CN1699966A - Surface reinforced Raman dissemination active substrate and production process thereof - Google Patents
Surface reinforced Raman dissemination active substrate and production process thereof Download PDFInfo
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- CN1699966A CN1699966A CN 200410010288 CN200410010288A CN1699966A CN 1699966 A CN1699966 A CN 1699966A CN 200410010288 CN200410010288 CN 200410010288 CN 200410010288 A CN200410010288 A CN 200410010288A CN 1699966 A CN1699966 A CN 1699966A
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Abstract
The invention relates to a surface reinforced scattering active base in the filed of laser spectrum measurement, which comprises glass substrate with mercapto treatment on the surface which deposits Ag nanometer modification inlay by silver mirror reaction. The process for preparing the base comprises substrate-hydroxylating treatment; substrate mercapto treatment and substrate surface Ag nanometer modification inlay formation.
Description
Technical field
The invention belongs to laser Raman spectroscopy and detect apparatus technical field, particularly a kind of surface-enhanced Raman scattering activity substrate and preparation method thereof.
Background technology
Based on the material impact of membrane structure to its assembling function, people extraordinarily pay attention to the research of unimolecular film cohesion and phase transition process in recent years, have developed various highly sensitive surface analysis techniques research membrane structure on the throne and coacervation process.The sensitivity of SERS technical research surface and interface is high, therefore becomes a kind of powerful measure of unimolecular film research.Preparing highly active enhancing substrate is the prerequisite that obtains the SERS signal.Usually the method that obtains the high activity substrate has silver electrode method, silver sol method, silver strip method, silver mirror method etc., utilize silver mirror reaction prepare increased activity substrate method simple, strengthen effectively, thereby be used widely.But because silver and substrate surface in conjunction with the combination a little less than, the silver mirror on surface came off easily when substrate was worked in water, thereby lost enhancement function.
Summary of the invention
The object of the invention is to provide a kind of silver mirror to combine firm surface-enhanced Raman scattering activity substrate and preparation method thereof with substrate.
For reaching above-mentioned purpose, the present invention adopts following technical scheme: a kind of surface-enhanced Raman scattering activity substrate, comprise glass substrate, substrate surface is handled through sulfhydrylation, and the substrate surface of handling through sulfhydrylation deposits Ag nano particle decorative layer by silver mirror reaction.
The preparation method of surface-enhanced Raman scattering activity substrate comprises that substrate sulfhydrylation and substrate surface Ag nano particle decorative layer form step.
Also has substrate hydroxylation treatment step before the substrate sulfhydrylation.
In substrate hydroxylation step, in inert atmosphere, the substrate that cleans up was immersed in the mixed liquor that the hydrogen peroxide of the concentrated sulphuric acid of 80 ℃, 7 parts (parts by volume) weight percent concentration 98% and 3 parts of (parts by volume) weight percent concentration 30% forms 10 minutes; In substrate sulfhydrylation step, substrate is immersed 24 ℃, 10
-2Soaked 12 hours in the organic solution of the sulfydryl propyl trimethoxy silicane of M.
In substrate sulfhydrylation step, the organic solution of used sulfydryl propyl trimethoxy silicane is toluene solution, benzole soln or the aqueous isopropanol of sulfydryl propyl trimethoxy silicane; Form step at Ag nano particle decorative layer, mixed liquor, 25-30 that substrate is put into 2 parts of (parts by volume) glucose solutions and 1 part of (parts by volume) silver ammino solution ℃ soaked 1-3 minute, wherein glucose solution is dissolved in the solution that forms in the 500ml water for 10.8g glucose, and silver ammino solution is that the ammonia spirit adding 2g silver nitrate of 0.7M is dissolved in the solution that forms in the liquor argenti nitratis ophthalmicus that forms in the 300ml water.
