CN109916879A - Material composition Raman spectra detection process based on the reunion enhancing of automatically controlled nano wire - Google Patents
Material composition Raman spectra detection process based on the reunion enhancing of automatically controlled nano wire Download PDFInfo
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Abstract
The present invention provides a kind of material composition Raman spectra detection process based on the reunion enhancing of automatically controlled nano wire, include the following steps: that (1) cleans microchannel；(2) synthesis of silver nano-wire, and silver nanowires is diluted 10 times with alcoholic solution；(3) sample to be tested is first configured to solution, is by volume then that 1:1 is mixed with solution to be measured by silver nanowires, form mixture, be then passed through mixture in microflow channels in the case where flow velocity is 1 μ L/min；(4) mixture of silver nanowires and sample to be tested is chosen as electric regulation and control object, captures the electric regulation and control object in microchannel using regulatable sine ac power supply；(5) micro-fluidic system in step (4) is placed on the objective table of confocal detection platform, adjustment microcobjective acquires the Raman spectrum of sample at a distance from electric regulation and control object.The detection method high sensitivity, SERS substrate are reusable, and can quantitative analysis difference micro substance SERS intensity, reproducibility and uniformity with higher.
Description
Technical field
The invention belongs to nano materials and optical technical field, and in particular to it is a kind of based on automatically controlled nano wire reunite enhancing
Material composition Raman spectra detection process.
Background technique
Highly sensitive effective detection of micro substance and real-time monitoring are in people's lives and social production in complicated liquid-phase system
In have huge demand, such as in rivers and lakes pesticide organic pollutant detection and monitoring, lead in water supply pipe system
The detection and monitoring of the heavy metal ion such as mercury, the detection and monitoring of the additives such as melamine in milk, Electric Power Equipment Insulation oil
The detection and monitoring of the aging characters object such as middle furfural, the detection and monitoring etc. of fault signature object, have huge in industrial lubricant
Economic value and wide application prospect.
Currently, the application of Surface enhanced Raman spectroscopy (SERS) has spread over every field, including to complicated liquid phase body
The detection of micro substance in system.In such applications, the SERS in conjunction with microfluidic device is tested in traditional macroscopical ring
Some apparent advantages are shown in border.In recent years, in microfluidic surface enhancing raman study, by metal Nano structure
Most of enhancing substrates of composition are all directly prepared in the channel.For example, Kang et al. reports a kind of photoinduction synthesis
Method is used to prepare the silver nano-grain for being embedded in the zinc oxide nanowire surface for being integrated into microfluidic system；Bai et al. preparation
A kind of three-dimensional microfluidic SERS system based on the etching of femtosecond laser Aided Wet；Leem et al. heats substrate with polyol process
When, Ag films are directly formd in microfluidic channel.In addition, other methods, such as photo-reduction and photo-thermal effect also by
For the manufacture enhancing substrate in micro-fluidic system.
However, in these micro-fluidic systems, because the micro substance of low concentration flows in several hundred microns of channel,
The micro substance is difficult to reach metal surface enhancing hot spot (≤100nm), brings certain difficulty to SERS detection.Therefore, many
Researcher makes micro substance molecule and metal form simple Bioconjugation using the method for bonding, to reach metal structure table
The hot spot in face realizes the detection to material molecule to be measured.But since SERS substrate is difficult to rinse well, (- HS group is deposited
), no matter for identical micro substance molecule or other micro substance molecules, all can to subsequent SERS signal analyze bring compared with
Big interference.In other words, these SERS substrates are being irreversible after chemical reaction or Physical Absorption occurs with analyte
, limit their recuperability and reusability.
To sum up, the recycling rate of waterused of SERS substrate how is improved, and then highly sensitive effective detection is different with real-time monitoring micro-
The Raman spectrum of quantity of material molecule, be improve miniflow SERS utilization rate of equipment and installations and reduce equipment cost expense critical issue it
One.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, the purpose of the present invention is to provide one kind to be based on automatically controlled nanowire cluster
The material composition Raman spectra detection process of poly- enhancing, the detection method high sensitivity, SERS substrate are reusable, and can determine
Amount analyzes the SERS intensity of different micro substances, reproducibility and uniformity with higher.
To achieve the above object, the invention provides the following technical scheme: a kind of object based on the reunion enhancing of automatically controlled nano wire
Matter ingredient Raman spectra detection process, includes the following steps:
(1) it uses and cleans microchannel at high speeds containing mass fraction for the alcoholic solution of 0.05-0.15% tween；
(2) polyol process chemical synthesis silver nanowires is utilized, and silver nanowires is diluted 10 times with alcoholic solution；
(3) sample to be tested is first configured to solution, is by volume then that 1:1 is mixed with solution to be measured by silver nanowires
It closes, and 25-50s is sufficiently stirred, form mixture, mixture is passed through in microflow channels in the case where flow velocity is 1 μ L/min then, is passed through
Time is 10min；
(4) mixture of silver nanowires and sample to be tested is chosen as electric regulation and control object, utilizes regulatable simple alternating current
Power supply captures the electric regulation and control object in microchannel, frequency 15-25MHz, voltage 8-10V, time 5-7min；
(5) micro-fluidic system that electric regulation and control object is captured in step (4) is placed in the objective table of confocal detection platform
On, laser spot is focused on electric regulation and control object at a distance from electric regulation and control object, acquires sample to be tested by adjustment microcobjective
Raman spectrum.
