CN105129724A - Manufacturing method of surface-enhanced Raman scattering (SERS) substrate - Google Patents
Manufacturing method of surface-enhanced Raman scattering (SERS) substrate Download PDFInfo
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Abstract
The invention provides a manufacturing method of a surface-enhanced Raman scattering (SERS) substrate. The manufacturing method comprises the following steps: A, acquiring a high-molecular polymer film, wherein the high-molecular polymer film is made of a high-molecular polymer material which can be subjected to oxygen plasma etching; B, performing oxygen plasma etching treatment on the high-molecular polymer film to form nanorod arrays which are arranged vertically upwards; and C, covering the surfaces of the nanorod arrays with a metal layer having SERS activity to form metal nanorod arrays which are arranged upwards in order to finish manufacturing of the SERS substrate. In the method, the sizes and gaps of metal nanorods can be controlled at a nanoscale, so that the manufactured SERS substrate has a large specific surface area; the adsorption of molecules to be tested is facilitated; and the reduction of luminous reflectance and intercoupling of electric fields among the metal nanorods are facilitated. Thus, the Roman scattering enhancing effect can be enhanced greatly through the SERS substrate.
Description
Technical field
The present invention relates to technical field of Raman spectrum, particularly relate to a kind of preparation method of SERS substrate.
Background technology
SERS (SERS), as a kind of analytical technology, has important application potential in chemical analysis and biological detection.And have higher enhancing effect, lower detectability and better conforming substrate be realize its application basis.
At present, being strengthened mechanism by the SERS extensively approved and mainly comprise Electromagnetic enhancement and Chemical enhancement, is again wherein chief reason with Electromagnetic enhancement.The effect of Electromagnetic enhancement depends on the concussion of metallic surface plasma, therefore has coarse structure and the surface texture that can realize field coupling between metallic is best suited for SERS substrate.
Silicified breccias is utilized to prepare coarse structure and with it for preparation that template realizes metal structure is preparation method (see reference document 1,2) conventional at present.Such as, bibliography 2 discloses and utilizes the aluminium with pit to be templated deposition gold film, then removes aluminum alloy pattern plate and is overturn, then obtaining a kind of structurally ordered and controlled SERS substrate.These preparation methods all obtain and strengthen effect preferably, but preparation method's all comparatively complicated and time consumption, and the local electric field intensity adjustment of some methods to metal surface is poor.
Utilizing polymer to prepare SERS structure is a kind of more novel preparation method.Because organic polymer plasticity is strong and be convenient to processing, cause the concern of researcher.Such as, bibliography 3 discloses and a kind ofly polymeric material is impressed out pattern and evaporation metal prepares the method for SERS substrate.These methods prepare coarse structure owing to make use of polymer, and therefore preparation process can be relatively simple and quick.The polymer being applied to preparing SERS substrate at present comprises polymetylmethacrylate (bibliography 4), dimethyl siloxane PDMS (bibliography 5) etc.But required by impression block still need through comparatively complicated processing, and metal structure prepared by these methods is difficult to control at nanoscale.
Plasma surface treatment is a kind of comparatively conventional process for treating surface, polymethyl siloxane (bibliography 6) after plasma treatment, the polymer surfaces such as polymethyl methacrylate (bibliography 7) and polystyrene (bibliography 8) all there will be nanostructured.Current plasma treatment organic matter surface is mainly used in the hydrophobicity improving organic matter surface, reduces the characteristics such as light reflection.And utilize plasma treatment polymer to obtain nanostructured and also rare with this report preparing nano-functional material.The array that bibliography 9 utilizes plasma treatment polystyrene sphere to form, and obtain SERS substrate at its surface sputtering metal.Although this patent make use of plasma treatment, just utilize the etching of p-poly-phenyl ethene bead side to regulate the distance between bead.
Bibliography 1: patent CN200810100562;
Bibliography 2: patent CN201310130493
Bibliography 3: patent CN201310032239
Bibliography 4: patent CN201310316980
Bibliography 5: patent CN201210543908
Bibliography 6:PlasmaProcess.Polym.2007,4:98-405; Nanotechnology2006,17:3977-3983
Bibliography 7:PlasmaProcess.Polym.2007,4:S878-S881
Bibliography 8:PS, Langmuir2008,24:5044-5051
Bibliography 9: patent CN201110115269
Summary of the invention
(1) technical problem that will solve
In view of above-mentioned technical problem, the invention provides a kind of preparation method of SERS substrate, to realize the adjustment to metal nano-rod size and spacing.