Utilize substrate of the present invention to carry out different material SERS spectral detection, Raman spectrometer is the burnt Raman spectrometer of U1000 type copolymerization that French YOBIN-YVON company produces, the excitation source that spectrometer adopts is a Model265 type water-cooled Argon ion laser, excitation wavelength is 488nm, spectral resolution 1.5cm
-1, arriving the sample laser power is 5mv, 0.2 second integral time, stacking fold 10 times.According to SERS spectral detection to pyridine (Pypidine) molecule, 992,1025cm
-1Be the characteristic peak of the ring around absorbing dynamic model formula of pyridine, with 1008cm
-1The peak is interior mark, can estimate enhancer and be about 8 * 10
-5
Utilize the inventive method can form firm decorative layer with surface reinforced Raman active; Can carry out the Raman signal measurement of monofilm for a long time at aqueous phase.)
Description of drawings
Fig. 1 is the DFM figure of surface-enhanced Raman scattering activity substrate surface;
Fig. 2 is the SERS spectrum of pyridine (Pypidine) molecule, and wherein A is the Raman spectrum of pure pyridine, and B is 10
-3The SERS spectrum of M pyridine solution;
Fig. 3 is 10
-9The SERS spectrum of M rhodamine (Rhodamine) solution molecule;
Fig. 4 is the SERS spectrum of individual layer stearic acid (SA) molecular film;
Fig. 5 is the SERS spectrum of individual layer 18 ammonia (0A) molecular film;
Fig. 6 is the SERS spectrum of individual layer dipalmitoyl phosphatidylcholine (DPPC) molecular film;
Embodiment
Embodiment, a kind of surface-enhanced Raman scattering activity substrate comprise glass substrate, and substrate surface is handled through sulfhydrylation, and the substrate surface of handling through sulfhydrylation deposits Ag nano particle decorative layer by silver mirror reaction.The preparation of this substrate comprises that the processing of substrate hydroxylation, substrate sulfhydrylation and substrate surface Ag nano particle decorative layer form step.In substrate hydroxylation step, in inert atmosphere, the substrate that cleans up was immersed in the mixed liquor that the hydrogen peroxide of the concentrated sulphuric acid of 80 ℃, 7 parts (parts by volume) weight percent concentration 98% and 3 parts of (parts by volume) weight percent concentration 30% forms 10 minutes; In substrate sulfhydrylation step, substrate is immersed 24 ℃, 10
-2Soaked 12 hours in the toluene solution of M sulfydryl propyl trimethoxy silicane.Form step at Ag nano particle decorative layer, mixed liquor, 25-30 that substrate is put into 2 parts of (parts by volume) glucose solutions and 1 part of (parts by volume) silver ammino solution ℃ soaked 3 minutes, wherein glucose solution is dissolved in the solution that forms in the 500ml water for 10.8g glucose, and silver ammino solution is that the ammonia spirit adding 2g silver nitrate of 0.7M is dissolved in the solution that forms in the liquor argenti nitratis ophthalmicus that forms in the 300ml water.
Claims (5)
1, a kind of surface-enhanced Raman scattering activity substrate comprises glass substrate, it is characterized in that, substrate surface is handled through sulfhydrylation, and the substrate surface of handling through sulfhydrylation deposits Ag nano particle decorative layer by silver mirror reaction.
2, the preparation method of the described surface-enhanced Raman scattering activity substrate of claim 1 is characterized in that, comprises that substrate sulfhydrylation and substrate surface Ag nano particle decorative layer form step.
3, method as claimed in claim 2 is characterized in that, also has substrate hydroxylation treatment step before the substrate sulfhydrylation.
4, method as claimed in claim 3, it is characterized in that, in substrate hydroxylation step, in inert atmosphere, the substrate that cleans up was immersed in the mixed liquor that the hydrogen peroxide of the concentrated sulphuric acid of 80 ℃, 7 parts (parts by volume) weight percent concentration 98% and 3 parts of (parts by volume) weight percent concentration 30% forms 10 minutes; In substrate sulfhydrylation step, substrate is immersed 24 ℃, 10
-2Soaked 12 hours in the organic solution of the sulfydryl propyl trimethoxy silicane of M.
