CN102706857B - Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate - Google Patents
Preparation method of multifunctional surface enhanced raman scattering (SERS) substrate Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 35
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 20
- 239000002071 nanotube Substances 0.000 claims abstract description 19
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000003491 array Methods 0.000 claims abstract description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001432 tin ion Inorganic materials 0.000 claims abstract description 4
- 239000002073 nanorod Substances 0.000 claims abstract description 3
- 230000000694 effects Effects 0.000 claims description 11
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 26
- 239000011787 zinc oxide Substances 0.000 description 15
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 239000004408 titanium dioxide Substances 0.000 description 8
- 238000001237 Raman spectrum Methods 0.000 description 5
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 5
- 239000004312 hexamethylene tetramine Substances 0.000 description 5
- 229960004011 methenamine Drugs 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 4
- VYXSBFYARXAAKO-UHFFFAOYSA-N ethyl 2-[3-(ethylamino)-6-ethylimino-2,7-dimethylxanthen-9-yl]benzoate;hydron;chloride Chemical compound [Cl-].C1=2C=C(C)C(NCC)=CC=2OC2=CC(=[NH+]CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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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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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明提供了一种多功能表面增强拉曼散射基底的制备方法。该方法包括以下步骤：（1）通过将毛细管内壁先铺上一层ZnO种子，在Zn(NO3)2和HMT溶液中先生长ZnO纳米棒阵列，将毛细管浸于(NH4)2TiF6和H3BO3中反应即可得到TiO2的纳米管阵列；（2）将已经生长有TiO2纳米管浸于SnCl2中使表层吸附一层二价锡离子，再通过将其浸于Ag(NH3)2 +中使其还原成银颗粒而得到。与传统的SERS基底相比较而言，本发明基于毛细管的多功能SERS基底兼具拉曼增强和重复使用的功能，同时该种基底也很方便携带、便于取样，可以实现实时的现场检测。
The invention provides a preparation method of a multifunctional surface-enhanced Raman scattering substrate. The method includes the following steps: (1) First grow ZnO nanorod arrays in Zn(NO 3 ) 2 and HMT solution by spreading a layer of ZnO seeds on the inner wall of the capillary, and immerse the capillary in (NH 4 ) 2 TiF 6 React with H 3 BO 3 to get TiO 2 nanotube array; (2) Immerse the grown TiO 2 nanotubes in SnCl 2 to absorb a layer of divalent tin ions on the surface, and then immerse it in Ag (NH 3 ) 2 + to reduce it to silver particles. Compared with the traditional SERS substrate, the capillary-based multifunctional SERS substrate of the present invention has the functions of Raman enhancement and reusability. At the same time, the substrate is also very convenient to carry and sample, and can realize real-time on-site detection.
Description
Technical field
The present invention relates to a kind of analysis and detection technology, be specifically related to a kind of Raman spectrum method for detecting surface reinforcement.
Background technology
Raman scattering is nineteen twenty-eight, by India scientist C.V. Raman, tests in test discovery, thereby this phenomenon is called Raman scattering, is in brief: when light can be changed by occurrence frequency by the light of molecular scattering through transparent medium.Raman spectrum is the same with infrared spectrum be all reflection molecular vibration-rotational energy level information, but the signal of Raman scattering very a little less than, its intensity only have 1,000,000 of incident intensity/, thereby by scientific circles, do not paid attention to widely one period at the beginning of finding.Until 1974, the people such as Fleishmann are carrying out after roughening processing smooth silver electrode surface, obtain first the high-quality Raman spectrum that is adsorbed on unimolecular layer Pyridine Molecules in silver electrode surface, its intensity is compared with the Raman scattering signal of pyridine in solution phase, strengthen approximately 6 orders of magnitude (1,000,000 times), this Raman enhancement effect relevant with rough surface is called as Surface enhanced raman spectroscopy (Surface Enhanced Raman Scattering, SERS) effect.From then on, SERS becomes a new study hotspot gradually.
After SERS effect is found, the various SERS substrates that have Raman to strengthen effect are constantly produced out, have that superpower Raman strengthens effect, the easy SERS substrate being easy to get is the focus of research always, in recent years, the various continuous studied personnel of SERS substrate with different-shape structure make, although detectability reaches 10
-12-10
-14the SERS substrate of M studied personnel is reported, but the preparation process of these SERS substrates is complicated, and equipment needed thereby is expensive, and cannot reuse, and can cause the waste of energy resources, from practicality, also has a certain distance, can only in laboratory, exist.Although there is the SERS substrate of higher enhancement effect, be the target that Science Institute is pursued, obtain a kind of more practical and cheap SERS substrate and seem more important.