(2) technical scheme
The preparation method of SERS substrate of the present invention comprises: steps A: obtain polymer membrane, the composition of this polymer membrane is the macromolecule polymer material that can carry out oxygen plasma etch; Step B: carry out oxygen plasma etch process to polymer membrane, forms the nanometer stick array arranged straight up; And step C: the metal level in nanometer stick array surface coverage with surface-enhanced Raman scattering activity, forms the metal nano-rod array upwards arranged, completes the preparation of SERS substrate.
(3) beneficial effect
As can be seen from technique scheme, in the preparation method of SERS substrate of the present invention, because metal nano-rod size can be controlled in nanoscale, the SERS substrate of preparation has larger specific area, is conducive to the absorption of testing molecule.In addition, the spacing of metal nano-rod array also can control at nanoscale, is conducive to intercoupling of electric field between the reduction of light reflectivity and metal nano-rod.Therefore, the SERS substrate that prepared by the method can realize the larger raising that Raman scattering strengthens effect.
Accompanying drawing explanation
Figure 1A is the flow chart of the preparation method according to embodiment of the present invention SERS substrate;
Figure 1B and Fig. 1 C performs the device stereogram after each step and profile for adopting the preparation method shown in Figure 1A;
The SEM photo of the Silver nanorod array vertical section that Fig. 2 is prepared for the preparation method shown in employing Figure 1A;
Fig. 3 is when adopting Kapton, the SEM photo of Silver nanorod array surface that finally formed of different oxygen plasma etch processing time in step B;
Fig. 4 is the SEM photo of the Silver nanorod array surface finally formed of different metal sputtering thickness in step C;
Fig. 5 is when adopting polyvinylidene difluoride film, the SEM photo of Silver nanorod array surface that finally formed of different oxygen plasma etch processing time in step B.
Detailed description of the invention
The present invention can realize the adjustment to metal nano nod gap by adjustment oxygen plasma etch processing time and splash-proofing sputtering metal thickness; The adjustment to metal nano-rod diameter can be realized by change sputtering thickness.
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
In first exemplary embodiment of the present invention, provide a kind of preparation method of SERS substrate.Figure 1A is the flow chart of the preparation method according to embodiment of the present invention SERS substrate.As shown in Figure 1A, the preparation method of the present embodiment SERS substrate comprises:
Steps A: make polymer membrane on substrate, as shown in (A) in Figure 1B and Fig. 1 C;
In the present embodiment, substrate adopts silicon chip, and polymer membrane adopts Kapton.Preparation process prepared by this Kapton is: first dropped on the silicon chip of surface cleaning by polyimide solution, and utilizes spin coater to rotate one minute with the speed of 1200r/min; Then film is placed in dry 2h under 80 DEG C of environment, forms Kapton at silicon chip surface.
It should be apparent to those skilled in the art that, except silicon wafer substrate, the hard substrates such as potsherd, sheet glass and poly (methyl methacrylate) plate can also be adopted, and except polyimides (PI) film, the polymer membranes such as Kynoar, polystyrene, polymethyl methacrylate and PETG can also be adopted.Except above-mentioned spin-coating method, the method preparing macromolecule membrane can also be membrane method.In addition, prepare except film except using polymer solution, the finished product diaphragm of the polymer such as polyimides, Kynoar, polystyrene, polymethyl methacrylate and PETG also can be used as mould material, in this case, can not use substrate.
Step B: oxygen plasma etch process is carried out to polymer membrane, form the nanometer stick array arranged straight up, i.e. SERS substrate template, as shown in (B) in Figure 1B and Fig. 1 C;
In the present embodiment, silicon chip surface with Kapton puts into reactive ion etching machine, utilize oxygen plasma treatment technology to Kapton surface etch, oxygen plasma treatment process is carried out in reactive ion etching machine, radio-frequency power supply frequency is 13.56MHz, and oxygen flow is 30mL/min, and reaction chamber pressure is 3Pa, RF-coupled power is 100W, and the processing time is 60s.
Wherein, the spacing in nanometer stick array between nanometer rods can realize regulating by changing the oxygen plasma etch processing time.The nanometer stick array of formation of different oxygen plasma etch processing time will be provided in subsequent embodiment.In this nanometer stick array, the diameter of nanometer rods is about 20-30nm, and its shape of cross section is circular, and the spacing of adjacent nano rod is less than 80nm.
Step C: the metal level at the nanometer stick array surface sputtering of SERS substrate template with SERS activity, forms the metal nano-rod array upwards arranged, completes the preparation of SERS substrate, as shown in (C) in Figure 1B and Fig. 1 C.
In the present embodiment, with the Kapton after oxygen plasma treatment for template, at its surface sputtering silver, wherein sputtering power is 100W, and chamber atmosphere is argon gas, and chamber pressure is 0.5Pa, and sputtering thickness is 20nm.The SEM image of the Silver nanorod array vertical section of preparation as shown in Figure 2.
