CN110412007A - A kind of Raman spectrum base, preparation method and application - Google Patents
A kind of Raman spectrum base, preparation method and application Download PDFInfo
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- CN110412007A CN110412007A CN201910654378.6A CN201910654378A CN110412007A CN 110412007 A CN110412007 A CN 110412007A CN 201910654378 A CN201910654378 A CN 201910654378A CN 110412007 A CN110412007 A CN 110412007A
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- 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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Abstract
The disclosure belongs to raman spectrum substrate technical field, and in particular to a kind of Raman spectrum base, preparation method and application.Electromagnetic enhancement Raman regulating and controlling effect is common surface Raman enhancement method in the art, but Electromagnetic enhancement method still has limitation, limits quick, in situ detection to molecule to a certain extent.Present disclose provides a kind of Raman spectrum bases, using piezoelectric material as substrate, surface coated with nano metallic particles.When pressing to the substrate, the pressure conversion of impression can be electric signal by piezoelectric material, form Raman reinforcing effect by metal nanoparticle.Verified, this method has good stability, and can obtain suitable detection effect by adjusting the size of impressed pressure, has good dissemination.
Description
Technical field
The disclosure belongs to raman spectrum substrate technical field, specifically relates to a kind of Raman enhancing base of flexible piezoelectric modulating properties
Bottom, preparation method and application.
Background technique
The information for disclosing the background technology part is merely intended to increase the understanding to the general background of the disclosure, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
A kind of " dactylogram " of the Surface Enhanced Raman Scattering Spectrum as molecule has been benefited since 1974 find for the first time
In unique advantages such as high specificity, high sensitivity, fast response times, it is widely applied to food safety, environmental monitoring, life
The fields such as object medicine and medical diagnosis on disease.Normal Raman scattering effect is very faint, and luminous intensity is only the 10 of incident intensity-10, need
Raman study is carried out to adsorption species by enhancement effect.Benefit, which is prepared with simple method, can be realized environment point
Extensive concern of sub, biomolecule in situ detection the surface enhanced Raman substrate by scientific research personnel.Currently used Raman increases
Strong approach includes the electromagnetic field intensity for changing surrounding molecules or the polarizability for changing molecule, i.e. Electromagnetic enhancement and Chemical enhancement.
Since electromagnetic field can regulate and control the plasma resonance of metal Nano structure, electricity regulation surface Raman enhancement exists
Unique advantage is highlighted in numerous different types of technologies, but still there is certain limitation.It has been recognised by the inventors that restricting electricity
In terms of the key factor of regulation surface enhanced Raman technique development mainly has following two, first, using Electromagnetic enhancement effect
It when carrying out Raman spectrum detection, needs will test device and is placed in electrochemistry sample cell and carry out, will limit detection to a certain extent
Progress；Second, substrate does not need only to have the urn Topography of achievable signal enhancing, and require substrate conductive.
Therefore electricity regulation surface enhanced Raman technique quick, the in situ detection difficult to realize to molecule is utilized.
Summary of the invention
For above-mentioned problems of the prior art, present disclose provides a kind of, and the Raman with piezoelectricity modulating properties increases
Strong basis bottom.The Raman enhancing substrate, which uses, has piezoelectric property material as substrate, is formed and is drawn by the nano metal on surface
Graceful enhancing substrate, in such a way that substrate surface is pressed to form potential difference, it can be achieved that Electromagnetic enhancement effect to Raman spectrum.
The enhancing substrate needs will test device when can be to avoid traditional electricity regulation Surface Raman Spectra detection and is placed in extra electric field
Step, position and weight by adjusting impressed pressure provide a kind of more flexible electric control methods, are advantageously implemented pair
Quick, the in situ detection of molecule.
In order to realize above-mentioned technical effect, the disclosure the following technical schemes are provided:
For the disclosure in a first aspect, providing a kind of Raman spectrum base, the substrate uses piezoelectric material surface
Coated with nano metallic particles.
It is known in the art that the piezoelectric material is under pressure voltage can occurs between both ends of the surface when acting on, potential difference is formed.
