CN104634772A - Method for preparing surface-enhanced Raman spectrum substrate and substrate prepared by using method - Google Patents
Method for preparing surface-enhanced Raman spectrum substrate and substrate prepared by using method Download PDFInfo
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- CN104634772A CN104634772A CN201510069685.XA CN201510069685A CN104634772A CN 104634772 A CN104634772 A CN 104634772A CN 201510069685 A CN201510069685 A CN 201510069685A CN 104634772 A CN104634772 A CN 104634772A
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Abstract
The invention provides a method for preparing a surface-enhanced Raman spectrum substrate. The method comprises the following steps: preparing a substrate layer; forming an adhesion layer on the substrate layer by virtue of evaporation plating or sputtering; forming a metal thin film layer on the adhesion layer by virtue of evaporation plating or sputtering; forming an insulating layer on the metal thin film layer by virtue of evaporation plating or sputtering or chemical vapor deposition or thin film wet-process transfer; forming a metal nano-structure array layer on the insulating layer by virtue of X-ray interference lithography, wherein the X-ray interference lithography comprises photoresist spin-coating; evaporating moisture in a photoresist at 120-180 DEG C; performing X-ray interference exposure; performing development by using a developing solution; curing the developed photoresist; depositing the metal thin film layer on the surface of an ordered nanostructure; and removing excess metals and photoresists. The invention also relates to a surface-enhanced Raman spectrum substrate comprising the substrate layer, the adhesion layer, the metal thin film layer, the insulating layer and the metal nano-structure array layer. The surface-enhanced Raman spectrum substrate prepared by using the method disclosed by the invention has both good sensitivity and stability.
Description
Technical field
The present invention relates to Surface enhanced raman spectroscopy technical field, relate more specifically to a kind of method and the substrate thereof of preparing Raman spectrum base.
Background technology
Raman spectrum is used to a kind of spectrographic technique studying effective molecular vibration, is a kind of important molecular spectroscopy techniques.According to different material molecule because their chemical compositions shown Raman spectrum characteristic different from structure is different, researchist then can be obtained the information of molecule by Raman spectrum, carries out differentiating and detects different material.Raman scattering is a kind of inelastic scattering, much more weak than Rayleigh intensity of its intensity, and thus conventional Raman spectrum is very insensitive when amalyzing substances valence state and composition.
Surface enhanced raman spectroscopy (surface enhanced raman scattering, SERS) technology can realize the detection of single molecules level simultaneously and provide the finger print information of molecule, can be used to amalyzing substances composition.In Surface enhanced raman spectroscopy technology, the analysis that laser wavelength of incidence, excitation intensity and SERS substrate effects on surface strengthen Raman spectrum is three vital factors; The very big enhancing of Raman scattering observed in an experiment mainly strengthens from the local electric field of metallic nanostructured surface, and secondly, Raman strengthens also by the impact that the particular electrical sub-resonance of raman active molecule directly contacts with metal surface with them.Therefore, the performance and preparation method thereof of SERS substrate seems most important.
The successively decreasing of distance of enhancing intensity two metallicss of SERS substrate exponentially increases.In the past in more than 30 year, strengthen signal for obtaining desirable SERS, people have studied the regulating and controlling effect of nanostructureds different in SERS substrate, and prepare the metal Nano structure array of compound with regular structure by multiple method.Mainly be included in prior art by self assembly beamwriter lithography on substrate layer, focused ion beam lithography and nano impression prepare the metal Nano structure array layer of compound with regular structure, obtain the SERS substrate with double-layer structure.But in SERS application process, interparticle distance even needs the rank reaching atomic layer, the needs that unimolecule SERS detects can be met.The resolution of the SERS substrate obtained by said method is subject to the restriction of photoetching.The SERS substrate strength utilizing photoetching technique to prepare like this does not reach and strengthens to greatest extent, and sensitivity still cannot meet actual unimolecule SERS and detect, and can not provide good sensitivity and stability simultaneously.
Summary of the invention
In order to solve above-mentioned prior art exist good sensitivity and the problem of stability cannot be provided simultaneously, the present invention aims to provide a kind of method and the substrate thereof of preparing Raman spectrum base.