Wherein, the diameter of metal nano-rod can be regulated by the thickness changing splash-proofing sputtering metal.Generally, the thickness of splash-proofing sputtering metal is less than 90nm.After sputtering, the diameter of metal nano-rod is between 30nm ~ 80nm, and adjacent metal nanorod spacings is between 5nm ~ 50nm.In addition to silver, gold, copper etc. can also be adopted to have the metal material of SERS activity.
In a second embodiment of the present invention, the preparation method of another kind of SERS substrate is additionally provided.The process of the present embodiment is as similar in the first embodiment, and difference is the time of oxygen plasma etch process in step B.
Fig. 3 is when adopting Kapton, the SEM photo of Silver nanorod array surface that finally formed of different oxygen plasma etch processing time in step B.Wherein, (a), (b), (c), (d) is respectively the stereoscan photograph that the oxygen plasma treatment time is the Silver nanorod array of 15s, 30s, 45s and 60s.Visible, the gap of nanometer stick array achieves adjustment by changing the oxygen plasma etch processing time.
In the 3rd exemplary embodiment of the present invention, further provide the preparation method of another kind of SERS substrate.The process of the present embodiment is as similar in the first embodiment, and difference is the thickness of splash-proofing sputtering metal in step C.
Fig. 4 is the SEM photo of the Silver nanorod array surface finally formed of different metal sputtering thickness in step C.Wherein, figure (a), (b), (c), the sputtering thickness of (d) is respectively 30nm, 50nm, 70nm and 90nm.Visible, the diameter of metal nano-rod achieves adjustment by the thickness changing splash-proofing sputtering metal.It should be noted that, be less than the thickness of in the vertical direction metal at the thickness of the metal of nanometer rods sidewall attachment, as shown in (C) in Fig. 1 C.
In the 4th exemplary embodiment of the present invention, further provide the preparation method of another kind of SERS substrate.The process of the present embodiment is as similar in the first embodiment, and difference is that in steps A, polymer membrane is polyvinylidene difluoride film, and in step B, oxygen plasma etch process changes.
Fig. 5 is when adopting polyvinylidene difluoride film, the SEM photo of Silver nanorod array surface that finally formed of different oxygen plasma etch processing time in step B.Wherein, (a), (b), (c), (d) is respectively the stereoscan photograph that the oxygen plasma treatment time is the Silver nanorod array of 15s, 30s, 45s and 60s.Visible, the gap of nanometer stick array achieves adjustment by changing the oxygen plasma treatment time.
So far, by reference to the accompanying drawings the present invention's four embodiments have been described in detail.Describe according to above, those skilled in the art should have the preparation method of SERS substrate of the present invention and have clearly been familiar with.
It should be noted that, in accompanying drawing or description text, the implementation not illustrating or describe, is form known to a person of ordinary skill in the art in art, is not described in detail.In addition, the above-mentioned definition to each element and method is not limited in various concrete structures, shape or the mode mentioned in embodiment, and those of ordinary skill in the art can change simply it or replace, such as:
(1) in step, except membrane method and spin-coating method, other method can also be adopted to prepare polymer membrane, even if employing spin-coating method, technological parameter wherein also can adjust as required, such as: by dry for the polyimide film dry of spin coating, baking temperature is 50-250 DEG C, maintenance time >=1h;
(2) in step B, the technological parameter of oxygen plasma etch process can adjust as required, and such as: reaction chamber pressure is 3Pa, RF-coupled power is between 50W-200W, and processing time t meets: 1s≤t≤60s;
(3) in step C, the method for sputtered metal film can use magnetron sputtering, pulsed laser deposition, electron beam evaporation etc.
In sum, the present invention utilizes oxygen plasma etch process polymer surfaces also to obtain the metal nano-rod array arranged straight up.Gap wherein between metal nano-rod can by changing oxygen plasma treatment time and splash-proofing sputtering metal thickness realization adjustment, and the diameter of metal nano-rod can be regulated by the thickness changing metal sputtering, the metal nano nod gap after overregulating and metal nano-rod diameter all can control at nanoscale.The method technique is comparatively simple and process is comparatively quick, has huge application potential in SERS technical field.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for SERS substrate, is characterized in that, comprising:
Steps A: obtain polymer membrane, the composition of this polymer membrane is the macromolecule polymer material that can carry out oxygen plasma etch;
Step B: carry out oxygen plasma etch process to polymer membrane, forms the nanometer stick array arranged straight up; And
Step C: the metal level in nanometer stick array surface coverage with surface-enhanced Raman scattering activity, forms the metal nano-rod array upwards arranged, completes the preparation of SERS substrate.
2. preparation method according to claim 1, is characterized in that, in described step B, regulates the spacing of adjacent nano rod in nanometer stick array by changing the oxygen plasma etch processing time.