Raman scattering effect can occur by increasing nano-metal particle formation rough surface in piezoelectric material surface, become a kind of surface
The Raman substrate of enhancing.Through the disclosure studies have shown that the Raman substrate of which preparation can be realized by regulation impressed pressure
To the humidification of Raman scattering, reinforcing effect is flexibly stablized.
Preferably, the piezoelectric material includes Kynoar, piezoelectric ceramics.
The piezoelectric material is preferably Kynoar (PVDF), and presently found PVDF includes at least five kinds of crystal phases, point
Not Wei α phase, β phase, γ phase, δ phase and ε phase, it is best with the piezoelectric property of β phase, γ phase.PVDF material itself is a kind of flexible material
Material has good flexibility, and weather resistance is good, stable chemical performance, piezoelectric modulus are high, impact resistance pressure.Using gathering inclined fluorine
As substrate, the mode of impressed pressure is not easy to damage this toughness substrate ethylene, has more compared to stiffened piezoelectric material
Good application value.
Preferably, the nano-metal particle is silver nanoparticle, gold nano or copper nano particles；It is further preferred that for silver
Nano particle.
Three kinds of common gold, silver, copper made of metal are in the art for rough surface, wherein and silver nano-grain cost is more cheap,
And preparation Raman substrate better performances wherein, common silver nano-grain include cube, cut off cube, positive bipyramid,
Rodlike, spheroid, triangular plate and threadiness.Through the disclosure studies have shown that using silver nanowires preparation enhancing substrate effect most
Good, the silver nanowires on the surface PVDF not still plasma active structure can also form surface plasmon resonance to right
Surface-enhanced raman scattering is enhanced, and is also flexible conducting material, plays conductive effect.
Even more important, disclosure research discovery: cooperated using silver nano-grain and PVDF piezoelectric material, silver nano-grain
The accounting that β phase in PVDF material can be increased improves the piezoelectric property of PVDF.The disclosure in substrate by placing different quality
Counterweight construct impressed pressure, come realize to Raman enhancing substrate electricity regulation.Counterweight is placed on the piezoelectric materials, can make to press
Electric material forms potential difference on surface, to there is certain humidification to Raman spectrum.And the Raman of the counterweight of different quality
Enhancement effect is different, and is based on the studies above as a result, the disclosure realizes that being based on regulation impressed pressure regulation Raman increases for the first time
The preparation at strong basis bottom.
Disclosure second aspect provides a kind of preparation method of Raman spectrum base, the method includes with
Lower step: metal nano solution is added dropwise and forms it into form uniform film in piezoelectric material surface.
Preferably, the metal nano solution is gold nano, silver nanoparticle or copper nano-solution；It is further preferred that institute's silver
Nano-solution is silver nanowires solution.
In some specific embodiments, the partial size of the silver nanowires is 60~70nm or length is 11~13 μm.It grinds
Study carefully and show that the length of silver nanowires is longer, diameter is smaller, and light transmittance is higher, resistance is smaller.
Preferably, the metal nano solution is the alcoholic solution of metal nano, uniform through ultrasonic vibration.
Preferably, the piezoelectric material is PVDF material.
Preferably, the metal nano solution is added dropwise after piezoelectric material surface, and drying obtains uniform film.
The disclosure third aspect provides Raman spectrum base described in first aspect in Raman spectrum context of detection
Application.
Compared with prior art, the beneficial effect of the disclosure is:
The surface-enhanced Raman detection of electricity regulation is placed in electrochemistry sample cell by needing will test equipment in the prior art
Middle progress operates relatively complicated, in some instances it may even be possible to will affect the progress of detection.Present disclose provides a kind of drawings with piezoelectric property
Graceful spectrum substrate, using piezoelectric material as substrate, surface metallization nano particle makes rough surface, by piezoelectric material
Electric signal is converted to Raman enhancement effect, provides a kind of flexible, stable, easily operated electricity regulation Raman spectrum detection side
Method.
Detailed description of the invention
The Figure of description for constituting a part of this disclosure is used to provide further understanding of the disclosure, and the disclosure is shown
Meaning property embodiment and its explanation do not constitute the improper restriction to the disclosure for explaining the disclosure.