The invention provides a kind of method preparing Raman spectrum base, comprise the following steps: S1, substrate layer is provided; S2, described substrate layer forms adhesion layer by evaporation or sputtering; S3, described adhesion layer forms metal film layer by evaporation or sputtering; S4, described metal film layer forms insulation course by evaporation or sputtering or chemical vapor deposition or the transfer of film wet method; S5, described insulation course forms metal Nano structure array layer by X ray interference lithography; Wherein, described step S5 comprises following sub-step: S51, spin coating photoresist on described insulation course; S52, evaporates moisture in described photoresist to improve the sensitivity of described photoresist at 120-180 DEG C; S53, X ray interferes exposure with the surface forming ordered nano-structure on the insulating layer; S54, removes the part that described photoresist is exposed with developing liquid developing; S55, the photoresist after solidification development, improves graphics resolution; S56, at the surface deposition metal film layer of ordered nano-structure; And S57, remove unnecessary metal and photoresist, thus form metal Nano structure array layer.
In described step S1, substrate bombards to remove substrate surface organism by oxygen gas plasma and forms described substrate layer.
Described substrate carries out surface clean with ultrasound wave, then bombards with oxygen gas plasma after the drying.
Described ultrasonic frequency is 20 ~ 50Hz, and oxygen flow is 1 ~ 25sccm, and plasma power is 30 ~ 100W.
Described step S5 comprises following sub-step: S51, spin coating photoresist on described insulation course; S52, evaporates moisture in described photoresist to improve the sensitivity of described photoresist at 120-180 DEG C; S53, X ray interferes exposure with the surface forming ordered nano-structure on the insulating layer; S54, removes the part that described photoresist is exposed with developing liquid developing; S55, the photoresist after solidification development, improves graphics resolution; And S56, at the surface deposition metal film layer of ordered nano-structure, thus form metal Nano structure array layer.
Described photoresist is polymethylmethacrylate or hydrogen silsesquioxane.
Described evaporation is hot evaporation, or described in be sputtered to magnetron sputtering, electronics sputtering or ion sputtering.
The invention provides a kind of Raman spectrum base, comprise the substrate layer, adhesion layer, metal film layer, insulation course and the metal Nano structure array layer that set gradually.
The material of described adhesion layer is chromium or titanium.
The material of described metal film layer is gold, silver or copper.
The material of described insulation course is silicon dioxide, titania or aluminium oxide.
The material of described metal Nano structure array layer is gold, silver or copper.
The material of described substrate layer is monocrystalline silicon, polysilicon, silicon dioxide or glass.
According to the method preparing Raman spectrum base of the present invention, metal Nano structure array layer is formed by X ray interference lithography, can not there is agglomeration in the metallics in this metal Nano structure array layer, have very high repeatability, and performance is also more stable, simultaneously, the Raman spectrum base obtained by the method has the structure of substrate layer-adhesion layer-metal film layer-insulator-metal nano-structure array layer, the metal film layer being positioned at insulation course both sides wherein and metal Nano structure array layer interact, make the nano metal particles interaction in the horizontal direction of light induced surface electric field, produce SERS to strengthen, nano metal particles subarray and metallic film also can produce greatly SERS enhancing in vertical direction simultaneously, its spacing is determined by the thickness of insulation course, so just breach the resolution restriction of photoetching.Simultaneously due to large area and the homogeneity of film, prepared according to the methods of the invention Raman spectrum base possesses good sensitivity and stability simultaneously.In addition, X ray interference photoetching technology is parallel exposure process, and it also has high yield that can be practical.And, due to X ray interference photoetching technology cycle, shape, size, density is all adjustable, therefore Raman spectrum base according to the present invention has good adjustability.Raman spectrum base of the present invention has better sensitivity, repeatability, adjustability simultaneously, stability, large area, the advantages such as high yield, for the basis of compacting has been laid in the correlative study of SERS technology and widespread use.