5, method as claimed in claim 4 is characterized in that, in substrate sulfhydrylation step, the organic solution of used sulfydryl propyl trimethoxy silicane is toluene solution, benzole soln or the aqueous isopropanol of sulfydryl propyl trimethoxy silicane; Form step at Ag nano particle decorative layer, mixed liquor, 25-30 that substrate is put into 2 parts of (parts by volume) glucose solutions and 1 part of (parts by volume) silver ammino solution ℃ soaked 1-3 minute, wherein glucose solution is dissolved in the solution that forms in the 500ml water for 10.8g glucose, and silver ammino solution is that the ammonia spirit adding 2g silver nitrate of 0.7M is dissolved in the solution that forms in the liquor argenti nitratis ophthalmicus that forms in the 300ml water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410010288 CN1699966A (en) | 2004-05-21 | 2004-05-21 | Surface reinforced Raman dissemination active substrate and production process thereof |
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| CN 200410010288 CN1699966A (en) | 2004-05-21 | 2004-05-21 | Surface reinforced Raman dissemination active substrate and production process thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024483B (en) * | 2007-03-27 | 2010-12-29 | 吉林大学 | Constituting method for metal ordered structure surface reinforced base |
| CN101676711B (en) * | 2008-09-21 | 2011-05-11 | 西北师范大学 | Substrate with surface-enhanced Raman scattering activity and preparation method thereof |
| CN101832932B (en) * | 2009-03-13 | 2011-09-14 | 中国科学院合肥物质科学研究院 | Method for detecting polychlorinated biphenyl by using silver nanometer tree branches and leaves |
| CN102285629A (en) * | 2011-05-05 | 2011-12-21 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN102632247A (en) * | 2012-04-20 | 2012-08-15 | 武汉大学 | Preparation method of load-type silver nano-composite material |
| CN102735675A (en) * | 2012-06-08 | 2012-10-17 | 中物院成都科学技术发展中心 | Surface-enhanced Raman spectrum substrate, and preparation method thereof |
| CN102103086B (en) * | 2009-12-16 | 2012-12-26 | 中国科学院理化技术研究所 | Method for detecting single molecule of single silicon nanowire in real time based on surface enhanced raman scattering effect |
| CN103364390A (en) * | 2012-04-10 | 2013-10-23 | 国家纳米科学中心 | Surface-enhanced Raman substrate, preparation method and application thereof |
| CN103868905A (en) * | 2012-12-13 | 2014-06-18 | 精工爱普生株式会社 | Optical device, detection apparatus, electronic apparatus, and method for producing optical device |
| CN106148925A (en) * | 2015-03-23 | 2016-11-23 | 中国科学院高能物理研究所 | A kind of preparation method of silver island material |
| CN107328750A (en) * | 2017-06-19 | 2017-11-07 | 吉林大学 | A kind of high activity, surface enhanced Raman scattering substrate of high homogeneity and preparation method thereof |
| CN108645838A (en) * | 2018-05-15 | 2018-10-12 | 上海应用技术大学 | A kind of method of dimehypo and Simanex field quick detection in tealeaves |
| CN109187489A (en) * | 2018-10-19 | 2019-01-11 | 福建师范大学 | A kind of preparation and application of bimolecular identification dopamine surface-enhanced Raman sensor |
| CN109406482A (en) * | 2018-10-19 | 2019-03-01 | 福建师范大学 | A method of detection dinotefuran |
| CN109837088A (en) * | 2019-04-10 | 2019-06-04 | 河南大学 | It is a kind of for enhancing the construction method of the plasma nano-array of quantum dot fluorescence |
| CN110068565A (en) * | 2019-06-06 | 2019-07-30 | 长江师范学院 | The application of SERS sensing chip and its detection method and preparation method |
| CN113466202A (en) * | 2021-06-18 | 2021-10-01 | 上海应用技术大学 | On-site rapid detection method for pesticide residues in fruit and vegetable samples |