3. preparation method according to claim 2, is characterized in that, in described nanometer stick array, the diameter of nanometer rods is between 20nm ~ 30nm, and shape of cross section is circular; The spacing d1 of adjacent nano rod meets: 10nm≤d1≤80nm.
4. preparation method according to claim 2, is characterized in that, described step B comprises: polymer membrane is put into reactive ion etching machine, utilizes oxygen plasma treatment method to etch polymer membrane surface;
Wherein, the technological parameter of described reactive ion etching is as follows: radio-frequency power supply frequency is 13.56MHz, and oxygen flow is 30mL/min, and reaction chamber pressure is 3Pa, and RF-coupled power is between 50W ~ 200W, and processing time t meets: 1s≤t≤60s.
5. preparation method according to claim 1, is characterized in that, in described step C, is regulated the diameter of metal nano-rod by the thickness changing covering metal layer.
6. preparation method according to claim 5, is characterized in that, the thickness d of described metal level meets: 10nm≤d≤90nm;
In metal nano-rod array, adjacent metal nanorod spacings d2 is between 5nm ~ 50nm.
7. preparation method according to claim 1, is characterized in that, in described step C, described in there is surface-enhanced Raman scattering activity metal be: gold, silver or copper;
Adopt following methods one of them has the metal level of surface-enhanced Raman scattering activity in nanometer stick array surface coverage: magnetron sputtering, pulsed laser deposition and electron beam evaporation.
8. preparation method according to any one of claim 1 to 7, is characterized in that, the approach obtaining polymer membrane in described steps A is:
Hard substrate makes the film of described macromolecule polymer material; Or
Adopt the diaphragm of described macromolecule polymer material as described polymer membrane.
9. preparation method according to claim 8, is characterized in that, described macromolecule polymer material is the one in following material: polyimides, Kynoar, polystyrene, polymethyl methacrylate and PETG.
10. preparation method according to claim 8, is characterized in that, obtains described polymer membrane by the film making macromolecule polymer material on hard substrate;
Wherein, the method making the film of macromolecule polymer material is spin-coating method or membrane method, and described hard substrate is with the one in infrabasal plate: silicon chip, potsherd, sheet glass and poly (methyl methacrylate) plate.
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| CN105372728A (en) * | 2015-12-21 | 2016-03-02 | 吉林大学 | One-dimension, two-dimension or three-dimension nanometer gap array having Raman enhancement property and preparation method for the same |
| CN107739020A (en) * | 2017-10-18 | 2018-02-27 | 苏州大学 | A kind of electro-magnetic wave absorption structure of flexible extensible and preparation method thereof |
| CN109929905A (en) * | 2019-04-01 | 2019-06-25 | 天津国科医工科技发展有限公司 | Three-dimensional Raman for bacterium Rapid identification enhances film and its method and system |
| CN110164693A (en) * | 2018-02-12 | 2019-08-23 | 北京纳米能源与系统研究所 | Electret electrode and preparation method thereof, electret device |
| CN110484918A (en) * | 2019-07-23 | 2019-11-22 | 南京大学 | Surface-enhanced Raman substrate and preparation method thereof based on hanging Au nanometers of finger closed array |
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| CN112537754A (en) * | 2020-12-08 | 2021-03-23 | 江苏创芯海微科技有限公司 | Electrical isolation structure and preparation method thereof |
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| CN105372728A (en) * | 2015-12-21 | 2016-03-02 | 吉林大学 | One-dimension, two-dimension or three-dimension nanometer gap array having Raman enhancement property and preparation method for the same |
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| CN110484918A (en) * | 2019-07-23 | 2019-11-22 | 南京大学 | Surface-enhanced Raman substrate and preparation method thereof based on hanging Au nanometers of finger closed array |
| CN112394053A (en) * | 2019-08-16 | 2021-02-23 | 吉林师范大学 | Preparation method of ultrasensitive SERS flexible composite membrane and application of ultrasensitive SERS flexible composite membrane in detection of enrofloxacin hydrochloride in water body |
| CN111777031A (en) * | 2020-07-15 | 2020-10-16 | 京东方科技集团股份有限公司 | Biological detection chip substrate and preparation method thereof |
| CN112537753A (en) * | 2020-12-08 | 2021-03-23 | 江苏创芯海微科技有限公司 | Scribing channel structure suitable for laser invisible cutting and preparation method thereof |
| CN112537753B (en) * | 2020-12-08 | 2021-12-24 | 江苏创芯海微科技有限公司 | Scribing channel structure suitable for laser invisible cutting and preparation method thereof |
| CN112537754A (en) * | 2020-12-08 | 2021-03-23 | 江苏创芯海微科技有限公司 | Electrical isolation structure and preparation method thereof |
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