Accompanying drawing explanation
Fig. 1 is according to the process chart preparing the method for Raman spectrum base of the present invention;
Fig. 2 is according to the process chart being formed metal Nano structure array layer method by X ray interference lithography of the present invention;
Fig. 3 is the schematic diagram according to Raman spectrum base of the present invention;
Fig. 4 is the result schematic diagram that Raman spectrum base according to first embodiment of the invention detects the R6G ethanolic solution of variable concentrations;
Fig. 5 is that Raman spectrum base according to first embodiment of the invention and ordinary silicon substrate detect 10
-7the comparing result schematic diagram of the R6G ethanolic solution of M;
Fig. 6 is to 10 according to the Raman spectrum base of second embodiment of the present invention
-7the R6G of the concentration of M is at the Raman signal information schematic diagram of 50 arbitrary zones of different points; And
Fig. 7 is to 10 according to the Raman spectrum base of the 3rd embodiment of the present invention
-7the R6G of the concentration of M is at the Raman signal information schematic diagram of 10 arbitrary zones of different points.
Embodiment
Below in conjunction with accompanying drawing, provide preferred embodiment of the present invention, and be described in detail.
As shown in Figure 1, according to the method preparing Raman spectrum base of the present invention, comprise the following steps: S1, substrate layer is provided, preferably, substrate carries out surface clean with ultrasound wave (ultrasonic frequency is for 20 ~ 50Hz), then uses oxygen (oxygen flow is 1 ~ 25sccm) plasma (plasma power is 30 ~ 100W) to bombard after the drying; S2, described substrate layer forms adhesion layer by evaporation (such as hot evaporation) or sputtering (such as magnetron sputtering, electronics sputtering or ion sputtering); S3, described adhesion layer forms metal film layer by evaporation (such as hot evaporation) or sputtering (such as magnetron sputtering, electronics sputtering or ion sputtering); S4, described metal film layer passes through evaporation (such as hot evaporation) or sputters (such as magnetron sputtering, electronics sputtering or ion sputtering) or chemical vapor deposition or the transfer of film wet method to form insulation course; S5, described insulation course forms metal Nano structure array layer by X ray interference lithography.Wherein, step S5 comprises following sub-step, as shown in Figure 2: S51, and spin coating photoresist (such as polymethylmethacrylate or hydrogen silsesquioxane) on described insulation course; S52, at 120-180 DEG C, evaporate moisture in described photoresist to improve the sensitivity of described photoresist, the evaporation process of this temperature range does not affect follow-up exposure; S53, X ray interferes exposure with the surface forming ordered nano-structure on the insulating layer; S54, removes the part that described photoresist is exposed with developing liquid developing; S55, the photoresist after solidification development, improves graphics resolution; S56, at the surface deposition metal film layer of ordered nano-structure, and S57, remove unnecessary metal and photoresist, thus form metal Nano structure array layer, preferably put into acetone and anhydrous alcohol is ultrasonic peels off, then can carry out drying more in a nitrogen environment and form metal Nano structure array layer.
As shown in Figure 3, the Raman spectrum base that said method according to the present invention obtains comprises substrate layer 1, adhesion layer 2, metal film layer 3, insulation course 4 and metal Nano structure array layer 5.Wherein, adhesion layer 2 is formed on substrate layer 1, and metal film layer 3 is formed on adhesion layer 2, and insulation course 4 is formed on metal film layer 3, and metal Nano structure array layer 5 is formed on insulation course 4.Wherein, the material of substrate layer 1 is monocrystalline silicon, polysilicon, silicon dioxide or glass, the material of adhesion layer 2 is chromium or titanium, the material of metal film layer 3 is gold, silver or copper, the material of insulation course 4 is silicon dioxide, titania or aluminium oxide, and the material of metal Nano structure array layer 5 is gold, silver or copper.