| CN113838974A (en) * | 2021-09-24 | 2021-12-24 | 长江先进存储产业创新中心有限责任公司 | Phase change memory and preparation method thereof |
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2004
- 2004-05-21 CN CN 200410010288 patent/CN1699966A/en active Pending
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024483B (en) * | 2007-03-27 | 2010-12-29 | 吉林大学 | Constituting method for metal ordered structure surface reinforced base |
| CN101676711B (en) * | 2008-09-21 | 2011-05-11 | 西北师范大学 | Substrate with surface-enhanced Raman scattering activity and preparation method thereof |
| CN101832932B (en) * | 2009-03-13 | 2011-09-14 | 中国科学院合肥物质科学研究院 | Method for detecting polychlorinated biphenyl by using silver nanometer tree branches and leaves |
| CN102103086B (en) * | 2009-12-16 | 2012-12-26 | 中国科学院理化技术研究所 | Method for detecting single molecule of single silicon nanowire in real time based on surface enhanced raman scattering effect |
| CN102285629A (en) * | 2011-05-05 | 2011-12-21 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN102285629B (en) * | 2011-05-05 | 2014-03-26 | 厦门大学 | Preparation method for surface-enhanced Raman spectrum active substrate |
| CN103364390A (en) * | 2012-04-10 | 2013-10-23 | 国家纳米科学中心 | Surface-enhanced Raman substrate, preparation method and application thereof |
| CN102632247A (en) * | 2012-04-20 | 2012-08-15 | 武汉大学 | Preparation method of load-type silver nano-composite material |
| CN102632247B (en) * | 2012-04-20 | 2013-12-04 | 武汉大学 | Preparation method of load-type silver nano-composite material |
| CN102735675A (en) * | 2012-06-08 | 2012-10-17 | 中物院成都科学技术发展中心 | Surface-enhanced Raman spectrum substrate, and preparation method thereof |
| CN102735675B (en) * | 2012-06-08 | 2015-11-11 | 中物院成都科学技术发展中心 | Surface enhanced raman substrate and preparation method thereof |
| CN103868905A (en) * | 2012-12-13 | 2014-06-18 | 精工爱普生株式会社 | Optical device, detection apparatus, electronic apparatus, and method for producing optical device |
| CN106148925A (en) * | 2015-03-23 | 2016-11-23 | 中国科学院高能物理研究所 | A kind of preparation method of silver island material |
| CN107328750A (en) * | 2017-06-19 | 2017-11-07 | 吉林大学 | A kind of high activity, surface enhanced Raman scattering substrate of high homogeneity and preparation method thereof |
| CN107328750B (en) * | 2017-06-19 | 2020-02-04 | 吉林大学 | High-activity high-uniformity surface enhanced Raman scattering substrate and preparation method thereof |
| CN108645838A (en) * | 2018-05-15 | 2018-10-12 | 上海应用技术大学 | A kind of method of dimehypo and Simanex field quick detection in tealeaves |
| CN109187489A (en) * | 2018-10-19 | 2019-01-11 | 福建师范大学 | A kind of preparation and application of bimolecular identification dopamine surface-enhanced Raman sensor |
| CN109406482A (en) * | 2018-10-19 | 2019-03-01 | 福建师范大学 | A method of detection dinotefuran |
| CN109187489B (en) * | 2018-10-19 | 2021-01-05 | 福建师范大学 | Preparation and application of bimolecular recognition dopamine surface-enhanced Raman sensor |
| CN109837088A (en) * | 2019-04-10 | 2019-06-04 | 河南大学 | It is a kind of for enhancing the construction method of the plasma nano-array of quantum dot fluorescence |
| CN110068565A (en) * | 2019-06-06 | 2019-07-30 | 长江师范学院 | The application of SERS sensing chip and its detection method and preparation method |
| CN110068565B (en) * | 2019-06-06 | 2021-11-23 | 长江师范学院 | Application of SERS sensing chip and detection method and preparation method thereof |
| CN113466202A (en) * | 2021-06-18 | 2021-10-01 | 上海应用技术大学 | On-site rapid detection method for pesticide residues in fruit and vegetable samples |
| CN113838974A (en) * | 2021-09-24 | 2021-12-24 | 长江先进存储产业创新中心有限责任公司 | Phase change memory and preparation method thereof |
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