CN107966429A - A kind of Gin Nanometer globoid stacked array substrate and preparation method with Surface enhanced Raman scattering - Google Patents
A kind of Gin Nanometer globoid stacked array substrate and preparation method with Surface enhanced Raman scattering Download PDFInfo
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- CN107966429A CN107966429A CN201711389231.6A CN201711389231A CN107966429A CN 107966429 A CN107966429 A CN 107966429A CN 201711389231 A CN201711389231 A CN 201711389231A CN 107966429 A CN107966429 A CN 107966429A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/20—Exposure; Apparatus therefor
- G03F7/2051—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source
- G03F7/2053—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source using a laser
Abstract
The present invention discloses a kind of Gin Nanometer globoid stacked array substrate and preparation method with Surface enhanced Raman scattering, utilize the standing wave effect in photoetching process, that is the surface reflection of incident light base material interferes with incident light and forms a kind of given stack three-dimensional structure on a photoresist, at the same time, multi-beam laser interference photoetching technology again arranges this stacking three-dimensional structure according to specified period profile, by the gold thin film for sputtering one layer of nano thickness, form Gin Nanometer globoid stacked array, the structure has the effect of Surface enhanced Raman scattering, base material available for Raman scattering detection, so as to effectively improve the Raman signal of tested substance.
Description
Technical field
The present invention relates to a kind of Gin Nanometer globoid stacked array substrate and preparation method with Surface enhanced Raman scattering, belongs to
In nano material manufacture field.
Background technology
Raman spectrum has unique advantage, is mainly reflected in the following aspects for other spectral techniques：
(1) what Raman spectrum detected is the change of light frequency, is not directly dependent upon with excitation source wavelength, therefore can be according to test material
The suitable excitation wavelength of the selections such as the characteristics of material, fluorescent characteristic；(2) Raman spectrum is particularly suitable for biology from the influence of water
The Non-Destructive Testing of sample and on-line checking in field；(3) sample is not strict with Raman spectrum detection, it is not necessary to sample preparation,
Usually only need micro sample to meet measurement demand, a kind of trace detection means can be used as；(4) Raman of each material
Spectrum is different and does not interfere with each other, and can detect many kinds of substance at the same time by Raman spectroscopy, this has for material analysis research
Very important meaning.
But since the sensitivity of Raman spectrum is low, signal strength is weak, usually there was only the 10 of Rayleigh intensity-6-10-9, and
Easily disturbed be subject to material fluorescence, the fluorescence signal signal-to-noise ratio for reducing Raman spectrum detection overlapping with Raman signal so that
Raman spectrum is restricted.
The discovery of Surface enhanced Raman scattering (Surface-enhanced Raman scattering, SERS) phenomenon makes
Raman spectroscopy is obtained further to be developed.SERS can carry out going deep into characterization to various surfaces and interfacial structure, its band
The enhancing of 6 orders of magnitude come, drastically increases the sensitivity of molecular material discriminating, is readily detected absorption in metallic substrates
The monomolecular on surface.
Since SERS has found, the mankind are to manufacture history that the SERS history studied is also on SERS substrates.From earliest
Rough surface Ag electrodes prepared by electrochemical corrosion, finally nanofabrication technique continue to bring out, it is various based on physics, chemistry
Nanofabrication technique be prepared for the SERS substrates of a variety of nanostructure types, including the nano particle of Au and Ag, nanoscale
Shell structure, nanometer pinpoint structure, nano-pore, nanometer bubble, nanometer striped etc..
Controllable periodic plasma nanostructured mainly has two class nanofabrication techniques.One kind is lithographic technique, separately
One kind is template synthesis method.Lithographic technique mainly includes：Electron beam, ion beam, laser etching techniques and scanning probe (SPM) skill
Art.This kind of technology, can be with the extraordinary plasmon nanostructure of manufacturing cycle property, and structure size and structure type can also be into
Row very good control.But this kind of technology uses the order processing method of point-to-point, process velocity is slower, and being not suitable for production should
With.Secondth, template synthesis method.Using self assembly phenomenon, the surface nano-structure of larger area can simply and be quickly manufactured.
