CN108318472A - A kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed - Google Patents
A kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed Download PDFInfo
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- 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
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- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The invention discloses a kind of preparation methods for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed.The preparation method includes the following steps：Prepare hydrofluoric acid, the mixed solution of silver nitrate and CTAB；Mixed solution is added to silicon chip surface；After reaction, silicon chip is rinsed well with deionized water, nitrogen drying；Wherein, hydrofluoric acid concentration 10‑3~10 M, silver nitrate concentration 10‑4~1 M, CTAB a concentration of 10‑6~1 M.Compared with the conventional method, the present invention has the following advantages：(1) it is answered using simple redox side, preparation process is simple and convenient, of low cost；(2) substrate prepared by is reproducible；(3) high sensitivity, when using rhodamine 6G molecule as probe, detection limit is up to 10‑14M；(4) can be achieved be measured in real time in the solution, quickly analyze, with common dry impregnation absorption need 1 hour even more long compared with, detection speed is fast.
Description
Technical field
The present invention relates to Raman detection technical fields, increase more particularly, to a kind of surface that high sensitivity is quickly analyzed
The preparation method of strong Raman scattering substrate.
Background technology
Raman spectrum (Raman spectra), is a kind of scattering spectrum.Raman spectrum analysis method is to be based on India scientist
C.V. the Raman scattering effect that Raman (Raman) is found, a pair scattering spectrum different from incident light frequency are analyzed to obtain
To molecular vibration, rotation aspect information, and applied to a kind of analysis method of molecular structure research.1974, surface enhanced was drawn
Graceful scattering is found for the first time.However, due to the backwardness of laser technology, Surface enhanced Raman scattering field develops slowly.In recent years
Come, due to the development of laser and spectral technique, Surface enhanced Raman spectroscopy is as a kind of important surface analysis tool by more
Carry out more concerns, is widely used in the fields such as biological detection, environmental monitoring, chemical analysis and food security.
Surface-enhanced Raman (Surface-Enhanced Raman Scattering, abbreviation SERS), with common Raman
Spectrographic determination is adsorbed on the sample of colloid metallic particles such as silver, gold or copper surface, or is adsorbed on the coarse table of these sheet metals
Sample on face.Although reason is still uncertain, it has been found that the intensity of sample its Raman spectrum adsorbed can be improved 103~106
Times.It is mainly used for the state parsing etc. of adsorbing species.The sensitivity one of existing surface enhanced Raman substrate detection rhodamine 6G
As be 10-10~10-12。
After SERS effects are found, the various SERS substrates for having Raman enhancing effect are constantly produced out how
It obtains and is had been a hot spot of research with Raman enhancing effect, the easy SERS substrates being easy to get.Currently used for preparing SERS activity
The method of substrate mainly has sol-gel method, electrochemical deposition, LB to form a film, template, nanometer embossing etc., but these
The preparation process of SERS substrates is complicated, and required equipment is expensive, can cause the waste of energy resources.
In addition, carrying out Raman detection, need first to be adsorbed on determinand molecule in Raman substrate.It is conventional at present to use
Be dry impregnation absorption, generally require and Raman substrate be immersed in determinand solution 1 hour even more long, can just make to be measured
Object molecule is fully adsorbed in Raman substrate.This process causes detection time long, can not be measured in real time in the solution, soon
The surface enhanced Raman scattering substrate of speed analysis.
The high sensitivity for lacking a kind of preparation that can be simple and fast now and being detected may be implemented to detect in real time fast
The Raman substrate of speed analysis, this is serious to constrain the application of Raman detection in practice.
Invention content
The first purpose of the invention is to provide a kind of surface enhanced Raman scattering substrates that high sensitivity is quickly analyzed
Preparation method, preparation method convenience simple for process are of low cost.
Second object of the present invention is to provide the surface enhanced Raman scattering substrate that the preparation method is prepared, system
Standby substrate is reproducible, high sensitivity.
Third object of the present invention is to provide application of the surface enhanced Raman scattering substrate in Raman detection, institutes
It states surface enhanced Raman scattering substrate and can realize and be measured in real time in the solution, quickly analyze.
Fourth object of the present invention is to provide a kind of real-time detection method of Raman detection, the detection method detection speed
Degree is fast.