Embodiment 1
The silicon chip of 2 inches is put into acetone and anhydrous alcohol successively, and carry out surface clean (ultrasonic frequency is for 50Hz) with ultrasound wave, with oxygen gas plasma bombardment (oxygen flow is 15sccm) after oven dry, plasma power is 100W, removes substrate surface organism as substrate layer 1;
Utilize the chromium of electron-beam vapor deposition method evaporation 2nm thickness on substrate layer 1 as adhesion layer 2, pressure is 1 × 10
-7torr, power is 145W, and rate of sedimentation is 0.04nm/s;
Utilize electron-beam vapor deposition method on adhesion layer 2, to deposit the gold thin film of 50nm thickness as metal film layer 3, pressure is 1 × 10
-7torr, power is 115W, and rate of sedimentation is 0.12nm/s;
Utilize magnetron sputtering method on metal film layer 3, deposit the SiO of 10nm thickness
2as insulation course 4, pressure is 5 × 10
-3torr, power is 150W, and rate of sedimentation is 0.01nm/s;
X ray interference photoetching technology is utilized to make metal Nano structure array layer 5:(1 respectively on insulation course 4 He in silicon base) spin coating photoresist on described insulation course: drip photoresist polymethylmethacrylate (PMMA), and rotate with the rotating speed of 4000rpm/min, make photoresist be evenly distributed on insulation course upper surface; (2) front baking: with 180 DEG C of heating 90s, the moisture in evaporation photoresist, improves the sensitivity of photoresist; (3) X ray interferes exposure, selects the grating of figure full symmetric as beam splitting, interferes superposition element, with x-ray bombardment, produce interference fringe on a photoresist, form the surface of ordered nano-structure on the insulating layer; (4) develop: remove the part that photoresist is exposed with developing liquid developing, the developer solution used is the cooperation mixed solution of methyl isobutyl ketone/isopropyl alcohol (MIBK/IPA)=1:3, development time is 45s, and then clean substrate layer with ultrapure water, dry up by nitrogen gun again after cleaning 3 times; (5) dry afterwards: with 100 DEG C of heating 30s, the photoresist after curing exposure, improves graphics resolution; (6) gold of electron beam evaporation evaporation 8nm thickness: put into filming equipment, adjustment parameter, pressure is 1 × 10
-7torr, power is 115W, and rate of sedimentation is 0.12nm/s; (7) peel off: put into acetone and anhydrous alcohol is ultrasonic to remove unnecessary metal and photoresist, dry in a nitrogen environment, finally obtain Raman spectrum base of the present invention.
The SERS substrate using this legal system standby detects rhodamine 6G (R6G) ethanolic solution of variable concentrations, and as shown in Figure 4, SERS substrate of the present invention is to variable concentrations (10 for result
-6m, 10
-7m, 10
-8m, 10
-9m) R6G solution has very strong Raman signal, and detection limit is 10
-10m.
Identical nano metal particles subarray is prepared in silicon base and adhesion layer-metal film layer-insulation course substrate of the present invention to Fig. 5.Detecting concentration is 10
-7m.Adhesion layer-metal film layer-insulation course substrate is at 1367cm as seen from Figure 5
-1the Raman signal that place records is on a silicon substrate 12 times.Adhesion layer-metal film layer-insulation course substrate makes the nano metal particles interaction in the horizontal direction of light induced surface electric field, produces SERS and strengthens, and nano metal particles subarray and metallic film also create greatly SERS enhancing in vertical direction simultaneously.
Embodiment 2
The silicon chip of 2 inches is put into acetone and anhydrous alcohol successively, and carry out surface clean (ultrasonic frequency is for 50Hz) with ultrasound wave, with oxygen gas plasma bombardment (oxygen flow is 10sccm) after oven dry, plasma power is 30W, removes substrate surface organism as substrate layer 1;
Utilize the titanium of magnetron sputtering method evaporation 2nm thickness on substrate layer 1 as adhesion layer 2, pressure is 5 × 10
-2torr, power is 100W, and rate of sedimentation is 0.24nm/s;
Utilize magnetron sputtering method on adhesion layer 2, to deposit the Ag films of 50nm thickness as metal film layer 3, pressure is 2.5 × 10
-3torr, power is 100W, and rate of sedimentation is 0.42nm/s;
Utilize chemical vapour deposition technique on metal film layer 3, deposit the TiO of 1.8nm thickness
2as insulation course 4, temperature is 150 DEG C, and flow is 20sccm, and the time is 30 minutes, and rate of sedimentation is 0.001nm/s;
Utilize X ray interference photoetching technology on insulation course 4, make metal Nano structure array layer 5:(1) spin coating photoresist on described insulation course: drip photoresist polymethylmethacrylate (PMMA), and rotate with the rotating speed of 4000rpm/min, make photoresist be evenly distributed on insulation course upper surface; (2) front baking: with 180 DEG C of heating 90s, the moisture in evaporation photoresist, improves the sensitivity of photoresist; (3) X ray interferes exposure, selects the grating of figure full symmetric as beam splitting, interferes superposition element, with x-ray bombardment, produce interference fringe on a photoresist, form the surface of ordered nano-structure on the insulating layer; (4) develop: remove the part that photoresist is exposed with developing liquid developing, the developer solution used is the cooperation mixed solution of methyl isobutyl ketone/isopropyl alcohol (MIBK/IPA)=1:3, development time is 45s, and then clean substrate layer with ultrapure water, dry up by nitrogen gun again after cleaning 3 times; (5) dry afterwards: with 100 DEG C of heating 30s, the photoresist after curing exposure, improves graphics resolution; (6) gold of electron beam evaporation evaporation 8nm thickness: put into filming equipment, adjustment parameter, pressure is 1 × 10
-7torr, power is 115W, and rate of sedimentation is 0.12nm/s; (7) peel off: put into acetone and anhydrous alcohol is ultrasonic to remove unnecessary metal and photoresist, dry in a nitrogen environment, finally obtain Raman spectrum base of the present invention.