By synthesizing various templates, plasmon nanostructure can also have various forms, but so far, due to method
Limitation, it is difficult to control interparticle distance.
In conclusion the above method can not all meet SERS substrates large area, homogeneity and high enhancing signal at the same time
Requirement.And laser interference photolithography technology has unique advantage in these areas, can directly or indirectly manufacturing cycle property receive
Rice structure, and structural parameters are easily controllable；Different from other photoetching techniques, laser interference lithography uses parallel fabrication, once adds
Work area is larger, and processing efficiency is of a relatively high；Secondly, simple system, is relatively adapted to commercial application.
The content of the invention
The technology of the present invention solves the problems, such as：To overcome while meeting the SERS substrates of large area, homogeneity and high enhancing signal
Prepare and require, there is provided a kind of Gin Nanometer globoid stacked array substrate and preparation method with Surface enhanced Raman scattering, have nothing
The advantages that mask, exposure area is big, it is easy to accomplish prepared by large area.
The technology of the present invention solution：Obtained using the standing wave effect in photoetching process and multi-beam laser interference photoetching technology
A kind of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering is obtained, this Gin Nanometer globoid stacked array substrate is one
Kind three-dimensional structure.Due to standing wave effect, this three-dimensional structure is gold nano ring-type stacked structure in the Z-axis direction, Gin Nanometer globoid
It is stacked together according to fixed periodic distance, from the bottom to top, the diameter of Gin Nanometer globoid gradually increases, and width is gradually reduced.This
Kind three-dimensional structure in X-Y axis, can form different shapes, different cycles by multi-beam laser interference photoetching technology
The array structure of distribution.This Gin Nanometer globoid stacked array substrate has good Surface enhanced Raman scattering effect.
The principle of the present invention：Research shows that Surface enhanced Raman scattering phenomenon is tens to hundreds of nanometers in characteristic size
Structures of metal nanoparticles surface (Zhu Z, Zhu T, Liu Z.Nanotechnology 2004,15 (3) the most obvious:
357；Jixiang Fang,Yan Yi,Bingjun Ding,and Xiaoping Song,Appl.Phys.Lett.2008,
92,131115；Lakshminarayana Polavarapu and Qinghua Xu,Langmuir 2008,24,10608-
10611) it is difficult, to obtain to obtain large area and the consistent nanostructured of structure under this feature scale by conventional art.
This Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering is a kind of three-dimensional structure, this three-dimensional
Structure is standing wave effect and the acquisition of multi-beam laser interference photoetching technology utilized in photoetching process；It is this due to standing wave effect
Three-dimensional structure is in the Z-axis direction gold nano ring-type stacked structure (as shown in Figure 1), and Gin Nanometer globoid is according to fixed periodic distance
It is stacked together, from the bottom to top, the diameter of Gin Nanometer globoid gradually increases, and width is gradually reduced；This three-dimensional structure can pass through
Multi-beam laser interference photoetching technology, in X-Y axis, forms different shapes, the array structure of different cycles distribution；It is this
Gin Nanometer globoid stacked array substrate all meets the scale requirement of Surface enhanced Raman scattering phenomenon in three dimensions, has good
Surface enhanced Raman scattering effect.
