CN102621126A - Metal nanodot array surface enhancing Raman active base and preparation method thereof - Google Patents
Metal nanodot array surface enhancing Raman active base and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a metal nanodot array surface enhancing Raman active base and a preparation method thereof. The base takes silicon single crystals as the substrate, and metal nano particles forming an array structure are deposited on the surface of silicon; and further, the particle sizes of the metal nano particles range from 16 to 85nm, and the center distances of the particles range from 99 to 111nm. The metal nanodot array surface enhancing Raman active base provided by the invention is uniform in morphology, is controllable in structure, has a remarkable surface Raman enhancing effect on analytes of different concentration, and has a uniform and stable enhancing signal. Through the method provided by the invention, structural parameters and morphology of the metal nanodot array can be adjusted according to structural parameter of an ultrathin aluminum oxide template, and different influences on the Raman surface enhancing effect by different metal nanodot array bases can be realized; and further, the base and method have the advantages of simplicity for operation, low cost and easiness for industrial production.
Description
Technical field
The present invention relates to a kind of gold nano dot matrix surface reinforced Raman active substrate and preparation method thereof; Particularly a kind of gold 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
(Surface enhanced Raman spectroscopy SERS) is a kind of research molecular surface and interactional highly sensitive real non-destructive detection technique thereof to SERS.The SERS technology has overcome the shortcoming of normal raman spectroscopy technology muting sensitivity; Can provide molecular structure information; Infer the absorption orientation of molecule, have a wide range of applications in the field of biological, chemistry, medical application and environmental monitoring at substrate surface.The signal of SERS and substrate have relation very closely; The activity of SERS substrate directly affects the surface raman enhancement effect, is one of its key issue and research focus and how to prepare at the bottom of the SERS active group of high sensitivity, good reproducibility, height stable homogeneous.
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, but the surfaceness that provides at the bottom of these self assembly active groups is difficult to control, thereby has 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, be badly in need of a kind of high efficient and flexible of exploitation, low cost, can prepare high sensitivity, can repeat, the method for the nanostructured SERS substrate of the large tracts of land of stable homogeneous, controllable structure.
Recently, novel UTAM (Ultra-Thin Alumina Mask, ultrathin alumina template) nano surface technology of preparing provides the method for the surface nano-structure 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 gold 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 gold 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 gold nano dot matrix surface reinforced Raman active is characterized in that this substrate is substrate with the silicon single crystal, at silicon face deposited gold nanoparticle array structure; The particle diameter of described gold nano grain is 16～85 nm, and particle centre distance is 99～111 nm.
A kind of method for preparing above-mentioned gold nano dot matrix surface reinforced Raman active substrate is characterized in that the concrete steps of this method are:
A. ultrathin alumina template (UTAM) preparation;
The b.UTAM aperture adjustment;
C.UTAM transfers on the Si substrate;
D. the preparation of metal nano dot matrix surface reinforced Raman active substrate:, be 8 * 10 in vacuum tightness with step ability c gained UTAM/Si sample
-4Pa, voltage 90 V, under evaporation rate 0.3～0.5 nm/s condition, evaporation bronze 100～200 s; Remove UTAM then, obtain the substrate of gold 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 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.
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 45～60 min, 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 the three-dimensional AFM figure of the UTAM of different reaming times, and insertion figure is the planimetric map of UTAM, and wherein the reaming time is: (a) 45 min; (b) 50 min; (c) 55 min; (d) 60 min, corresponding UTAM aperture is: (a) 28 nm; (b) 42 nm; (c) 63 nm; (d) 85 nm.Particle centre distance is 105 ± 6 nm.
Fig. 2 is the SEM figure that has removed part UTAM in the UTAM sample of thermal evaporation deposition Au.
Fig. 3 is the SEM figure of surface reinforced Raman active substrate of the Au nano-dot matrix of large tracts of land high-sequential variable grain diameter, wherein (a) 16 nm; (b) 20 nm; (c) 35 nm; (d) 43 nm; (e) 50 nm; (f) 55 nm; (g) 67 nm; (h) 77 nm.
