CN110426385A - A kind of flexible surface enhancing Raman substrate and preparation method and application - Google Patents
A kind of flexible surface enhancing Raman substrate and preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of flexible surface enhancing Raman substrate and preparation method and application, the composite material being made of polymethyl methacrylate and silver nano-grain, the substrate of polymethyl methacrylate formation inverted pyramid type structure, silver nano-grain is evenly distributed on the inside of substrate, as flexible surface enhances Raman substrate, and substrate appearance is transparent.With good reinforcing effect and detection sensitivity, stretchable or bending, and do not influence detection effect.
Description
Technical field
The invention belongs to LR laser ramans and molecular recognition technical field, and in particular to a kind of flexible surface enhancing Raman substrate
And preparation method and application.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, 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.
The raman scattering cross section that Surface enhanced Raman scattering (SERS) can well solve general molecule is small, Raman test
The weak problem of signal, to achieve the purpose that highly sensitive, fast detection of trace substance, be widely used in material surface research,
The fields such as biological surface science, environmental monitoring, food safety.At present Surface enhanced Raman scattering signal mostly be using gold, silver,
The nano material of the noble metals such as copper is formed by " hot spot (hot spot) " effect in substrate surface and generates enhancing to Raman signal
Effect obtains.It is found in long-term research, in comparison silver nano-grain has better reinforcing effect, but exist easy
Being oxidized causes Basal Activity short-lived, generates chemical catalysis, bio-compatible, nanostructure repeatability with detection molecules
Low, high cost problem.Inventors have found that major part SERS substrate is all hard and opaque at present, generally require by dividing
It from method of purification from object to be detected surface extractions test substance, then is added drop-wise in SERS substrate and is detected, whole process is multiple
Miscellaneous time-consuming, randomness are higher and vulnerable to the influence for analyzing environment.These problems, which all become, hinders SERS technical application and development
Major obstacle.
Summary of the invention
For above-mentioned problems of the prior art, the present invention provides a kind of flexible surface enhancing Raman substrate and preparation
Methods and applications.Surface enhanced Raman substrate provided by the invention have Raman reinforcing effect is obvious, repeatability is high, be not easy by
Pollution, can long-term preservation, the advantages that analysis efficiency is high, analysis object range is wide, at low cost.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
In a first aspect, a kind of flexible surface enhances Raman substrate, by polymethyl methacrylate (PMMA) and silver nanoparticle
The composite material of grain composition, polymethyl methacrylate form the substrate of inverted pyramid type structure, and silver nano-grain is uniformly distributed
In the inside of substrate, as flexible surface enhances Raman substrate.
Preferably, the diameter of silver nano-grain is 50-100nm, and the spacing between silver nano-grain is 18-22nm.
PMMA forms flexible substrates, and silver nano-grain is evenly distributed in substrate, under the protection of PMMA, silver nanoparticle
Particle is not easy to be oxidized, reinforcing effect and sensitivity with preferable Raman detection, the composite wood of PMMA and silver nano-grain
Material forms base material and is flexible.
Second aspect, a kind of preparation method of flexible surface enhancing Raman substrate, specific steps are as follows:
Silver nano-grain suspension is added in PMMA solution, mixed solution is spun on pyramid silicon substrate,
Heat treatment removes pyramid silicon substrate, obtains flexible surface enhancing Raman substrate.
In some embodiments, silver nano-grain suspension is the aqueous solution of silver nano-grain, the preparation method comprises the following steps: using poly-
Vinylpyrrolidone (polyvinyl pyrrolidone, abbreviation PVP) and silver nitrate (AgNO3) carry out reduction reaction obtain.It is excellent
Choosing, the concentration of silver nano-grain suspension is 0.5-1.0g/mL；Further preferably 0.68-0.94g/mL, it is further excellent
It is selected as 0.71-0.86g/mL.Preferably, the diameter of silver nano-grain is 50-100nm.
Inventors have found that the concentration of silver nano-grain suspension influences the spacing of the silver nano-grain in the substrate to be formed,
The reinforcing effect and sensitivity of the effect of distance Raman detection of silver nano-grain in substrate.