A kind of preparation method of the Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering of the present invention, including with
Lower step：
(1) substrate sample of the cleaning with high reflectance, one layer of photoresist coating of spin coating simultaneously carry out front baking, after the completion of keep away
Optical condition places pending exposure；
(2) exposure light source is used as using multi-beam laser interference optical field, often the power density of light beam reaches 1- in multiple beam
20mW/cm2, preferably 1-10mW/cm2, photoresist coating is exposed, time for exposure 30-200s, exposure is placed on development
In liquid, developed with matching the developer solution of selected photoresist, developing time 0.5-5s, weak vibrations sample in the solution
Product are cleaned with accelerating developing powder with deionized water, are dried up rapidly with ear washing bulb, to prevent photoresist due to long-time immersion
Produce demoulding or suppress gas and blow brokenly substrate film, so as to form the photoresist masterplate of nano-rings stacked array；
(3) using magnetron sputtering coater a layer thickness is sputtered in the photoresist masterplate sample surfaces of nano-rings stacked array
For the gold thin film of 20-100nm, when wherein thickness is 50-60nm, best results, form the gold with Surface enhanced Raman scattering
Nano-rings stacked array substrate.
The Gin Nanometer globoid stacked structure number of plies obtained by above-mentioned steps is 3-15 layers, and the cycle of Z-direction is 60-
150nm, a diameter of 50nm-3 μm of Gin Nanometer globoid, Gin Nanometer globoid width is 20-100nm, and Gin Nanometer globoid stacks, in X-axis and Y-axis
The cycle in direction is 300nm-5 μm, and it is 1-13cm that structure, which prepares area,2。
Base material in above-mentioned steps is polishing monocrystalline silicon piece, or has the polishing material of more than 60% reflectivity,
This material can be more advantageous to the generation of standing wave effect, and base material thickness is 0.2-2mm.
Photoresist in above-mentioned steps can be positive photoresist, or negative photoresist, its resolution ratio are not less than
500nm, photoresist thickness are 500nm-2 μm.
The optical maser wavelength selected by multi-beam laser interference optical field in above-mentioned steps is 250-400nm, it is preferable that 325nm,
355nm or 360nm.
Multi-beam laser interference optical field in above-mentioned steps can be the Three-beam Interfere for having non-modulation property, can be four
Light beam, five light beams or more multiple-beam interference.The Three-beam Interfere photoetching of wherein non-modulation property, it is desirable in three-beam the first beam with
The incidence angle of second beam coherent light is θ, 0 °<θ<45 °, meanwhile, the Space Angle of beam of coherent light is respectively 0 °, the second beam phase
The Space Angle of dry light is 180 °, and the incidence angle of three beams coherent light is θ ± δ, wherein 1 °≤δ≤5 °, Space Angle is 90 °, this
The amplitude ratio that can be obtained more than 10, the more preparation beneficial to Gin Nanometer globoid stacked array are set.And four light beams, five light beams or more
After multiple-beam interference, the same amplitude ratio for obtaining bigger, obtains the Gin Nanometer globoid stacked structure of more numbers of plies.
The Gin Nanometer globoid stacked array substrate has good Surface enhanced Raman scattering effect, refers to dense in solution
Spend and be detected for the rhodamine 6G molecule of 100nM, dripped the rhodamine 6G solution that 5 μ L concentration are 100nM with micro syringe
On the substrate, after anhydrous ethanol solvent volatilization, the micro confocal laser Raman spectrometer of 532nm is selected with optical maser wavelength
Raman detection is carried out, can clearly detect 9 features above peaks of rhodamine 6G molecule, spectral strength is minimum more than 4000au.
If beam energy 1mW/cm2, the time for exposure is 200s, and developing time 0.5s, can reach optimal effect, such as
Fruit beam energy is 10mW/cm2, time for exposure 0.5s, developing time 0.5s, can reach optimal effect.
The present invention compared with prior art the advantages of be：
(1) technology of the present invention only includes multi-beam interference photoetching technology and coating technique, therefore technique letter
It is single, since multi-beam laser interference photoetching technology has the advantages that no mask, exposure area is big, it is easy to accomplish large area preparation；
(2) present invention without mask, therefore can obtain uniformity using multi-beam laser interference optical field as exposure light source
Good large area structure, structural cycle can be by simply changing the incident angle of interfering beam and the optical maser wavelength of selection
To realize, therefore the cycle of structure is easily controllable；
(3) the Gin Nanometer globoid stacked array structure that the present invention designs all meets that Surface enhanced Raman scattering shows in three dimensions
The scale requirement of elephant, and the structure is demonstrated by experiment test can realize stronger Raman signal enhancing effect, reality below
Apply example and specifically illustrate this point.