Fig. 4 j) is concentration 1 * 10
-6The R6G of M is the surface raman enhancement spectrum of probe molecule, wherein sample corresponding (a) 16 nm of the curve of spectrum and Fig. 2; (b) 20 nm; (c) 35 nm; (d) 43 nm; (e) 50 nm; (f) 55 nm; (g) 67 nm; (h) 77 nm.K) R6G spectrum is at 1362 cm
-1The enhancer sample pairing of characteristic peak with it
Fig. 5 is a concentration 3 * 10
-3The 4-MPy of M is the surface raman enhancement spectrum of probe molecule, and wherein the diameter of the pairing Au nano-dot matrix of curve of spectrum particle is respectively (a) 20nm; (b) 35nm; (c) 40 nm; (d) 50 nm; (e) 60 nm; (f) 65 nm.Particle centre distance is 105 ± 6 nm.
Fig. 6 is a concentration 3 * 10
-3The 4-MPy of M is the surface raman enhancement spectrum of probe molecule, and test diameter is the homogeneity of signal of the Au dot matrix sample of 50 nm, adopts 25 test SERS spectrum at random at sample surfaces.
Embodiment
Embodiment one: present embodiment is mask with UTAM, in the Si substrate, prepares Au nano particle dot matrix large-area ordered, homogeneous, and with 1 * 10
-6(rhodamine 6G is R6G) with 3 * 10 for the rhodamine of M
-3(4-mercaptopyridine 4-MPy) as probe molecule, carries out the test of surperficial Raman spectrum to the 4-mercaptopyridine of M.Detailed process is following:
1) preparation of large-area ordered UTAM:
A. the pre-service of aluminium flake: acetone ultrasonic cleaning 30 min, the CVD high annealing, 450～550 ℃ of nitrogen protections in the mixed liquor of the ethanol of 0 ℃ of temperature and perchloric acid, are carried out electrochemical polish under constant current (750 mA) condition.
B. anodic oxidation: utilizing homemade anodic oxidation device, is electrolyte with 0.3 M oxalic acid solution, and two-step approach prepares UTAM under constant voltage 40 V.Earlier aluminium flake is carried out the anodized first time, placing it in temperature then is 60 ℃, soaks appropriate time in the mixed liquor of massfraction 6% phosphoric acid and 1.8% chromic acid, the alumina layer that forms when removing oxidation for the first time; With the identical electrolytic condition of the anodic oxidation first time under, carry out second time anodization again and can form order UTAM preferably.
C. the removal of unreacted aluminium substrate: use CuCl
2With the mixed liquor of HCl, unoxidized aluminium substrate is dissolved away fully, to obtain purer UTAM.
D. UTAM aperture adjustment: big or small with adjustment aperture in order to remove the thicker barrier layer in bottom; There is the UTAM sample barrier layer of photoresist to swim in 30 ℃ of constant temperature down with top; In massfraction 5% dilute phosphoric acid solution; Regulate the reaming time according to the experiment needs, obtain the UTAM in different apertures, as shown in Figure 1.
E. the transfer of UTAM and moulding: transferring in the Si substrate through the UTAM that obtains after the reaming.
2) preparation of the Au nano-dot matrix of large tracts of land high-sequential, controllable structure:
The UTAM for preparing with step 1) evaporates mask as metal fever; Utilize vacuum electron beam coating machine thermal resistance vapor deposition, vaporization voltage 90 V, evaporation current 104 A; Under evaporation rate 0.3 ~ 0.5 nm/s condition; Evaporate the thickness of 50 nm, remove at last after the suprabasil UTAM, can obtain the surface reinforced Raman active substrate of the Au nano-dot matrix of large tracts of land high-sequential, controllable structure based on the Si substrate.Fig. 2 removes the Au dot matrix SEM figure of half UTAM for after depositing Au.Can see of the structural growth arrangement of dot matrix particle, prove that the height of Au nano-dot matrix structural parameters is controlled, adjustable in strict accordance with UTAM.Fig. 3 is the same thickness of deposition on the UTAM of different reaming time, behind the removal UTAM, and the SEM figure of dot matrix particle diameter different samples.
