CN103575721B - A kind of sandwich construction surface enhanced Raman scattering substrate and preparation method thereof - Google Patents
A kind of sandwich construction surface enhanced Raman scattering substrate and preparation method thereof Download PDFInfo
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- CN103575721B CN103575721B CN201310549478.5A CN201310549478A CN103575721B CN 103575721 B CN103575721 B CN 103575721B CN 201310549478 A CN201310549478 A CN 201310549478A CN 103575721 B CN103575721 B CN 103575721B
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- 239000000758 substrate Substances 0.000 title claims abstract description 32
- 238000010276 construction Methods 0.000 title claims abstract description 15
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000010931 gold Substances 0.000 claims abstract description 13
- 229910052737 gold Inorganic materials 0.000 claims abstract description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 4
- 239000003292 glue Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- 238000005530 etching Methods 0.000 claims description 15
- 238000004528 spin coating Methods 0.000 claims description 15
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 14
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000005240 physical vapour deposition Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 229920002521 macromolecule Polymers 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 238000005566 electron beam evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000001020 plasma etching Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 3
- 238000009415 formwork Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229910001923 silver oxide Inorganic materials 0.000 claims description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000003623 enhancer Substances 0.000 abstract description 8
- 238000004049 embossing Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 238000001883 metal evaporation Methods 0.000 abstract 1
- 238000000992 sputter etching Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 17
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000560 biocompatible material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to nanometer embossing and spectral technique field, be specially a kind of sandwich construction surface enhanced Raman scattering substrate and preparation method thereof, object is to prepare a kind of surface enhanced Raman scattering substrate having simple, efficient, the high enhancer of technique, have biocompatibility.This substrate is made up of substrate and the periodicity nanometer column structure be positioned on substrate, and wherein, nanometer column structure is sandwich construction, and the layer gold of the alternating layer that sandwich construction is made up of silver and medium and most top layer forms.The present invention take nanometer embossing as core, the techniques such as association reaction ion etching, metal evaporation, applying silicon oxide, metal-stripping prepare multi-layer nano structure, coordinate silver-colored structural substrates and do not have biocompatibility and a low technical matters of golden structural substrates enhancer, on the basis ensureing biocompatibility, substantially increase the enhancer of substrate, make detection more efficient, sensitive, can be used for biological detection after process further.
Description
Technical field
The invention belongs to nanometer embossing and spectral technique field, relate to the preparation method of the column-like multi-layer structures that a kind of metal level/dielectric layer cycle that can be used as surface enhanced Raman scattering substrate replaces.
Background technology
In recent years, Surface enhanced raman spectroscopy (SERS) is one of research field the most popular.Nano gap between the point effect of irregular nano particle, particle and coarse metal surface can strengthen local electric field greatly, compared to normal Raman scattering, signal intensity increases substantially, wherein extensive with the research of silver, gold nano structure, thus how preparing more closely spaced metal Nano structure fast and effectively will become crucial.The method of what current people mainly adopted is spin coating self assembly and vapour deposition.The former is convenient and swift, but is unfavorable for regulation and control, simultaneously because nano particle is comparatively easy to assemble, is unfavorable for the nanostructured that preparation size is less.The latter can prepare nanometer result comparatively accurately, but process is comparatively loaded down with trivial details, and cost is higher.
Nano impression is the technology of a kind of high resolving power, high yield, low cost, this technology is particularly suitable for the metal nanodot array structure that manufacturing cycle is little, resolution is high, density is large, can repeat, stablize, prepare uniform metal nanodot array structure reliably.This class formation as SERS substrate, can greatly improve the homogeneity of Raman detection, stability, repeatability and confidence level.
Argent is known to the most effective metal of Raman signal enhancing at present, but its poor biocompatibility.Gold is biocompatible material, but its ability strengthening Raman signal is weaker than silver.How to make up both deficiency; How to improve the enhancer of Surface enhanced raman spectroscopy further, the sensitivity improving detection obtains to be paid close attention to widely.
Summary of the invention
The preparation method of that the object of this invention is to provide a kind of long-term stability, that there is high sensitivity and biocompatibility surface enhanced Raman scattering substrate.