Brief description of the drawings
Fig. 1 is a kind of preparation method of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering of the present invention
Principle schematic；
Fig. 2 is the laser interference lithographic system figure in the present invention；
Wherein, 1 is laser, and 2 and 3 be spectroscope, and 4,5,6,7 and 8 be speculum, and 9,10,11 and 14 be half
Wave plate, 12,13,15 and 24 be polarizer, and 16,17,18 and 19 be convex lens, and 20,21,22 and 23 be pin hole, and 25 be sample stage；
Fig. 3 is the preparation flow figure of Gin Nanometer globoid stacked array surface enhanced Raman scattering substrate of the present invention；
Wherein, 26 be gluing process, and 27 be exposure imaging process, and 28 be sputter coating process, and 29 be positive photoresist, 30
It is gold thin film for base material, 31；
The Gin Nanometer globoid stacked array plane SEM figures of Fig. 4 embodiment of the present invention 1；
Fig. 5 is that the Gin Nanometer globoid of the embodiment of the present invention 1 stacks detail view；
Fig. 6 is that the Gin Nanometer globoid stacked array section SEM of the embodiment of the present invention 1 schemes；
Fig. 7 is that the Raman of the embodiment of the present invention 1 tests spectrogram；
Fig. 8 is that the Gin Nanometer globoid stacked array section SEM of the embodiment of the present invention 2 schemes；
Fig. 9 is that the Raman of the embodiment of the present invention 2 tests spectrogram.
Embodiment
Embodiments of the present invention and the function, the effect that are reached are further illustrated with reference to attached drawing.
Tend to standing wave effect occur in Photolithography Technology, this effect has often seriously affected lithographic results, ground
Study carefully personnel and all try every possible means and elimination or take some measures and reduce this effect, and the present invention really exactly make use of this feature,
It is proposed a kind of new surface enhanced Raman scattering substrate technology of preparing.Utilize the standing wave effect in photoetching process, i.e. incident light base
The surface reflection of bottom material interferes with incident light and forms a kind of given stack three-dimensional structure on a photoresist, same with this
When, multi-beam laser interference photoetching technology again arranges this stacking three-dimensional structure according to specified period profile, by sputtering
The gold thin film of one layer of nano thickness, forms Gin Nanometer globoid stacked array, which has the effect of Surface enhanced Raman scattering, can
For the base material of Raman scattering detection, so as to effectively improve the Raman signal of tested substance.
Embodiment 1
(1) substrate is cleaned, the single-sided polishing silicon using thickness as 1.2mm is base material 30, it is in the anti-of visible-range
Rate is penetrated higher than 80%, is sequentially placed into acetone, absolute ethyl alcohol, deionized water and is cleaned by ultrasonic, each 100-150s, use is high-purity
Nitrogen dries up, and selects positive photoresist 29, and type carries out gluing for AR-P3740, its resolution ratio is 0.5 μm, and sol evenning machine revolution is
4000r/min, glue thickness be 1.5 μm, be placed on hot plate, with 100 DEG C progress front bakings, the front baking time is 1min, removes, keeps away
Optical condition is placed, as shown in the gluing process 26 in Fig. 3；
(2) it is exposed using four beam laser interference lithography systems, four beam interference systems are by controlling incidence angle to produce
Raw modulation phenomenon, 360nm semiconductor lasers are the system source, as shown in Fig. 2, laser 1, which sends light beam, successively passes through three
A spectroscope 2,3 and 6 obtains four beam coherent lights, is converged at using four speculums 4,5,7 and 8 on sample stage 25 a bit, four
Beam light passes through half wave plate 9,10,11 and 14, polarizer 12,13,15 and 24, convex lens 16,17,18 and 19 and pin respectively
Hole 20,21,22 and 23.Power density in system per light beam is 7.8mW/cm2, time for exposure 10s, exposes and is placed on developer solution
In, developer solution is with AR 300-26 solution and deionized water with 1：3 proportional arrangements form, developing time 1s, slight in the solution to shake
Dynamic sample is cleaned with accelerating developing powder with deionized water, and ear washing bulb drying, obtains nano-rings stacked array formwork structure, such as
Shown in exposure imaging process 27 in Fig. 3；
(3) gold thin film 31 that a layer thickness is 50nm is sputtered in sample surfaces using magnetron sputtering coater, obtains Jenner
Rice ring stacked array substrate, as shown in the sputter coating process 28 in Fig. 3.