The SERS substrate using this legal system standby is to 10
-7the concentration R6G of M in the Raman signal information of 50 arbitrary zones of different points as Fig. 6, from in figure, the SERS substrate of preparing itself has good SERS repeatability as surface Raman enhancement substrate, the main 1367cm of R6G in suprabasil Raman signal
-1the standard deviation of the intensity of peak position is less than 10%, illustrates that it has very high repeatability.
Embodiment 3
The silicon chip of 2 inches is put into acetone and anhydrous alcohol successively, and carry out surface clean (ultrasonic frequency is for 50Hz) with ultrasound wave, with oxygen gas plasma bombardment (oxygen flow is 10sccm) after oven dry, plasma power is 50W, removes substrate surface organism as substrate layer 1;
Utilize the chromium of electron-beam vapor deposition method evaporation 2nm thickness on substrate layer 1 as adhesion layer 2, pressure is 1 × 10
-7torr, power is 145W, and rate of sedimentation is 0.14nm/s;
Utilize electron-beam vapor deposition method on adhesion layer 2, to deposit the gold thin film of 100nm thickness as metal film layer 3, pressure is 1 × 10
-7torr, power is 115W, and rate of sedimentation is 0.14nm/s;
Film wet method transfer method deposited graphite alkene on metal film layer 3 is utilized as insulation course 4, to comprise the PMMA of (1) graphenic surface spin coating one deck 200nm as protective seam; (2) Graphene immerses ferric chloride solution 8 hours, and concentration is 0.4M; (3) Graphene pulled out and put into deionized water cleaning three times; (4) Graphene is transferred in substrate; (5) acetone is put in substrate and Graphene, remove PMMA, temperature is 80 DEG C;
Utilize X ray interference photoetching technology on insulation course 4, make metal Nano structure array layer 5:(1) spin coating photoresist on described insulation course: drip photoresist polymethylmethacrylate (PMMA), and rotate with the rotating speed of 4000rpm/min, make photoresist be evenly distributed on insulation course upper surface; (2) front baking: with 180 DEG C of heating 90s, the moisture in evaporation photoresist, improves the sensitivity of photoresist; (3) X ray interferes exposure, selects the grating of figure full symmetric as beam splitting, interferes superposition element, with x-ray bombardment, produce interference fringe on a photoresist, form the surface of ordered nano-structure on the insulating layer; (4) develop: remove the part that photoresist is exposed with developing liquid developing, the developer solution used is the cooperation mixed solution of methyl isobutyl ketone/isopropyl alcohol (MIBK/IPA)=1:3, development time is 45s, and then clean substrate layer with ultrapure water, dry up by nitrogen gun again after cleaning 3 times; (5) dry afterwards: with 100 DEG C of heating 30s, the photoresist after curing exposure, improves graphics resolution; (6) gold of electron beam evaporation evaporation 8nm thickness: put into filming equipment, adjustment parameter, pressure is 1 × 10
-7torr, power is 115W, and rate of sedimentation is 0.12nm/s; (7) peel off: put into acetone and anhydrous alcohol is ultrasonic to remove unnecessary metal and photoresist, dry in a nitrogen environment, finally obtain Raman spectrum base of the present invention.
The SERS that the method is prepared strengthens substrate and reuses ten times, at every turn to 10
-7m concentration R6G is at 1367cm
-1the Raman signal information at place is as Fig. 7, and from figure, the SERS substrate of preparing itself has good SERS repeatability as surface Raman enhancement substrate, the main 1367cm of R6G in suprabasil Raman signal
-1the standard deviation of the intensity of peak position is less than 10%, illustrates that it has very high repeatability.
