described silver nano-grain is 30～90 nm, and particle centre distance is 99～111nm.
A kind of method for preparing above-mentioned silver-colored nano-dot matrix surface reinforced Raman active substrate is characterized in that the concrete steps of this method do,
A. ultrathin alumina template UTAM preparation;
The b.UTAM aperture adjustment;
C.UTAM transfers on the Si substrate;
The preparation of d. silver-colored nano-dot matrix surface reinforced Raman active substrate:, be 5 * 10 in vacuum tightness with step ability c gained UTAM/Si sample
-6Torr, under evaporation rate 0.3～0.5nm/s condition, evaporation silver powder 100～200 s; Remove UTAM then, obtain the substrate of silver-colored nano-dot matrix surface reinforced Raman active.
The concrete steps that prepare 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: will be electrolytic solution with 0.3 M oxalic acid solution through the aluminium flake after step a_1 handles, after carrying out the anodized first time under the 40 V constant voltages, the time be 7～12 h; Under 60 ℃ of conditions of temperature, in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, soaking 10 h then, is electrolytic solution with 0.3 M oxalic acid solution again, under the 40V constant voltage, carries out the anodic oxidation second time 3～5 min;
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 that the reaming time is 45～60min, obtains the UTAM in different apertures in 5% the dilute phosphoric acid solution.
The concrete steps that above-mentioned UTAM transfers on the Si substrate are: will pass through after the reaming and the surface swims in the acetone soln with the UTAM sample of photoresist, the photoresist of treating the surface all after the dissolving, is transferred to UTAM on the Si substrate that cleans up gently.
Advantage of the present invention and effect are: the present invention has the following advantages compared with prior art:
1) the metal nano dot matrix surface reinforced Raman active substrate pattern homogeneous of UTAM method provided by the invention preparation, controllable structure has significant surface raman enhancement effect for the analyte of variable concentrations, and the enhancing signal stable homogeneous.
2) preparation method of the surface reinforced Raman active substrate of large tracts of land high-sequential provided by the invention, controllable structure metal nano dot matrix; Can regulate the structural parameters and the pattern of metal nano dot matrix according to the structural parameters of ultrathin alumina template, realize the Different Effects of different metal nano-dot matrix substrate the Raman surface reinforced effects.
3) preparation method of the surface reinforced Raman active substrate of large tracts of land high-sequential provided by the invention, controllable structure metal nano dot matrix 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 dot matrix on the Si substrate, has simple to operately, and cost is low, is easy to industrial advantage.
Description of drawings
Fig. 1 is ESEM (SEM) figure of the UTAM for preparing among the present invention.
Fig. 2 is the SEM figure that utilizes the silver-colored nano-dot matrix of UTAM preparation among the present invention.
Fig. 3 is the Raman spectrogram at the bottom of different-grain diameter (being followed successively by 50,65,70 and 75 nm from bottom to top) the SERS active group of testing among the present invention.
Embodiment
Embodiment 1: present embodiment is template with UTAM, on the Si substrate, prepares Ag nano particle dot matrix large-area ordered, homogeneous, and with 1 * 10
-7(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 subsequent use aluminium flake.With pretreated subsequent use 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 phosphoric acid of 1.8w% chromic acid and the 6w% of 1:1, corrode 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, dissolve and 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 thicker barrier layer in bottom and adjustment aperture size.Regulate the reaming time according to the experiment needs, obtain the bilateral UTAM in different apertures.At last UTAM is dipped in to dissolve in the acetone soln and removes photoresist, transfer on the Si substrate, dry, subsequent use, as shown in Figure 1.The UTAM/Si sample is placed evaporating and coating equipment, and vacuum tightness is 5 * 10
-6Under Torr, evaporation rate 0.3 ~ 0.5 nm/s condition, 50 nm are thick for evaporation silver powder.Remove UTAM then, make and arrange silver nano-grain array orderly, the structure and morphology homogeneous on the silicon base as shown in Figure 2.Structural parameters according to UTAM are regulated the argent nano-dot matrix surface reinforced Raman active substrate that can prepare a series of different holes particle diameter.It is 1 * 10 that the above-mentioned sample that obtains is dipped in concentration
-7Take out behind 30 min in the solution of M rhodamine 6G, nitrogen dries up, and tests with the laser capture microdissection Raman spectrometer.Fig. 3 is that the face of the silver-colored nano-dot matrix of different-grain diameter (being followed successively by 50,65,70 and 75 nm from bottom to top) strengthens Raman spectrum.The SERS signal reinforced effects that can see the different-grain diameter substrate is all fine, and especially remarkable with the substrate enhancing of 75 nm, enhancer can reach 1.2 * 10
8The substrate surface Raman signal that the present invention's preparation is described strengthens significantly, and the signal stable homogeneous, can be used for the detection of trace compound.
Claims (5)
1. silver-colored nano-dot matrix surface reinforced Raman active substrate is characterized in that this substrate is substrate with the silicon single crystal, at silicon face depositing silver nanoparticle array structure; The particle diameter of described silver nano-grain is 30～90 nm, and particle centre distance is 99～111 nm.
2. a method for preparing silver-colored nano-dot matrix surface reinforced Raman active according to claim 1 substrate is characterized in that the concrete steps of this method do,
A. ultrathin alumina template UTAM preparation;
The b.UTAM aperture adjustment;
C.UTAM transfers on the Si substrate;
The preparation of d. silver-colored nano-dot matrix surface reinforced Raman active substrate:, be 5 * 10 in vacuum tightness with step ability c gained UTAM/Si sample
-6Under Torr, evaporation rate 0.3～0.5 nm/s condition, evaporation silver powder 100～200 s; Remove UTAM then, obtain the substrate of silver-colored nano-dot matrix surface reinforced Raman active.