This long-term stability, the feature of the surface enhanced Raman scattering substrate with high sensitivity and biocompatibility has column-like multi-layer structures, quartz substrate is prepared argent and silicon dioxide cycle alternately, and the superiors is the nanostructured of gold.The gold of the superiors can ensure biocompatibility; Silver strengthens the best metal of effect, and the dielectric layer increased can strengthen Surface enhanced raman spectroscopy signal further, improves enhancer, improves the sensitivity detected.
Technical solution of the present invention is as follows:
A kind of sandwich construction surface enhanced Raman scattering substrate, be made up of substrate and the periodicity nanometer column structure be positioned on substrate, nanometer column structure is sandwich construction, and the layer gold of the alternating layer that sandwich construction is made up of silver and medium and the superiors forms.
Prepare the method for above-mentioned a kind of sandwich construction surface enhanced Raman scattering substrate, step is as follows:
(1) nano impression
A) substrate prepares: get suitable size piezoid, use N
2blow away surface dirt;
B) with spin-coating method spin coating double-layer glue on piezoid: spin coating lower floor glue: lower floor is the PMMA that about 160nm is thick; Heat dries 5min, organic solvent in removing PMMA; Spin coating upper strata glue: upper strata is the UV glue that about 50nm is thick;
C) by anodic oxidation aluminium formwork preparation, the soft template that obtains fits in step b) sample on, and make there is no bubble between the two as far as possible;
D) ultraviolet light polymerization: by step c) sample inserts in exposure device, logical N
25min is to drain the O in device
2, continue to pass into N
2, at N
2ultraviolet glue was solidified in 15 minutes by UV-irradiation in atmosphere;
E) close uviol lamp, take out sample, carefully take template off with tweezers, obtain the sample with template inverse structure;
(2) reactive ion etching (ICP) removes remnant layer, comprises remaining upper strata UV glue and lower floor macromolecule transfer layer PMMA
A) CHF is used
3and O
2mixed gas be etching gas etching upper strata remnants UV glue;
B) O is used
2for etching gas etching lower floor macromolecule transfer layer PMMA;
(3) plated film
A) silver-plated: with the silverskin method of the resistance heating evaporation in physical vapour deposition (PVD) sample after etching plating about 25nm;
B) applying silicon oxide: 1. activation cleaning matrix surface: matrix is placed in plasma device chamber, is evacuated to 1.0 × 10
-4pa ~ 1.0 × 10
-3pa, passing into argon gas to vacuum tightness is 1.5Pa ~ 2.0Pa; Open radio-frequency power supply, power setting is 100W ~ 400W, carries out activation cleaning 5-10 minute with argon plasma to matrix surface; 2. deposit film: stop argon gas passing into, pass into SiH
4and N
2the mixed gas of O is 4.0Pa ~ 6.0Pa to pressure, opens radio-frequency power supply, and power setting is 150 ~ 300W, the silica membrane that using plasma chemical vapor deposition 15nm is thick; Wherein SiH
4and N
2the mass rate number percent of O is respectively 8% ~ 21%, 79% ~ 92%;
C) as required, step a) and b) is repeated;
D) gold-plated: the gold alternating layer formed at silver and silicon dioxide by the method for the electron beam evaporation deposition in physical vapor deposition plating about 35nm;
(4) lift off
Insert in chlorobenzene or acetone by the sample after step (3) plated film, ultrasonic about 5min, the metal construction on glue-line is peeled off.
The present invention has coordinated silver-colored structural substrates does not have biocompatibility and a low technical matters of golden structural substrates enhancer, on the basis ensureing biocompatibility, substantially increase the enhancer of substrate, make detection more efficient, sensitive, can be used for biological detection after process further.There is following beneficial effect:
1) can repeat, stablize, reliably and with long-term prepare uniform large-area nano-dot matrix structure, improve the homogeneity of Raman detection, stability, repeatability and confidence level.
2) technique is simple, and cost is low.
3) this surface enhanced Raman scattering substrate obtained has biocompatibility.
4) compare single layer structure, enhancer significantly improves, and detection sensitivity strengthens.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention Ag/SiO
2/ Ag/SiO
2/ Au five-layer structure SERS substrate preparation flow schematic diagram, 1-quartz substrate; 2-PMMA; 3-UV glue; 4-impression block; 5-silver; 6-silicon dioxide; 7-gold; 8-ultraviolet light.