To achieve the goals above, the present invention is achieved by the following technical programs：
A kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed, preparation process include with
Lower step：
S1. hydrofluoric acid, the mixed solution of silver nitrate and CTAB are prepared；
S2. the mixed solution prepared by step S1 is added to silicon chip surface；
S3. after reacting, silicon chip is rinsed well with deionized water, nitrogen drying；
Wherein, hydrofluoric acid concentration 10-3~10M, silver nitrate concentration 10-4~1M, CTAB a concentration of 10-6~1M.
Preferably, hydrofluoric acid concentration described in step S1 is 0.75~5M, and silver nitrate concentration is 0.01~0.1M, and CTAB is dense
Degree is 0.005~0.05M
It is highly preferred that hydrofluoric acid concentration described in step S1 is 3M, silver nitrate concentration 0.06M, CTAB is a concentration of
0.01M。
Preferably, silicon chip described in step S2 is cleaned before use, nitrogen drying.
Preferably, the time reacted described in step S3 is 0.5~30min.
It is highly preferred that the time reacted described in step S3 is 5min.
The surface enhanced Raman scattering substrate that the preparation method is prepared, also belongs to protection scope of the present invention.
Application of the surface enhanced Raman scattering substrate in Raman detection, also belongs to protection scope of the present invention.
A kind of detection method of Raman detection, the surface enhanced Raman scattering substrate are immersed in detected sample, into
Row detection in real time.
In the present invention, directly by hydrofluoric acid, the mixed solution dropwise addition of silver nitrate and CTAB are in silicon chip surface, one timing of reaction
Between, you can prepare surface enhanced Raman scattering substrate that is highly sensitive, being measured in real time in the solution in silicon chip surface.
Compared with prior art, the present invention has the advantages that：
The present invention provides a kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed.With
Existing method is compared, and the present invention has the following advantages：(1) it being answered using simple redox side, preparation process is simple and convenient, at
This is cheap；(2) substrate prepared by is reproducible；(3) high sensitivity, when using rhodamine 6G molecule as probe, detection limit is reachable
10-14M；(4) it can be achieved to be measured in real time in the solution, quickly analyze, needs are adsorbed 1 hour very with common dry impregnation
To comparing more long, detection speed is fast.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the surface enhanced Raman scattering substrate prepared by embodiment 1.
Fig. 2 is for surface enhanced Raman scattering substrate prepared in embodiment 1 with comparative example 1 in the solution to rhodamine 6G
(5×10-14M the Raman spectrogram) being detected.
Fig. 3 is surface enhanced Raman scattering substrate prepared in embodiment 1 in the solution to rhodamine 6G (5 × 10- 10M it) is detected, has taken the Raman spectrogram of 30 positions at random.
Fig. 4 is the scanning electron microscope (SEM) photograph of the surface enhanced Raman scattering substrate prepared by comparative example 1.
Specific implementation mode
The present invention is made with specific embodiment with reference to the accompanying drawings of the specification and further being elaborated, the embodiment
It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Test method used in following embodiments is such as without spy
Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained
And material.
Embodiment 1
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 3M hydrofluoric acid, the mixed solution of 0.06M silver nitrates and 0.01M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
It in rhodamine 6G, is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, time of integration 0.1s, accumulation
Number 10 times.
As a result it shows：The scanning electron microscope (SEM) photograph of the surface enhanced Raman scattering substrate of preparation is as shown in Figure 1, detection rhodamine 6G
(5×10-14M Raman spectrogram) has taken 30 positions, has detected sieve at random as shown in Fig. 2, in order to verify the repeatability of substrate
Red bright 6G (5 × 10-10M Raman spectrogram) is as shown in Figure 3.
Embodiment 2
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1. 3M hydrofluoric acid, the mixed solution of 0.06M silver nitrates and 0.005M CTAB are prepared；
S2. the mixed solution prepared by step S1 is added dropwise in silicon chip surface；
S3. 5min is reacted, silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-10M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 3
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1. 3M hydrofluoric acid, 0.06M silver nitrates and 5 × 10 are prepared-5The mixed solution of M CTAB；
S2. the mixed solution prepared by step S1 is added dropwise in silicon chip surface；
S3. 5min is reacted, silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-7M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 4
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 3M hydrofluoric acid, 0.06M silver nitrates and 2 × 10-4The mixed solution of M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-8M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 5
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 3M hydrofluoric acid, the mixed solution of 0.06M silver nitrates and 0.02M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-11M it in), is measured in real time, optical maser wavelength used is 532nm, power 2.4mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 6
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 3M hydrofluoric acid, the mixed solution of 0.06M silver nitrates and 0.015M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-9M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 7
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 10-3M hydrofluoric acid, 10-4M silver nitrates and 10-6The mixed solution of M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-14M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 8
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 10M hydrofluoric acid, the mixed solution of 1M silver nitrates and 1M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-14M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 9
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 0.75M hydrofluoric acid, the mixed solution of 0.01M silver nitrates and 0.005M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-14M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Embodiment 10
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 5M hydrofluoric acid, the mixed solution of 0.1M silver nitrates and 0.05M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-14M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, there is stronger Raman signal.