Shown in the Gin Nanometer globoid stacked array substrate obtained by SEM observations, such as Fig. 4, Fig. 5 and Fig. 6.Gin Nanometer globoid stacks
Array structure is 1 μm in the cycle of X-direction, is 1 μm in the cycle of Y direction, and nano-rings stack the week in vertical (Z axis) direction
Phase is about 100nm, and 11 layers of nano-rings stacking number, a diameter of 280-920nm of Gin Nanometer globoid, ring width 16-55nm, prepare face
Product is 13cm2。
(4) surface obtained above has the active substrate of enhancing Raman scattering effect as Raman detection substrate, with nothing
Water-ethanol is as the rhodamine 6G solution that solvent compound concentration is 100nM, sieve for being 100nM by 5 μ L concentration with micro syringe
Red bright 6G solution is dropped in the substrate (size is 5mm × 5mm), is placed on 50 DEG C of hot plate, accelerates anhydrous ethanol solvent volatilization,
Raman detection (optical maser wavelength of micro confocal laser Raman spectrometer selects 532nm) is carried out after solution drying, detects Luo Dan
The characteristic peak of bright 6G, spectral strength is more than 40000au, and each resonance characteristics peak is also very clear, as shown in Figure 7, it is seen that the structure
Show extraordinary SERS performances.
Embodiment 2
(1) substrate is cleaned, the single-sided polishing silicon using thickness as 1.2mm is base material 30, it is in the anti-of visible-range
Rate is penetrated higher than 80%, is sequentially placed into acetone, absolute ethyl alcohol, deionized water and is cleaned by ultrasonic, each 100-150s, use is high-purity
Nitrogen dries up, and selects positive photoresist 29, and type carries out gluing for AR-P3740, its resolution ratio is 0.5 μm, and sol evenning machine revolution is
4000r/min, glue thickness be 1.5 μm, be placed on hot plate, with 100 DEG C progress front bakings, the front baking time is 1min, removes, keeps away
Optical condition is placed, as shown in the gluing process 26 in Fig. 3；
(2) it is exposed using the Three-beam Interfere etching system with non-modulation property, the first beam and second in three-beam
The incidence angle of beam coherent light is 14 °, meanwhile, the Space Angle of beam of coherent light is respectively 0 °, the space of the second beam coherent light
Angle is 180 °, and the incidence angle of three beams coherent light is 16 °, and Space Angle is 90 °, and 360nm semiconductor lasers are the system source.
Power density in system per light beam is 4mW/cm2, time for exposure 60s, exposes and is placed in developer solution, developer solution is with AR
300-26 solution is with deionized water with 1:3 proportional arrangements form, developing time 1s, and weak vibrations sample is to accelerate to show in the solution
Shadow speed, is cleaned with deionized water, and ear washing bulb drying, obtains nano-rings stacked array formwork structure, such as the exposure imaging in Fig. 3
Shown in process 27；
(3) gold thin film 31 that a layer thickness is 50nm is sputtered in sample surfaces using magnetron sputtering coater, obtains Jenner
Rice ring stacked array substrate, as shown in the sputter coating process 28 in Fig. 3.