Embodiment
The concrete preparation process of the present embodiment is as follows:
(1) nano impression
A) substrate prepares: get suitable size piezoid, use N
2blow away surface dirt;
B) with spin-coating method spin coating double-layer glue on piezoid:
Spin coating lower floor glue: lower floor is the PMMA(3%PMMA that about 160nm is thick, sol evenning machine rotating speed 3000r/min, spin coating 40s);
Heat dries about 5min, organic solvent in removing PMMA;
Spin coating upper strata glue: upper strata is the UV glue (2.5%UV, sol evenning machine rotating speed 3000r/min, spin coating 40s) that about 50nm is thick;
C) soft template preparation of anodised aluminium masterplate obtained fits on sample, and makes do not have bubble therebetween as far as possible;
D) ultraviolet light polymerization: sample is inserted in exposure device, logical N
25min is to drain the O in device
2, continue to pass into N
2, at N
2ultraviolet glue was solidified in 15 minutes by UV-irradiation in atmosphere;
E) close uviol lamp, take out sample.Carefully template is taken off with tweezers.Obtain impressing sample that is upper and template inverse structure.
(2) reactive ion etching (ICP) removes remnant layer (comprising remaining upper strata UV glue and lower floor macromolecule transfer layer PMMA).
A) CHF is used
3and O
2mixed gas be etching gas etching upper strata remnants UV glue;
B) O is used
2for etching gas etching lower floor macromolecule transfer layer PMMA.
(3) plated film is (with Ag/SiO
2/ Ag/SiO
2/ Au five-layer structure is example)
A) silver-plated: with the silverskin method of the resistance heating evaporation in physical vapour deposition (PVD) sample after etching plating about 25nm;
B) applying silicon oxide: 01 activation cleaning matrix surfaces: matrix is placed in plasma device chamber, is evacuated to 1.0 × 10
-4pa ~ 1.0 × 10
-3pa, passing into argon gas to vacuum tightness is 1.5Pa ~ 2.0Pa.Open radio-frequency power supply, power setting is 100W ~ 400W, carries out activation cleaning 5-10 minute with argon plasma to matrix surface; 2. deposit film: stop argon gas passing into, the mixed gas passing into SiH4 and N2O is 4.0Pa ~ 6.0Pa to pressure, opens radio-frequency power supply, and power setting is 150 ~ 300W, and using plasma chemical vapor deposition is about the silica membrane of 15nm; Wherein SiH
4and N
2the mass rate number percent of O is respectively 8% ~ 21%, 79% ~ 92%;
C) step a) and b) is repeated, the plating silver of 25nm and the silicon dioxide of 15nm;
D) gold-plated: the gold plating about 35nm by the method for the electron beam evaporation deposition in physical vapor deposition on sample.
4) lift off
Inserted by sample after plated film in chlorobenzene or acetone, ultrasonic about 5min, the metal construction on glue-line is peeled off.
Claims (1)
1. the preparation method of a sandwich construction surface enhanced Raman scattering substrate, this substrate is made up of substrate and the periodicity nanometer column structure be positioned on substrate, nanometer column structure is sandwich construction, sandwich construction is made up of the layer gold of silver and the alternating layer that forms of medium and most top layer, it is characterized in that, the concrete steps of preparation method are as follows:
(1) nano impression
A) substrate prepares: get suitable size piezoid, use N
2blow away surface dirt;
B) with spin-coating method spin coating double-layer glue on piezoid: spin coating lower floor glue: lower floor is the PMMA that about 160nm is thick; Heat dries 5min, organic solvent in removing PMMA; Spin coating upper strata glue: upper strata is the UV glue that about 50nm is thick;
C) by anodic oxidation aluminium formwork preparation, the soft template that obtains fits in step b) sample on, and make there is no bubble between the two as far as possible;
D) ultraviolet light polymerization: by step c) sample inserts in exposure device, logical N
25min is to drain the O in device
2, continue to pass into N
2, at N
2ultraviolet glue was solidified in 15 minutes by UV-irradiation in atmosphere;
E) close uviol lamp, take out sample, carefully take template off with tweezers, obtain the sample with template inverse structure;