Summary of the invention
1. the technical matters that invention will solve
The present invention overcome the deficiencies in the prior art provide a kind of sampling facilitate, be easy to carry, reusable, can be for the SERS substrate with Raman enhancement effect of Site Detection.
2. technical scheme
In order to solve above technical matters, the present invention is achieved by the following technical programs.
Multifunction surface strengthens a preparation method for Raman spectrum substrate, comprises the following steps:
(1) at capillary tube inner wall, construct TiO
2nano-tube array: by by the first layer overlay ZnO of capillary tube inner wall seed, at Zn (NO
3)
2with first growing ZnO nanorod arrays in HMT solution, kapillary is dipped in to (NH
4)
2tiF
6and H
3bO
3middle reaction can obtain TiO
2nano-tube array;
(2) again by silver-colored particle modification at TiO
2surface: have TiO by growing
2nanotube is dipped in SnCl
2in make top layer absorption one deck divalent tin ion, then by being dipped in Ag (NH
3)
2 +in make it be reduced into silver-colored particle and obtain;
Utilize TiO
2the photocatalytic degradation function of nanotube and silver-colored Raman enhancement effect, make this substrate can be used as multi-functional SERS substrate.
The principles of science of the present invention is analyzed:
One, capillary tube inner wall is first used to Zn (Ac)
2ethanolic solution process, at 350 ℃, process 20min, make capillary tube inner wall produce layer of ZnO seed.There is the kapillary of ZnO seed to be dipped in Zn (NO inwall
3)
2with hexamethylene tetramine (HMT) solution reacts at 90 ℃, can obtain the nanometer stick array of zinc paste, through at (NH
4)
2tiF
6and H
3bO
3middle reaction can obtain the nano-tube array of titanium dioxide.Because titania has the function of photocatalytic degradation, therefore, this SERS active substrate will produce photodegradative effect, thereby makes it have the function that repeats can be recycled.
Two, in titania nanotube finishing after silver-colored particle, because silver has SERS enhancement effect, can produce Raman and strengthen, thereby make to have Raman enhancing and reusable function concurrently based on multi-functional SERS substrate capillaceous.
3. beneficial effect
Traditional SERS substrate is all constructed in plane, when practical operation, other instruments for object solution (as liquid-transfering gun) to be measured need to be dripped in substrate, after dry, under Raman spectrum, detect, its operation steps is more, be inconvenient to carry, be unsuitable for Site Detection.The present invention is based on SERS substrate capillaceous because capillary action can not need the non-productive operation of other instruments, simultaneously because inwall growth has one deck TiO
2array, makes it have the performance of photocatalytic degradation, can realize reusing of SERS substrate, and required sample size few, be easy to carry, be convenient to sampling, can realize real-time Site Detection.
Accompanying drawing explanation
Fig. 1 is Multifunctional fur tubule surface enhanced Raman substrate preparation method's of the present invention technical scheme schematic diagram.
Fig. 2 is that ZnO array changes TiO into
2the scanning electron microscope of array (SEM) figure.
Fig. 3 is scanning electron microscope (SEM) figure of the nano-particle modified Nano tube array of titanium dioxide of Ag.
Fig. 4 for to adsorb the Raman spectrogram after R6G in the multi-functional SERS substrate of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated.
As shown in Figure 1, multi-functional capillary surface strengthens Raman substrate preparation method and comprises the following steps: A: at capillary tube inner wall, by the method for thermal decomposition, produce layer of ZnO seed, then allow kapillary at Zn (NO
3)
2with HMT growth from solution ZnO array; B: change ZnO array into TiO
2array; C: at TiO
2the outer above silver-colored particle of modifying of nanotube.
Fig. 2 is that ZnO array changes TiO into
2the scanning electron microscope diagram of array.It is comprised of A, B, C, D tetra-parts, wherein, and A: the nanometic zinc oxide rod array scanning electron microscope (SEM) photograph of growing on a large scale; B: large-scale Nano tube array of titanium dioxide scanning electron microscope (SEM) photograph; C: the partial enlarged drawing to figure A, the nanometic zinc oxide rod array of visible proper alignment; D: the partial enlarged drawing to figure B, can see Nano tube array of titanium dioxide neat grow in capillary tube inner wall.