In some embodiments, pyramid silicon substrate the preparation method comprises the following steps: using doped single crystal is handled in NaOH solution
Silicon method pre-processes to obtain pyramid silicon base.
In some embodiments, the temperature of heat treatment process is 127-133 DEG C, and the time of heat treatment is 25-35min.
The process of heat treatment is molding process, forms the compound of PMMA and silver nano-grain stable, fixed shape
The flexible surface of shape enhances Raman substrate material, while being conducive to silver nano-grain and being uniformly distributed in the substrate, in the mistake of heating
Cheng Zhong, it is too high or too low for temperature, it will affect the suppleness of PMMA.
In some embodiments, the method for pyramid silicon substrate is removed are as follows: with 30% NaOH solution immersion method
Remove pyramid silicon substrate.
The third aspect, application of the above-mentioned flexible surface enhancing Raman substrate in Raman detection.
Preferably, test object is R6G probe molecule or CV probe molecule.
The method for carrying out Raman detection using above-mentioned flexible surface enhancing Raman substrate are as follows: flexible surface is enhanced into Raman base
Bottom is put into the aqueous solution of determinand, is then taken out, and after moisture evaporation, is tested using Raman spectrometer.
Preferably, the concentration of determinand aqueous solution is 10-6-10-14mol/L.Preferably, flexible surface enhances Raman substrate
The time infiltrated in the aqueous solution of determinand is 1.5-2.5h.
Beneficial effects of the present invention:
(1) base material of the invention can meet or exceed silver nanostructured SERS base material in the prior art
Reinforcing effect and detection sensitivity；
(2) base material of the present invention enhances for Raman, simple, efficient, nontoxic, reusable with preparation method,
Stability is good, will not generate the advantages of being chemically bonded with probe molecule；
(3) base material provided by the invention, transparent, flexible stretching can pass through the concentration of silver nano-grain suspension
Regulate and control the sensitivity of the substrate, method is simple, and controllability is strong；
(4) the present invention provides easy, quick, extensive, the repeatable preparation methods of the base material.
Detailed description of the invention
The Figure of description for constituting a part of the invention is used to provide further understanding of the present application, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
The inverted pyramid structure flexible surface that Fig. 1 is the PMMA that embodiment 1 is mixed with silver nano-grain enhances Raman active base
The structural schematic diagram at bottom；
The inverted pyramid structure flexible surface that Fig. 2 is the PMMA that embodiment 1 is mixed with silver nano-grain enhances Raman active base
The stretching (a) at bottom, bending figure (b).
The inverted pyramid structure flexible surface that Fig. 3 is the PMMA that embodiment 1 is mixed with silver nano-grain enhances Raman active base
The scanning electron microscope (SEM) photograph at bottom, 3a, 3b are respectively the scanning electron microscope (SEM) photograph that scale is 2 μm and 200nm；
Fig. 4 is that the present invention is based on the Raman lights of the R6G probe molecule of the various concentration of the base material prepared in embodiment 1
Spectrogram；
Fig. 5 is that the present invention is based on the 10 of the various concentration of the base material prepared in embodiment 1 and comparative example-7Mol/L's
The Raman spectrogram of R6G probe molecule；
Fig. 6 is that the present invention is based on the Raman lights of the CV probe molecule of the various concentration of the base material prepared in embodiment 2
Spectrogram；
Fig. 7 is that the present invention is based on the 10 of the base material prepared in embodiment 3-7The drawing of the R6G probe molecule of mol/L concentration
Graceful spectrogram；
Fig. 8 is that the present invention is based on the 10 of the base material prepared in embodiment 4-7The drawing of the R6G probe molecule of mol/L concentration
Graceful spectrogram.