Fig. 1 is the schematic diagram that Raman spectrum base is prepared in embodiment 1.
Fig. 2 is surface enhanced Raman substrate electron microscope scanning figure in embodiment 1；
Wherein, Fig. 2 (a) is flexible PVDF thin film, and Fig. 2 (b) is the silver nanowires uniformly adhered in PVDF thin film.
Fig. 3 is the Fourier infrared absorption spectrogram of pure PVDF and the PVDF for being added to Ag nano wire.
Fig. 4 is the placement that Raman prepared in embodiment 1 enhances substrate and general substrate obtains rhodamine 6G (R6G)
Raman enhanced spectrum compares figure when not placing counterweight.
Fig. 5 is that Raman prepared by embodiment 1 enhances substrate rhodamine 6G obtained when placing the counterweight of different quality
(R6G) Raman enhanced spectrum figure.
Fig. 6 is that Raman enhances base pressure performance of control figure in embodiment 1；
Wherein, the counterweight that Fig. 6 (a) is 50g, which is placed on Raman, enhances the schematic diagram of substrate different location；
Fig. 6 (b) is that Raman enhances Raman enhancing base of the substrate in different location by the pressure of 50g counterweight in embodiment 1
Bottom detects the Raman enhanced spectrum figure of R6G molecule.
Fig. 7 is the Raman that Raman enhances substrate glucose solution obtained under the pressure of the counterweight of 50g in embodiment 5
Enhanced spectrum figure.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the disclosure.Unless another
It indicates, all technical and scientific terms used herein has usual with disclosure person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the disclosure.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As background technique is introduced, Electromagnetic enhancement is common surface Raman enhancement method in the art, but electricity
Magnetic field-enhanced method still has limitation, limits quick, in situ detection to molecule to a certain extent.The disclosure provides
A kind of Raman spectrum base, using piezoelectric material as substrate, surface coated with nano metallic particles is a kind of soft
Property, Raman spectrum base with piezoelectric property.
In order to enable those skilled in the art can clearly understand the technical solution of the disclosure, below with reference to tool
The technical solution of the disclosure is described in detail in the embodiment and comparative example of body.
Embodiment 1
A kind of preparation method of the Raman spectrum base of flexible piezoelectric modulating properties, including following preparation step
It is rapid:
The silver nanowires solution that concentration is 10mg/ml is carried out ultrasonic vibration 10~20 minutes first, is cooled to room
Temperature.Then the film of PVDF is cleared up: is wiped using two sides of the cotton ball soaked in alcohol to film, removing may influence to test
Dust and impurities.The preparation process of Raman spectrum base provided in this embodiment is as shown in Figure 1, pass through liquid-transfering gun
The silver nanowires solution prepared is sucked, one layer of silver nanowires is uniformly coated in the upper and lower surface of flexible PVDF, is put into later
It is dried 10 minutes for 30 DEG C in electric drying oven with forced convection (GZX-9076MBE), so that silver nanowires is become immobilising film morphology, obtain
To a kind of Raman spectrum base of flexible piezoelectric modulating properties, the scanning electron microscope (SEM) photograph of the Raman enhancing substrate is as schemed
Shown in 2, as shown in Figure 2, the diameter of Ag nanometers of line fibers is about 65.46nm.In addition, converting infrared spectrum analysis using fourier
Instrument respectively analyzes pure PVDF with the PVDF for being added to Ag nano wire, as a result as shown in figure 3, from the figure 3, it may be seen that being added to
After Ag nano wire, the content of β phase PVDF is increased.
Embodiment 2
The Raman enhancing substrate obtained using common substrate and embodiment 1 is to 10-6The rhodamine 6G (R6G) of mol/L into
Row Raman detection, test parameter are 532nm laser, 0.48mW power, 600gr/nm grating, the 8s time of integration.As a result such as Fig. 4 institute
Show, as shown in Figure 4, the Raman enhancing substrate prepared in embodiment 1 can be regulated and controled by piezoelectricity, and other common substrates
This effect can not be generated.