3) utilize step 2) carry out SERS test at the bottom of the active group of preparation:
Select 1 * 10 for use
-6(rhodamine 6G is R6G) with 3 * 10 for the rhodamine of M
-3(4-mercaptopyridine 4-MPy) as probe molecule, carries out the test of surperficial Raman spectrum to the substrate of the Au nano particle dot matrix of controllable structure to the 4-mercaptopyridine of M.During sample measurement, employing be Renishaw inVia plus laser capture microdissection Raman spectrometer, 50 double-lengths are apart from object lens; When probe molecule is rhodamine (rhodamine 6G; R6G) time, adopting LASER Light Source is 514 nm excitation wavelengths, when probe molecule is 4-mercaptopyridine (4-mercaptopyridine; In the time of 4-MPy), excitation source is 785 nm excitation wavelengths.Fig. 4 j is the Raman spectrum of the Au nano-dot matrix substrate of variable grain diameter, is probe molecule with R6G, and concentration is 1 * 10
-6M, wherein sample corresponding (a) 16 nm among the curve of spectrum and Fig. 2; (b) 20 nm; (c) 35 nm; (d) 43 nm; (e) 50 nm; (f) 55 nm; (g) 67 nm; (h) 77 nm.Can obtain from Fig. 4 j, when the diameter of dot matrix particle when 16nm increases to 55 nm gradually, the diffraction peak intensity of Raman spectrum increases gradually, with 1362 cm
-1, 1507 cm
-1, 1649 cm
-1The diffraction peak at place is represented the characteristic peak of R6G, and when sample diameter was 55 nm, reinforced effects was the most obvious; But along with sample dot matrix particle diameter continues to increase 1362 cm
-1, 1507 cm
-1, 1649 cm
-1Instead the reinforced effects of the diffraction peak at place has reduced.According to enhancer (enhancement factor) computing formula EF=
I SERS C Raman / I Raman C SERS , wherein
I SERS With
I Raman Correspond respectively to the intensity of Raman peaks in SERS spectrum and the conventional Raman spectrum of molecule,
C SERS With
C Raman The concentration of used R6G molecule when being respectively test SERS and conventional Raman spectrum.With 1362 cm
-1The raman characteristic peak at place is a foundation, calculates the enhancer of different sample substrate, and wherein diameter is that the enhancer of the Au nano-dot matrix of 55 nm is 7.4 * 10 to the maximum
7, and other samples in the enhancer of this characteristic peak shown in Fig. 4 k.
Fig. 5 is a concentration 3 * 10
-3The 4-MPy of M is the surface raman enhancement spectrum of probe molecule, and wherein the diameter of the pairing Au nano-dot matrix of curve of spectrum particle is respectively (a) 20 nm; (b) 35 nm; (c) 40 nm; (d) 50 nm; (e) 60 nm; (f) 65 nm.The surface raman enhancement spectral signal variation that can obtain 4-MPy from Fig. 5 equally is relevant with the sample diameter variation, with 938 cm
-1, 999 cm
-1, 1092 cm
-1The diffraction peak at place is represented the characteristic peak of 4-MPy, and when the diameter of sample dot matrix was 50 nm, the reinforced effects of diffraction peak was the most obvious.For the signal conformance of specimen, at diameter random acquisition 25 points on the sample of 50 nm, with 3 * 10
-3The 4-MPy of M is a probe molecule, obtains 25 spectroscopic datas under the 785 nm excitation wavelengths, and is as shown in Figure 6.The chart that wherein embeds is that 25 spectroscopic datas are at 938 cm
-1, 999 cm
-1, 1092 cm
-1The diffraction peak at place strengthens the standard difference of intensity, and its standard deviation is respectively 5.7 %, 6.2 %, 4.4 %.
Substrate surface Raman signal in conjunction with Fig. 4-6 explanation the present invention preparation strengthens significantly, and the signal stable homogeneous, can be used for the detection of trace compound.
Claims (5)
1. gold nano dot matrix surface reinforced Raman active substrate is characterized in that this substrate is substrate with the silicon single crystal, at silicon face deposited gold nanoparticle array structure; The particle diameter of described gold nano grain is 16～85 nm, and particle centre distance is 99～111 nm.
2. method for preparing gold nano dot matrix surface reinforced Raman active according to claim 1 substrate is characterized in that the concrete steps of this method are:
A. ultrathin alumina template UTAM preparation;
The b.UTAM aperture adjustment;
C.UTAM transfers on the Si substrate;
D. the preparation of metal nano dot matrix surface reinforced Raman active substrate:, be 8 * 10 in vacuum tightness with step ability c gained UTAM/Si sample
-4Pa, voltage 90 V, under evaporation rate 0.3～0.5 nm/s condition, evaporation bronze 100～200 s; Remove UTAM then, obtain the substrate of gold nano dot matrix surface reinforced Raman active.
3. method according to claim 2; It is characterized in that the concrete steps that prepare described ultrathin alumina template (UTAM) are: the pre-service of a_1. 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 that the reaming time is 45～60 min, obtains the UTAM in different apertures in 5% the dilute phosphoric acid solution.
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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