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: will be electrolytic solution with 0.3 M oxalic acid solution through the aluminium flake after step a_1 handles, after carrying out the anodized first time under the 40 V constant voltages, the time be 7～12 h; Under 60 ℃ of conditions of temperature, in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, soaking 10 h then, is electrolytic solution with 0.3 M oxalic acid solution again, under 40 V constant voltages, carries out the anodic oxidation second time 3～5 min;
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 time 45～60min 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 pass through after the reaming and the surface swims in the acetone soln with the UTAM sample of photoresist; After treating the whole dissolvings of photoresist on surface, UTAM is transferred on the Si substrate that cleans up gently.
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Cited By (14)
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| CN102849672A (en) * | 2012-09-17 | 2013-01-02 | 无锡英普林纳米科技有限公司 | Surface enhanced Raman micro-structural substrate and preparation method thereof |
| CN102998297A (en) * | 2012-12-11 | 2013-03-27 | 东南大学 | Porous microscale reaction plate for surface enhanced Raman scattering spectrum analysis |
| CN103257132A (en) * | 2013-04-16 | 2013-08-21 | 上海大学 | Silver nanoparticle cap array surface-enhanced raman activity substrate and preparation method thereof |
| CN103526288A (en) * | 2013-10-10 | 2014-01-22 | 宋玉军 | Method for interface effect induced self-assembly of high-density nano array |
| CN104568896A (en) * | 2013-10-23 | 2015-04-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Surface enhanced Raman scattering sensor and preparation method thereof |
| CN104630772A (en) * | 2013-11-12 | 2015-05-20 | 中国科学院物理研究所 | Multilayer stacked metal nanosphere array and preparation method thereof |
| CN104949957A (en) * | 2015-04-07 | 2015-09-30 | 上海大学 | Embedded type nano dot array surface enhanced Raman active substrate and preparation method thereof |
| CN105158228A (en) * | 2015-07-30 | 2015-12-16 | 西北大学 | SERS (Surface enhanced Raman Scattering) substrate based on boehmite nanometer film and preparation method thereof |
| 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 |
| 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 |
| CN108802006A (en) * | 2018-05-28 | 2018-11-13 | 宁德师范学院 | A kind of computational methods of preparation and its surface enhanced factor with SERS substrates |
| CN108823541A (en) * | 2018-06-06 | 2018-11-16 | 常州大学 | A kind of preparation method of surface-enhanced Raman scattering activity substrate |
| CN108872192A (en) * | 2018-01-30 | 2018-11-23 | 苏州天际创新纳米技术有限公司 | SERS unit and SERS system |
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2012
- 2012-03-28 CN CN2012100846764A patent/CN102590179A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| MELISSA S.SANDER,LE-SHON TAN: "Nanoparticle Arrays on Surfaces Fabricated Using Anodic Alumina Films as Templates", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| 张波: "银微纳米结构的制备及其表面增强拉曼散射性质", 《中国科学技术大学硕士学位论文》 * |
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| CN102849672A (en) * | 2012-09-17 | 2013-01-02 | 无锡英普林纳米科技有限公司 | Surface enhanced Raman micro-structural substrate and preparation method thereof |
| CN102998297A (en) * | 2012-12-11 | 2013-03-27 | 东南大学 | Porous microscale reaction plate for surface enhanced Raman scattering spectrum analysis |
| CN103257132A (en) * | 2013-04-16 | 2013-08-21 | 上海大学 | Silver nanoparticle cap array surface-enhanced raman activity substrate and preparation method thereof |
| CN103257132B (en) * | 2013-04-16 | 2015-03-25 | 上海大学 | Silver nanoparticle cap array surface-enhanced Raman activity substrate and preparation method thereof |
| CN103526288B (en) * | 2013-10-10 | 2016-08-24 | 宋玉军 | The method of interface interaction induction self assembly high density nano-array |
| CN103526288A (en) * | 2013-10-10 | 2014-01-22 | 宋玉军 | Method for interface effect induced self-assembly of high-density nano array |
| CN104568896A (en) * | 2013-10-23 | 2015-04-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Surface enhanced Raman scattering sensor and preparation method thereof |
| CN104630772A (en) * | 2013-11-12 | 2015-05-20 | 中国科学院物理研究所 | Multilayer stacked metal nanosphere array and preparation method thereof |
| 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 |
| CN104949957A (en) * | 2015-04-07 | 2015-09-30 | 上海大学 | Embedded type nano dot array surface enhanced Raman active substrate and preparation method thereof |
| CN105158228B (en) * | 2015-07-30 | 2018-07-20 | 西北大学 | SERS substrates and preparation method based on boehmite nano thin-film |
| CN105158228A (en) * | 2015-07-30 | 2015-12-16 | 西北大学 | SERS (Surface enhanced Raman Scattering) substrate based on boehmite nanometer film 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 |
| 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 |
| 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 |
| CN108872192A (en) * | 2018-01-30 | 2018-11-23 | 苏州天际创新纳米技术有限公司 | SERS unit and SERS system |
| CN108872192B (en) * | 2018-01-30 | 2024-01-12 | 苏州纳微生命科技有限公司 | SERS unit and SERS system |
| CN108802006A (en) * | 2018-05-28 | 2018-11-13 | 宁德师范学院 | A kind of computational methods of preparation and its surface enhanced factor with SERS substrates |
| CN108823541A (en) * | 2018-06-06 | 2018-11-16 | 常州大学 | A kind of preparation method of surface-enhanced Raman scattering activity substrate |
| CN108823541B (en) * | 2018-06-06 | 2022-02-15 | 常州大学 | Preparation method of surface-enhanced Raman scattering active substrate |
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Application publication date: 20120718 |