The Gin Nanometer globoid stacked array substrate obtained by SEM observations, as shown in Figure 8.Gin Nanometer globoid stacked array structure
It is 1 μm in the cycle of X-direction, is 1 μm in the cycle of Y direction, the cycle that nano-rings stack vertical (Z axis) direction is about
110nm, 10 layers of nano-rings stacking number, golden ring diameter 80-400nm, the width about 100-30nm of Gin Nanometer globoid, preparing area is
10cm2。
(4) surface obtained above has the active substrate of enhancing Raman scattering effect as Raman detection substrate, with nothing
Water-ethanol is as the rhodamine 6G solution that solvent compound concentration is 100nM, sieve for being 100nM by 5 μ L concentration with micro syringe
Red bright 6G solution is dropped in the substrate (size is 5mm × 5mm), is placed on 50 DEG C of hot plate, accelerates anhydrous ethanol solvent volatilization,
Raman detection (optical maser wavelength of micro confocal laser Raman spectrometer selects 532nm) is carried out after solution drying, detects Luo Dan
Several characteristic peaks of bright 6G, each resonance characteristics peak is also very clear, as shown in figure 9, the characteristic peak in figure has 537cm-1、
614cm-1、640cm-1、663cm-1、776cm-1、1094cm-1、1129cm-1、1186cm-1、1314cm-1、1363cm-1、
1515cm-1、1574cm-1、1603cm-1And 1654cm-1, totally 14 characteristic peaks, these characteristic peaks highests are close to 8000au, most
It is low also above 4000au, it is seen that the structure shows extraordinary SERS performances.In addition, the present invention is structureless in 50nm thickness
Gold thin film surface is detected the rhodamine 6G solution of same concentration, there is no the characteristic peak of rhodamine 6G, this is because
Rhodamine 6G solution concentration is too low, causes same equipment can not be accurately detected the presence of its characteristic peak, when we are by concentration
More than the 10 μM characteristic peaks for just detecting rhodamine 6G solution are brought up to, this point is enough the underlying structure tool for showing that we design
There are good SERS performances.
Above example is provided just for the sake of the description purpose of the present invention, and is not intended to limit the scope of the present invention.This
The scope of invention is defined by the following claims.The various equivalent substitutions that do not depart from spirit and principles of the present invention and make and repair
Change, should all cover within the scope of the present invention.
Claims (9)
- A kind of 1. Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering, it is characterised in that：It is described that there is surface The Gin Nanometer globoid stacked array substrate of enhancing Raman scattering is a kind of three-dimensional structure, and the three-dimensional structure is utilized in photoetching process Standing wave effect and multi-beam laser interference photoetching technology obtain；The three-dimensional structure is gold nano toroidal reactor in the Z-axis direction Stack structure, Gin Nanometer globoid are stacked together according to fixed periodic distance, from the bottom to top, the diameter of Gin Nanometer globoid gradually increase or It is gradually reduced, and width is gradually reduced；The three-dimensional structure is by multi-beam laser interference photoetching technology, in X-axis and Y direction It is interior, different shapes, the Gin Nanometer globoid stacked array structure of different cycles distribution are formed, so that forming Gin Nanometer globoid stacks battle array Row substrate.