According to the method preparing Raman spectrum base of the present invention, metal Nano structure array layer is formed by X ray interference lithography, can not there is agglomeration in the metallics in this metal Nano structure array layer, have very high repeatability, and performance is also more stable; Simultaneously, the Raman spectrum base obtained by the method has the structure of substrate layer-adhesion layer-metal film layer-insulator-metal nano-structure array layer, the metal film layer being positioned at insulation course both sides wherein and metal Nano structure array layer interact, make light induced surface electric field can produce high enhancing in horizontal and vertical two directions, and then greatly improve the detection sensitivity of SERS substrate, so, prepared according to the methods of the invention Raman spectrum base possesses good sensitivity and stability simultaneously.In addition, X ray interference photoetching technology is parallel exposure process, and it also has high yield that can be practical.And, due to X ray interference photoetching technology cycle, shape, size, density is all adjustable, therefore Raman spectrum base according to the present invention has good adjustability.Raman spectrum base of the present invention has better sensitivity, repeatability, adjustability simultaneously, stability, large area, the advantages such as high yield, for the basis of compacting has been laid in the correlative study of SERS technology and widespread use.
Above-described, be only preferred embodiment of the present invention, and be not used to limit scope of the present invention, the above embodiment of the present invention can also make a variety of changes.Namely every claims according to the present patent application and description are done simple, equivalence change and modify, and all fall into the claims of patent of the present invention.The not detailed description of the present invention be routine techniques content.
Claims (12)
1. prepare a method for Raman spectrum base, it is characterized in that, comprise the following steps:
S1, provides substrate layer;
S2, described substrate layer forms adhesion layer by evaporation or sputtering;
S3, described adhesion layer forms metal film layer by evaporation or sputtering;
S4, described metal film layer forms insulation course by evaporation or sputtering or chemical vapor deposition or the transfer of film wet method; And
S5, described insulation course forms metal Nano structure array by X ray interference lithography;
Wherein, described step S5 comprises following sub-step:
S51, spin coating photoresist on described insulation course;
S52, evaporates moisture in described photoresist to improve the sensitivity of described photoresist at 120-180 DEG C;
S53, X ray interferes exposure with the surface forming ordered nano-structure on the insulating layer;
S54, removes the part that described photoresist is exposed with developing liquid developing;
S55, the photoresist after solidification development, improves graphics resolution;
S56, at the surface deposition metal film layer of ordered nano-structure; And
S57, removes unnecessary metal and photoresist, thus forms metal Nano structure array layer.
2. method according to claim 1, is characterized in that, in described step S1, substrate bombards to remove substrate surface organism by oxygen gas plasma and forms described substrate layer.
3. method according to claim 2, is characterized in that, described substrate carries out surface clean with ultrasound wave, then bombards with oxygen gas plasma after the drying.
4. method according to claim 3, is characterized in that, described ultrasonic frequency is 20 ~ 50Hz, and oxygen flow is 1 ~ 25sccm, and plasma power is 30 ~ 100W.
5. method according to claim 1, is characterized in that, described photoresist is polymethylmethacrylate or hydrogen silsesquioxane.
6. method according to claim 1, is characterized in that, described evaporation is hot evaporation, or described in be sputtered to magnetron sputtering, electronics sputtering or ion sputtering.
7. the Raman spectrum base prepared according to above-mentioned any one claim, it is characterized in that, described Raman spectrum base comprises the substrate layer, adhesion layer, metal film layer, insulation course and the metal Nano structure array layer that set gradually.
8. Raman spectrum base according to claim 7, is characterized in that, the material of described adhesion layer is chromium or titanium.
9. Raman spectrum base according to claim 7, is characterized in that, the material of described metal film layer is gold, silver or copper.
10. Raman spectrum base according to claim 7, is characterized in that, the material of described insulation course is silicon dioxide, titania or aluminium oxide.
11. Raman spectrum base according to claim 7, is characterized in that, the material of described metal Nano structure array layer is gold, silver or copper.
12. Raman spectrum base according to claim 7, is characterized in that, the material of described substrate layer is monocrystalline silicon, polysilicon, silicon dioxide or glass.
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