Fig. 9 is the inverted pyramid structure flexible surface enhancing Raman active for being mixed with the PMMA of silver nano-grain of various concentration
Substrate is in drop upper 10-7The Raman spectrogram of the R6G probe molecule of mol/L；
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
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 application.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.Below with reference to embodiment to this hair
Bright further explanation
Embodiment 1
Step 1, by 0.25g PVP and 0.05g AgNO3It is implanted sequentially in 20mL ethylene glycol solution, laser heating 30min,
Being vigorously stirred to oil bath temperature is 135 DEG C.It continuously stirs 1 hour, until the color of previous mixed solution becomes yellow transparent glue
Body.
Step 2, reaction mixture is cooled to room temperature.Then other 30mL acetone soln is added rapidly in step 1
In the colloid of preparation, high density and uniform silver nano-grain aqueous suspension are obtained.
Step 3, silver nano-grain aqueous suspension will be obtained in step 2 to receive by centrifugation (12000rpm, 5min) washing silver
Rice grain is simultaneously suspended from deionized water again, and the step is repeated 3 times.
Step 4, moisture removal is removed into the drying of silver nano-grain suspension obtained in step 3, adds PMMA solution, configure
For the mixed solution of 0.75g/ml, concentration is stirred at room temperature and is and stands overnight.
Step 5, it by mixture solution dip-coating obtained in step 4 on pyramid silicon substrate, and is heated at 130 DEG C
30 minutes.
Step 6, electric hybrid board obtained in step 5 is immersed in the NaOH aqueous solution that concentration is 30% to remove pyramid
Shape silicon chip carrier, drying nitrogen dry up to obtain inverted pyramid structure flexible surface enhancing Raman active substrate.It can be with by Fig. 3 a
It obtains, flexible surface enhances Raman substrate into inverted pyramid type structure.As shown in Fig. 3 b, silver nano-grain is evenly distributed on substrate
In.It is uniformly distributed in the substrate by the available silver nano-grain of Fig. 3.
Step 7, the flexible surface enhancing Raman active substrate of inverted pyramid structure obtained in step 6 is placed on 50mL's
Concentration is respectively 10-6-10-14In the R6G aqueous solution of mol/L, two hours are stood, are taken out later, after moisture volatilizees naturally,
Raman spectrum (as shown in Figure 4) is tested using the Raman spectrometer that excitation wavelength is 532nm.
Step 8, test result is analyzed, is placed on 50mL's in the flexible surface enhancing Raman active substrate of inverted pyramid structure
Concentration respectively on obtain R6G Molecular Raman spectrum 612cm-1, 774cm-1, 1182cm-1, 1308cm-1, 1360cm-1, 1508cm-1,
1572cm-1, 1650cm-1With apparent characteristic peak, illustrate that this example prepares the flexible surface enhancing Raman of inverted pyramid structure
Active substrate is obvious to R6G Molecular Raman signal enhancing effect.
Comparative example
Step 1, by 0.25g PVP and 0.05g AgNO3It is implanted sequentially in 20mL ethylene glycol solution, laser heating 30min,
Being vigorously stirred to oil bath temperature is 135 DEG C.It continuously stirs 1 hour, until the color of previous mixed solution becomes yellow transparent glue
Body.
Step 2, reaction mixture is cooled to room temperature.Then other 30mL acetone soln is added rapidly in step 1
In the colloid of preparation, high density and uniform silver nano-grain aqueous suspension are obtained.
Step 3, silver nano-grain aqueous suspension will be obtained in step 2 to receive by centrifugation (12000rpm, 5min) washing silver
Rice grain is simultaneously suspended from deionized water again, and the step is repeated 3 times.
Step 4, moisture removal is removed into the drying of silver nano-grain suspension obtained in step 3, adds in PMMA solution, matches
It is set to the mixed solution of 0.75g/ml, concentration is stirred at room temperature and is and stands overnight.
Step 5, by mixture solution dip-coating obtained in step 4 on plane silicon substrate, and 30 points are heated at 130 DEG C
Clock.
Step 6, electric hybrid board obtained in step 5 is immersed in the NaOH aqueous solution that concentration is 30% to remove planar silicon
Substrate carrier, drying nitrogen dry up to obtain planar flexible surface reinforced Raman active substrate.