Fig. 3 is scanning electron microscope (SEM) figure of the nano-particle modified Nano tube array of titanium dioxide of Ag.It is comprised of A, B two parts, wherein, and A: the scanning electron microscope (SEM) photograph of the Nano tube array of titanium dioxide of capillary tube inner wall silver particle modification; B: to the partial enlarged drawing of figure A, visible silver-colored particle is modified at the surface of titanium oxide nanotubes uniformly.
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to following embodiment.
At capillary tube inner wall, construct TiO
2nano-tube array:
First, make the ethanolic solution of zinc acetate enter kapillary inside, in baking oven 60 degrees Celsius draw under condition dry after, under the condition of 350 degrees Celsius, anneal 20 minutes, so just can make the seed of its inwall generation one deck zinc paste.Then, this kapillary is placed in to Zn (NO
3)
2with in HMT solution, under 90 degree, react 90 minutes, can be at the inwall layer of ZnO array of growing.ZnO array is at (NH
4)
2tiF
6and H
3bO
3middle reaction 90 minutes, just can obtain the nano-tube array of titanium dioxide.Fig. 2 A and C are respectively the SEM photos of the zinc oxide array under different amplification, the visible interior zinc oxide array distributing on a large scale; Fig. 2 B and D are replaced into zinc paste in the SEM photo of titanium dioxide.
By silver-colored particle modification at TiO
2surface:
Have the kapillary of titania nanotube array to be first dipped in the sub-tin aqueous solution of dichloro of 0.05g/20mL growth, after one hour, with intermediate water, rinse for several times, titania surface can be adsorbed one deck divalent tin ion like this.Be placed on again in the silver ammino solution of 1mmol/L, after 30 minutes, take out, clean, can obtain the titania nanotube array of silver-colored particle modification, as shown in Figure 3.
Whether detect SERS substrate of the present invention possesses Raman enhancing and reuses function:
In substrate, adsorb 10
-5the R6G(chemistry rhodamine 6G by name of mol/L) after ethanolic solution, under Raman spectrometer, detect, can obtain stronger enhancing signal, and substrate is through after photocatalytic degraded, SERS blackout, substrate still can be used after reusing 5 times, and signal is without obviously weakening.As shown in Figure 4,1～5 signal representing respectively after substrate absorption R6G; The SERS signal of " light degradation " representative after photocatalytic degraded, can find out the characteristic peak that there is no R6G.More than experimental results show that this substrate has Raman enhancing function and possesses the organic function of catalytic degradation simultaneously, can recycle.
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| CN102944544B (en) * | 2012-11-08 | 2015-01-21 | 清华大学 | Recycling surface-reinforced Raman scattering substrate as well as preparation method and application |
| CN103048304A (en) * | 2012-12-07 | 2013-04-17 | 江苏大学 | Preparation method of recyclable surface-enhanced Raman-spectrum active substrate |
| CN103018462B (en) * | 2012-12-18 | 2016-05-18 | 西南大学 | Nano oxidized Zinc modified immune capillary and its preparation method and application |
| CN103257134A (en) * | 2013-04-18 | 2013-08-21 | 东南大学 | Method for preparing surface-enhanced Raman scattering (SERS) substrate based on capillary tube |
| CN104164698B (en) * | 2014-07-25 | 2016-08-24 | 中国科学院理化技术研究所 | Method for improving surface enhanced Raman scattering signal of single crystal zinc oxide nano rod |
| CN105372223A (en) * | 2015-10-20 | 2016-03-02 | 安徽理工大学 | A Ag/TiO2 flexible, reusable SERS substrate and its preparation method |
| CN109112601B (en) * | 2018-07-30 | 2021-04-06 | 合肥工业大学 | Based on TiO2Preparation method and application of Ag nano array photoinduction enhanced Raman substrate |
| CN109932351B (en) * | 2019-03-15 | 2021-11-19 | 佳木斯大学 | TiO 22Preparation method of/ZnO semiconductor heterojunction SERS active substrate |
| CN110487769A (en) * | 2019-06-28 | 2019-11-22 | 江汉大学 | A kind of preparation method and applications of titanic oxide nanorod array/argentum nano composite material |
| CN111122538B (en) * | 2019-12-23 | 2022-07-12 | 中国科学院合肥物质科学研究院 | A surface-enhanced Raman spectroscopy substrate based on target molecule partitioned space-occupying capillary and its preparation method and application |
| CN112098390B (en) * | 2020-09-16 | 2021-12-14 | 燕山大学 | Surface enhanced Raman scattering substrate and preparation method thereof |
| CN115639184A (en) * | 2022-10-25 | 2023-01-24 | 山东师范大学 | Preparation method and application of Raman-enhanced active substrate for small molecule screening and enrichment |
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