Comparative example 1
A kind of preparation method of surface enhanced Raman scattering substrate, includes the following steps：
S1. 3M hydrofluoric acid and 0.06M silver nitrate mixed solutions are prepared；
S2. the mixed solution prepared by step S1 is added dropwise in silicon chip surface；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-14M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times.
As a result it shows：Fig. 4 is the scanning electron microscope (SEM) photograph of prepared surface enhanced Raman scattering substrate, and Raman spectrogram is as schemed
Shown in 2, occur without Raman signal.
Comparative example 2
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 15M hydrofluoric acid, the mixed solution of 2M silver nitrates and 2M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-10M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, occurs without Raman signal.
Comparative example 3
A kind of high sensitivity, the preparation method for the surface enhanced Raman scattering substrate quickly analyzed, includes the following steps：
S1 prepares 10-4M hydrofluoric acid, 10-5M silver nitrates and 10-7The mixed solution of M CTAB；
Mixed solution prepared by step S1 is added dropwise in silicon chip surface S2；
S3 reacts 5min, and silicon chip is rinsed well, nitrogen drying.
The highly sensitive surface enhanced Raman scattering substrate being prepared according to above-mentioned steps is immersed in be detected
Rhodamine 6G (5 × 10-10M it in), is measured in real time, optical maser wavelength used is 532nm, power 0.14mw, and the time of integration is
0.1s, cumulative frequency 10 times, obtains Raman spectrogram, occurs without Raman signal.
Claims (9)
1. a kind of preparation method for the surface enhanced Raman scattering substrate that high sensitivity is quickly analyzed, which is characterized in that including with
Lower step：
S1. hydrofluoric acid, the mixed solution of silver nitrate and CTAB are prepared；
S2. the mixed solution prepared by step S1 is added to silicon chip surface；
S3. after reacting, silicon chip is rinsed well with deionized water, nitrogen drying；
Wherein, hydrofluoric acid concentration 10-3~10 M, silver nitrate concentration 10-4~1 M, CTAB a concentration of 10-6~1 M.
2. preparation method according to claim 1, which is characterized in that hydrofluoric acid concentration described in step S1 is 0.75~5 M,
Silver nitrate concentration is 0.01~0.1 M, a concentration of 0.005~0.05 M of CTAB.
3. preparation method according to claim 1, which is characterized in that hydrofluoric acid concentration described in step S1 is 3 M, nitric acid
Silver concentration is 0.06 M, a concentration of 0.01 M of CTAB.
4. preparation method according to claim 1, which is characterized in that silicon chip described in step S2 is carried out clearly using preceding
It washes, nitrogen drying.
5. preparation method according to claim 1, which is characterized in that the time reacted described in step S3 is 0.5~30
min。
6. preparation method according to claim 5, which is characterized in that the time reacted described in step S3 is 5 min.
7. the surface enhanced Raman scattering substrate that claim 1~6 preparation method is prepared.
8. application of the surface enhanced Raman scattering substrate described in claim 7 in Raman detection.
9. a kind of real-time detection method of Raman detection, which is characterized in that by Surface enhanced Raman scattering base described in claim 7
Bottom is immersed in detected sample.
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| CN109187487A (en) * | 2018-09-27 | 2019-01-11 | 肇庆市华师大光电产业研究院 | A kind of ag nano-cluster surface enhanced Raman scattering substrate and its preparation method and application |
| CN109321904A (en) * | 2018-09-27 | 2019-02-12 | 肇庆市华师大光电产业研究院 | A kind of metal Nano structure array and its preparation method and application of controllable pattern |
| CN109342389A (en) * | 2018-10-19 | 2019-02-15 | 肇庆市华师大光电产业研究院 | A kind of visual surface enhanced Raman scattering substrate and its preparation method and application |
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