Step 7, it is respectively by the concentration that planar flexible surface reinforced Raman active substrate obtained in step 6 is placed on 50mL
10-7In the R6G aqueous solution of mol/L, two hours are stood, are taken out later, after moisture volatilizees naturally, is using excitation wavelength
The Raman spectrometer test Raman spectrum of 532nm is simultaneously and Raman map obtained in embodiment 1 compares (as shown in Figure 5).
Available by Fig. 5, the flexible surface enhancing Raman active substrate reinforcing effect that plane silicon substrate obtains is poor.
Embodiment 2
Step 1, by 0.25g PVP and 0.05g AgNO3It is implanted sequentially in 20mL ethylene glycol solution, laser heating 30min,
Being vigorously stirred to oil bath temperature is 135 DEG C.It continuously stirs 1 hour, until the color of previous mixed solution becomes yellow transparent glue
Body.
Step 2, reaction mixture is cooled to room temperature.Then other 30mL acetone soln is added rapidly in step 1
In the colloid of preparation, high density and uniform silver nano-grain aqueous suspension are obtained.
Step 3, silver nano-grain aqueous suspension will be obtained in step 2 to receive by centrifugation (12000rpm, 5min) washing silver
Rice grain is simultaneously suspended from deionized water again, and the step is repeated 3 times.
Step 4, moisture removal is removed into the drying of silver nano-grain suspension obtained in step 3, adds in PMMA solution, matches
It is set to the mixed solution of 0.65g/ml, concentration is stirred at room temperature and is and stands overnight.
Step 5, it by mixture solution dip-coating obtained in step 4 on pyramid silicon substrate, and is heated at 130 DEG C
30 minutes.
Step 6, electric hybrid board obtained in step 5 is immersed in the NaOH aqueous solution that concentration is 30% to remove pyramid
Shape silicon chip carrier, drying nitrogen dry up to obtain inverted pyramid structure flexible surface enhancing Raman active substrate.
Step 7, the flexible surface enhancing Raman active substrate of inverted pyramid structure obtained in step 6 is placed on 50mL's
Concentration is respectively 10-5-10-12In the CV aqueous solution of mol/L, two hours are stood, are taken out later, after moisture volatilizees naturally, are made
Raman spectrum (as shown in Figure 6) is tested with the Raman spectrometer that excitation wavelength is 532nm.
Step 8, test result is analyzed, is placed on 50mL's in the flexible surface enhancing Raman active substrate of inverted pyramid structure
Concentration respectively on obtain CV Molecular Raman spectrum in 808cm-1, 1176cm-1, 1389cm-1, 1541cm-1, 1583cm-1, 1617cm-1With apparent characteristic peak, illustrate that this example prepares the flexible surface enhancing Raman active substrate of inverted pyramid structure to CV points
Sub- Raman signal reinforcing effect is obvious.
Embodiment 3
Step 1, by 0.25g PVP and 0.05g AgNO3It is implanted sequentially in 20mL ethylene glycol solution, laser heating 30min,
Being vigorously stirred to oil bath temperature is 135 DEG C.It continuously stirs 1 hour, until the color of previous mixed solution becomes yellow transparent glue
Body.
Step 2, reaction mixture is cooled to room temperature.Then other 30mL acetone soln is added rapidly in step 1
In the colloid of preparation, high density and uniform silver nano-grain aqueous suspension are obtained.
Step 3, silver nano-grain aqueous suspension will be obtained in step 2 to receive by centrifugation (12000rpm, 5min) washing silver
Rice grain is simultaneously suspended from deionized water again, and the step is repeated 3 times.
Step 4, moisture removal is removed into the drying of silver nano-grain suspension obtained in step 3, adds in PMMA solution, matches
It is set to the mixed solution of 0.75g/ml, concentration is stirred at room temperature and is and stands overnight.
Step 5, it by mixture solution dip-coating obtained in step 4 on pyramid silicon substrate, and is heated at 132 DEG C
28 minutes.
Step 6, electric hybrid board obtained in step 5 is immersed in the NaOH aqueous solution that concentration is 30% to remove pyramid
Shape silicon chip carrier, drying nitrogen dry up to obtain inverted pyramid structure flexible surface enhancing Raman active substrate.