- 2. a kind of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 1, it is special Sign is：The number of plies of the Gin Nanometer globoid stacked structure is 3-15 layers, and the cycle of Z-direction is 60-150nm, Gin Nanometer globoid A diameter of 50nm-3 μm, Gin Nanometer globoid width is 10-100nm, and Gin Nanometer globoid is stacked on X-axis and the cycle of Y direction is 300nm-5 μm, it is 1-13cm that structure, which prepares area,2。
- A kind of 3. preparation method of the Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering, it is characterised in that：Bag Include following steps：(1) clean substrate sample, one layer of photoresist of spin coating simultaneously carry out front baking, after the completion of lucifuge condition place pending exposure；(2) exposure light source is used as using multi-beam laser interference optical field, often the power density of light beam reaches 1-20mW/ in multiple beam cm2, preferably 1-10mW/cm2, photoresist coating being exposed, time for exposure 30-200s, exposure is placed in developer solution, Developed with matching the developer solution of selected photoresist, developing time 0.5-5s, in the solution weak vibrations sample with Accelerate developing powder, cleaned with deionized water, dried up rapidly with ear washing bulb, produced with preventing photoresist since long-time is soaked Demoulding suppresses gas and blows brokenly substrate film, so as to form the photoresist masterplate of nano-rings stacked array；(3) sputtering a layer thickness in the photoresist masterplate sample surfaces of nano-rings stacked array using magnetron sputtering coater is The gold thin film of 20-100nm, wherein, when thickness is 50-60nm, best results, form the Jenner with Surface enhanced Raman scattering Rice ring stacked array substrate, the Gin Nanometer globoid stacked array substrate have good Surface enhanced Raman scattering effect.
- A kind of 4. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：The base material is polishing monocrystalline silicon piece, or has the polishing material of more than 60% reflectivity, The base material thickness is 0.2-2mm.
- A kind of 5. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：The photoresist is positive photoresist or negative photoresist, and photoresist resolution ratio is not less than 500nm, light The thickness of photoresist is 500nm-2 μm.
- A kind of 6. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：Optical maser wavelength selected by the multi-beam laser interference optical field is 250-400nm, it is preferable that 325nm, 355nm or 360nm.
- A kind of 7. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：The multi-beam laser interference optical field can be the Three-beam Interfere for having non-modulation property, can be four Light beam, five light beams or more multiple-beam interference.
- A kind of 8. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：The Gin Nanometer globoid stacked array substrate has good Surface enhanced Raman scattering effect, refers to pair Concentration is that the rhodamine 6G molecule of 100nM is detected in solution, the rhodamine for being 100nM by 5 μ L concentration with micro syringe 6G solution drips on the substrate, and after anhydrous ethanol solvent volatilization, the micro confocal laser for selecting 532nm with optical maser wavelength is drawn Graceful spectrometer carries out Raman detection, can clearly detect 9 features above peaks of rhodamine 6G molecule, spectral strength is minimum to be exceeded 4000au。
- A kind of 9. preparation of Gin Nanometer globoid stacked array substrate with Surface enhanced Raman scattering according to claim 3 Method, it is characterised in that：If beam energy 1mW/cm2, the time for exposure is 200s, and developing time 0.5s, can reach optimal Effect, if beam energy is 10mW/cm2, time for exposure 0.5s, developing time 0.5s, can reach optimal effect.
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| CN108680979A (en) * | 2018-06-21 | 2018-10-19 | 中国人民解放军63908部队 | Two-dimension grating resists Polarization-Sensitive SERS substrates and its processing method |
| CN108827933A (en) * | 2018-05-17 | 2018-11-16 | 华南师范大学 | A kind of surface enhanced Raman scattering substrate and its preparation method and application |
| CN109911844A (en) * | 2019-03-05 | 2019-06-21 | 中车工业研究院有限公司 | A kind of the 3-D nano, structure preparation method and 3-D nano, structure of imitative butterfly's wing |
| CN109975270A (en) * | 2019-04-12 | 2019-07-05 | 北京师范大学 | A kind of silver nano flower-like periodic array SERS substrate and preparation method thereof |
| CN110873707A (en) * | 2018-08-29 | 2020-03-10 | 电子科技大学 | 3D surface enhanced Raman sensing chip and preparation method thereof |
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| CN109975270A (en) * | 2019-04-12 | 2019-07-05 | 北京师范大学 | A kind of silver nano flower-like periodic array SERS substrate and preparation method thereof |
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