Embodiment 3
The Raman enhancing substrate obtained using embodiment 1 is under the pressure of different quality counterweight to 10-6The rhodamine of mol/L
6G (R6G) carries out Raman detection, and test parameter is 532nm laser, 0.48mW power, 600gr/nm grating, the 8s time of integration.Knot
Fruit is as shown in figure 5, as shown in Figure 5, pressure suffered by Raman enhancing substrate prepared by embodiment 1 is bigger, and Raman reinforcing effect is got over
It is good.
Embodiment 4
The Raman enhancing substrate obtained using embodiment 1 is in the case where identical mass weight is placed on different location to 10-6mol/L
Rhodamine 6G (R6G) carry out Raman detection, test parameter be 532nm laser, 0.48mW power, 600gr/nm grating, 8s product
Between timesharing.As a result as shown in fig. 6, it will be appreciated from fig. 6 that pressure suffered by Raman enhancing substrate prepared by embodiment 1 is got over from tested point
Closely, Raman reinforcing effect is better.
Embodiment 5
The Raman enhancing substrate obtained using embodiment 1 draws the glucose of 50mg/ml under the pressure of 50g counterweight
Graceful detection, and compareed simultaneously with common Raman enhancing substrate.Test parameter be 532nm laser, 0.48mW power,
600gr/nm grating, the 8s time of integration.As a result as shown in fig. 7, as shown in Figure 7, Raman enhancing substrate prepared by example 1 can be used
In the detection of glucose, and compared to common substrate, reinforcing effect is obvious.
The foregoing is merely preferred embodiment of the present disclosure, are not limited to the disclosure, for the skill of this field
For art personnel, the disclosure can have various modifications and variations.It is all within the spirit and principle of the disclosure, it is made any to repair
Change, equivalent replacement, improvement etc., should be included within the protection scope of the disclosure.
Claims (10)
1. a kind of Raman spectrum base, which is characterized in that the substrate is using piezoelectric material surface coated with nano gold
Metal particles.
2. Raman spectrum base as described in claim 1, which is characterized in that the piezoelectric material includes polyvinylidene fluoride
Alkene, piezoelectric ceramics；It preferably, is Kynoar.
3. Raman spectrum base as described in claim 1, which is characterized in that the nano-metal particle is received for silver
Rice, gold nano or copper nano particles；It preferably, is silver nano-grain.
4. a kind of preparation method of Raman spectrum base, which is characterized in that the described method comprises the following steps: will be golden
Belong to nano-solution dropwise addition to form it into form uniform film in piezoelectric material surface.
5. the preparation method of Raman spectrum base as claimed in claim 4, which is characterized in that the metal nano is molten
Liquid is gold nano, silver nanoparticle or copper nano-solution；Preferably, institute's silver nano solution is silver nanowires solution.
6. the preparation method of Raman spectrum base as claimed in claim 5, which is characterized in that the silver nanowires
Partial size is 60~70nm or length is 11~13 μm.
7. the preparation method of Raman spectrum base as claimed in claim 4, which is characterized in that the metal nano is molten
Liquid is the alcoholic solution of metal nano, uniform through ultrasonic vibration.
8. the preparation method of Raman spectrum base as claimed in claim 4, which is characterized in that the piezoelectric material is
PVDF material.
9. the preparation method of Raman spectrum base as claimed in claim 4, which is characterized in that the metal nano is molten
After drop is added on piezoelectric material surface, drying obtains uniform film.
10. application of any one of the claim 1-3 Raman spectrum base in Raman spectrum detection.
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| CN111912524A (en) * | 2019-12-25 | 2020-11-10 | 南开大学 | Raman spectrum imaging method and imaging device |
| CN112260586A (en) * | 2020-10-20 | 2021-01-22 | 德州学院 | Light-driven thermoelectric nano-generator, preparation thereof and application thereof in SERS (surface enhanced Raman scattering) in-situ detection catalysis |
| CN114199853A (en) * | 2021-11-23 | 2022-03-18 | 香港城市大学深圳福田研究院 | Biological sample detection method based on surface enhanced Raman spectroscopy |
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Application publication date: 20191105 |