Step 7, the flexible surface enhancing Raman active substrate of inverted pyramid structure obtained in step 6 is placed on 50mL's
Concentration is respectively 10-7In the R6G aqueous solution of mol/L, two hours are stood, are taken out later, after moisture volatilizees naturally, laterally drawn
Stretching is 110%, 120%, the 130% of original length, and the Raman spectrometer that excitation wavelength is 532nm is used to test Raman spectrum (such as Fig. 7
It is shown).It is available by Fig. 7, it is stretched in 130% long range of original, Raman detection reinforcing effect and sensitivity do not have substantially
Change.
Step 8, test result is analyzed, the flexible surface of the inverted pyramid structure stretched in step 7 enhances Raman active
10 are obtained in substrate-7The R6G Molecular Raman spectrum of mol/L is in 612cm-1, 774cm-1, 1182cm-1, 1308cm-1, 1360cm-1,
1508cm-1, 1572cm-1, 1650cm-1Still there is apparent characteristic peak, and compared with former long base material peak intensity almost without change
Change, illustrates that this example prepares the flexible surface enhancing Raman active substrate of inverted pyramid structure to R6G Molecular Raman signal enhancing
Effect is obvious.
Embodiment 4
Step 1, by 0.25g PVP and 0.05g AgNO3It is implanted sequentially in 20mL ethylene glycol solution, laser heating 30min,
Being vigorously stirred to oil bath temperature is 135 DEG C.It continuously stirs 1 hour, until the color of previous mixed solution becomes yellow transparent glue
Body.
Step 2, reaction mixture is cooled to room temperature.Then other 30mL acetone soln is added rapidly in step 1
In the colloid of preparation, high density and uniform silver nano-grain aqueous suspension are obtained.
Step 3, silver nano-grain aqueous suspension will be obtained in step 2 to receive by centrifugation (12000rpm, 5min) washing silver
Rice grain is simultaneously suspended from deionized water again, and the step is repeated 3 times.
Step 4, moisture removal is removed into the drying of silver nano-grain suspension obtained in step 3, adds in PMMA solution, matches
It is set to the mixed solution of 0.75g/ml, concentration is stirred at room temperature and is and stands overnight.
Step 5, it by mixture solution dip-coating obtained in step 4 on pyramid silicon substrate, and is heated at 127 DEG C
33 minutes.
Step 6, electric hybrid board obtained in step 5 is immersed in the NaOH aqueous solution that concentration is 30% to remove pyramid
Shape silicon chip carrier, drying nitrogen dry up to obtain inverted pyramid structure flexible surface enhancing Raman active substrate.
Step 7, the flexible surface enhancing Raman active substrate of inverted pyramid structure obtained in step 6 is placed on 50mL's
Concentration is respectively 10-7In the R6G aqueous solution of mol/L, stand two hours, take out later, after moisture volatilizees naturally, laterally into
180 ° of row distortions, then restore.10 times, 20 times, 30 above-mentioned circulations are carried out respectively.It the use of excitation wavelength is later 532nm's
Raman spectrometer carries out test Raman spectrum (as shown in Figure 8) to a sample.Available by Fig. 8, substrate is bent 30 underranges
Interior, Raman detection reinforcing effect and sensitivity do not change substantially.Available by Fig. 2, substrate is transparence, and substrate can be curved
It is bent.
Step 8, test result is analyzed, the flexible surface of the inverted pyramid structure stretched in step 7 enhances Raman active
10 are obtained in substrate-7The R6G Molecular Raman spectrum of mol/L is in 612cm-1, 774cm-1, 1182cm-1, 1308cm-1, 1360cm-1,
1508cm-1, 1572cm-1, 1650cm-1Still have apparent characteristic peak, and compared with not distorting base material peak intensity almost without change
Change, illustrates that this example prepares the flexible surface enhancing Raman active substrate of inverted pyramid structure to R6G Molecular Raman signal enhancing
Effect is obvious.