(2) reactive ion etching removes remnant layer, comprises remaining upper strata UV glue and lower floor macromolecule transfer layer PMMA
A) CHF is used
3and O
2mixed gas be etching gas etching upper strata remnants UV glue;
B) O is used
2for etching gas etching lower floor macromolecule transfer layer PMMA;
(3) plated film
A) silver-plated: with the silverskin method of the resistance heating evaporation in physical vapor deposition sample after etching plating about 25nm;
B) applying silicon oxide: 1. activation cleaning matrix surface: matrix is placed in plasma device chamber, is evacuated to 1.0 × 10
-4pa ~ 1.0 × 10
-3pa, passing into argon gas to vacuum tightness is 1.5Pa ~ 2.0Pa; Open radio-frequency power supply, power setting is 100W ~ 400W, carries out activation cleaning 5-10 minute with argon plasma to matrix surface; 2. deposit film: stop argon gas passing into, pass into SiH
4and N
2the mixed gas of O is 4.0Pa ~ 6.0Pa to pressure, opens radio-frequency power supply, and power setting is 150 ~ 300W, the silica membrane that using plasma chemical vapor deposition 15nm is thick; Wherein SiH
4and N
2the mass rate number percent of O is respectively 8% ~ 21%, 79% ~ 92%;
C) as required, step a) and b) is repeated;
D) gold-plated: the gold alternating layer formed at silver and silicon dioxide by the method for the electron beam evaporation deposition in physical vapour deposition (PVD) plating about 35nm;
(4) lift off
Insert in chlorobenzene or acetone by the sample after step (3) plated film, ultrasonic about 5min, the metal construction on glue-line is peeled off.
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| CN103575721B true CN103575721B (en) | 2016-04-13 |
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| CN105129724A (en) * | 2015-08-11 | 2015-12-09 | 中国科学院电子学研究所 | Manufacturing method of surface-enhanced Raman scattering (SERS) substrate |
| CN106645077B (en) * | 2015-10-28 | 2019-06-25 | 上海大学 | The preparation method of SERS active-substrate of the spot size less than 5nm |
| CN105648413A (en) * | 2016-01-22 | 2016-06-08 | 吉林师范大学 | Preparing method for metal/oxide compound surface enhanced Raman active substrate |
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| CN105911044B (en) * | 2016-04-25 | 2019-02-15 | 中国科学院理化技术研究所 | Surface enhanced Raman spectrum substrate with nanogap and preparation method thereof |
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| CN110412010B (en) * | 2019-07-31 | 2020-02-21 | 广东食品药品职业学院 | Preparation and application of Raman enhanced substrate based on multilayer composite structure |
| CN113125405B (en) * | 2019-12-31 | 2023-06-06 | 有研工程技术研究院有限公司 | SERS substrate based on nano conical needle structure and preparation method |
| CN113125406B (en) * | 2019-12-31 | 2023-06-06 | 有研工程技术研究院有限公司 | SERS substrate with microscopic ordered nano structure and preparation method thereof |
| CN113533295A (en) * | 2021-06-01 | 2021-10-22 | 山东师范大学 | Based on ReS2Three-dimensional SERS substrate and preparation method and application thereof |
| WO2024191346A1 (en) * | 2023-03-13 | 2024-09-19 | Agency For Science, Technology And Research | A multi-functional sensor for molecular spectroscopy |
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| CN102285629A (en) * | 2011-05-05 | 2011-12-21 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN103163115A (en) * | 2011-12-11 | 2013-06-19 | 欧普图斯(苏州)光学纳米科技有限公司 | Multi-layer variable microstructure capable of sensing substance |
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| US8975205B2 (en) * | 2008-11-10 | 2015-03-10 | University Of Georgia Research Foundation, Inc. | Photocatalytic structures, methods of making photocatalytic structures, and methods of photocatalysis |
| JP5487066B2 (en) * | 2010-10-04 | 2014-05-07 | ルネサスエレクトロニクス株式会社 | Inspection method of semiconductor device |
| TWI490474B (en) * | 2012-01-12 | 2015-07-01 | Phansco Corp | Metal nanopillars for surface-enhanced raman spectroscopy (sers) substrate and method for preparing same |
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| CN102285629A (en) * | 2011-05-05 | 2011-12-21 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN103163115A (en) * | 2011-12-11 | 2013-06-19 | 欧普图斯(苏州)光学纳米科技有限公司 | Multi-layer variable microstructure capable of sensing substance |
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