Embodiment 5
Unlike the first embodiment, the concentration of the silver nano-grain in silver nano particles suspension be respectively 0.52g/mL,
The preparation method of 0.68g/mL, 0.71g/mL, 0.86g/mL, 0.96g/mL, remaining Raman substrate are same as Example 1, point
It Jian Ce 10-7The R6G probe molecule of mol/L, detection method is identical, obtains shown in Fig. 9, available, silver nano-grain it is dense
Degree is influenced to detection intensity and sensitivity.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of flexible surface enhances Raman substrate, it is characterised in that: be made of polymethyl methacrylate and silver nano-grain
Composite material, polymethyl methacrylate forms the substrate of inverted pyramid type structure, and silver nano-grain is evenly distributed on substrate
Inside, as flexible surface enhance Raman substrate, substrate appearance is transparent.
2. flexible surface according to claim 1 enhances Raman substrate, it is characterised in that: the diameter of silver nano-grain is
50-100nm, the spacing between silver nano-grain are 18-22nm.
3. a kind of preparation method of flexible surface enhancing Raman substrate, it is characterised in that: silver nano-grain suspension to be added to
In PMMA solution, mixed solution is spun on pyramid silicon substrate, is heat-treated, pyramid silicon substrate is removed, obtains
Bright flexible surface enhances Raman substrate.
4. the preparation method of flexible surface enhancing Raman substrate according to claim 3, it is characterised in that: silver nano-grain
Suspension is the aqueous solution of silver nano-grain, the preparation method comprises the following steps: carrying out reduction reaction using polyvinylpyrrolidone and silver nitrate
It obtains；
Preferably, the diameter of silver nano-grain is 50-100nm.
5. the preparation method of flexible surface enhancing Raman substrate according to claim 3, it is characterised in that: silver nano-grain
The concentration of suspension is 0.5-1.0g/mL；
Preferably, 0.68-0.94g/mL；It is further preferred that 0.71-0.86g/mL.
6. the preparation method of flexible surface enhancing Raman substrate according to claim 3, it is characterised in that: pyramid silicon
Substrate the preparation method comprises the following steps: using in NaOH solution handle doped monocrystalline silicon method pre-process to obtain pyramid silicon base.
7. the preparation method of flexible surface enhancing Raman substrate according to claim 3, it is characterised in that: heat treatment process
Temperature be 125-135 DEG C, time of heat treatment is 25-35min.
8. the preparation method of flexible surface enhancing Raman substrate according to claim 3, it is characterised in that: removal pyramid
The method of shape silicon substrate are as follows: remove pyramid silicon substrate with 30% NaOH solution immersion method.
9. application of any flexible surface enhancing Raman substrate of claim 1 to 2 in Raman detection；
Preferably, test object is R6G probe molecule or CV probe molecule.
10. the method for carrying out Raman detection using any flexible surface enhancing Raman substrate of claim 1 to 2, special
Sign is: transparent flexible surface enhanced Raman substrate is put into the aqueous solution of determinand, is then taken out, after moisture evaporation, and benefit
It is tested with Raman spectrometer；
Preferably, the concentration of determinand aqueous solution is 10-6-10-14mol/L；
Preferably, the time that transparent flexible surface enhanced Raman substrate infiltrates in the aqueous solution of determinand is 1.5-2.5h.
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| CN111426676A (en) * | 2020-04-21 | 2020-07-17 | 东华大学 | Surface enhanced Raman scattering substrate based on metal nanometer bowl and preparation method thereof |
| CN111426676B (en) * | 2020-04-21 | 2022-03-25 | 东华大学 | Surface enhanced Raman scattering substrate based on metal nanometer bowl and preparation method thereof |
| CN112014371A (en) * | 2020-07-22 | 2020-12-01 | 山东师范大学 | Preparation method and application of flexible semitransparent surface enhanced Raman substrate |
| CN112014371B (en) * | 2020-07-22 | 2024-05-24 | 山东师范大学 | Preparation method and application of flexible semitransparent surface enhanced Raman substrate |
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