Further, the synthetic method of silver nanowires is as follows in step (2):
(a) AgNO for being 0.1mol/L by 3mL concentration3Ethylene glycol solution is added to the poly- second that 3mL concentration is 0.6mol/L
In alkene pyrrolidone ethylene glycol solution, 10min is reacted；
(b) the above-mentioned solution of 6ml is taken to be added dropwise in 5ml ethylene glycol solution, temperature is 160 DEG C, reacts 6min；It is added dropwise
Afterwards, 1h is heated at 160 DEG C；
(c) solution that step (b) obtains is cooled to room temperature, is centrifuged, washs, dries to get silver nanowires is arrived.
Further, frequency is 20MHz, voltage 10V, time 6min in step (4).
Further, the condition of sample Raman spectrum is acquired in step (5) are as follows: optical maser wavelength 633nm, laser power are
10mW, acquisition time 20s, Raman spectrum detection range are 400-1800cm-1。
It is compared with the prior art, the invention has the following beneficial effects:
It is provided by the invention based on automatically controlled nano wire reunite enhancing material composition Raman spectra detection process high sensitivity,
SERS substrate is reusable, and can quantitative analysis difference micro substance SERS intensity, reproducibility with higher and uniformly
Property.
Detailed description of the invention
Fig. 1 is the Raman spectrogram of rhodamine 6G (R6G)；
Fig. 2 is the Raman spectrogram of melamine；
Fig. 3 is the Raman spectrogram of R6G and MB exchange detection；
Fig. 4 is the linearity curve of R6G molecule.
Specific embodiment
A kind of material composition Raman spectra detection process based on the reunion enhancing of automatically controlled nano wire, includes the following steps:
(1) it uses and cleans microchannel at high speeds containing mass fraction for the alcoholic solution of 0.05-0.15% tween；
(2) polyol process chemical synthesis silver nanowires is utilized, and silver nanowires is diluted 10 times with alcoholic solution；
(3) sample to be tested is first configured to solution, is by volume then that 1:1 is mixed with solution to be measured by silver nanowires
It closes, and 25-50s is sufficiently stirred, form mixture, mixture is passed through in microflow channels in the case where flow velocity is 1 μ L/min then, is passed through
Time is 10min；
(4) mixture of silver nanowires and sample to be tested is chosen as electric regulation and control object, utilizes regulatable simple alternating current
Power supply captures the electric regulation and control object in microchannel, frequency 15-25MHz, voltage 8-10V, time 5-7min；
(5) micro-fluidic system that electric regulation and control object is captured in step (4) is placed in the objective table of confocal detection platform
On, laser spot is focused on electric regulation and control object at a distance from electric regulation and control object, acquires sample to be tested by adjustment microcobjective
Raman spectrum, the condition of acquisition are as follows: optical maser wavelength 633nm, laser power 10mW, acquisition time 20s.
Wherein, the synthetic method of silver nanowires is as follows:
(a) AgNO for being 0.1mol/L by 3mL concentration3Ethylene glycol solution is added to the poly- second that 3mL concentration is 0.6mol/L
In alkene pyrrolidone ethylene glycol solution, 10min is reacted；
(b) the above-mentioned solution of 6ml is taken to be added dropwise in 5ml ethylene glycol solution, temperature is 160 DEG C, reacts 6min；It is added dropwise
Afterwards, 1h is heated at 160 DEG C；
(c) solution that step (b) obtains is cooled to room temperature, primary, removing ethylene glycol solution is centrifuged using acetone, then use
Ethanol washing twice, removes remaining polyvinylpyrrolidonesolution solution, dries to get silver nanowires is arrived.
Combined with specific embodiments below, the method for the present invention is described in detail.The sinusoidal ac used in the present invention
The model Agilent 33250A (maximum voltage 10V) in source.Miniflow dielectrophoresis (DEP) principle: positioned at the particle of non-well-balanced electric field
Due to dielectric polarization effect effect and the translational motion that generates, alternating voltage be applied on the electrode being integrated on chip,
To generate required space electric field gradient, the silver nanowires near electrode is captured by DEP power to electrode movement, and attachment is on the electrode
Silver nanowires can produce very strong internal field's gradient, to attract other nano wires.
Embodiment 1
The Raman spectrum of R6G is detected, specific to detect as follows:
(1) it uses and cleans microchannel at high speeds containing mass fraction for the alcoholic solution of 0.1% tween；
(2) polyol process chemical synthesis silver nanowires is utilized, and silver nanowires is diluted 10 times with alcoholic solution；
(3) R6G is first configured to concentration is 10-10M、10-12M and 10-14The aqueous solution of M, then by silver nanowires and above-mentioned
R6G solution is that 1:1 is mixed, and 30s is sufficiently stirred using vortex method by volume, forms mixture, then application injection
Mixture is passed through in microflow channels by device pump in the case where low flow velocity is 1 μ L/min, and being passed through the time is 10min；
(4) mixture of silver nanowires and R6G are chosen as electric regulation and control object, is caught using regulatable sine ac power supply
Obtain the electric regulation and control object in microchannel, frequency 20MHz, voltage 10V, time 6min；
(5) micro-fluidic system that electric regulation and control object is captured in step (4) is placed in the objective table of confocal detection platform
On, laser spot is focused on electric regulation and control object at a distance from electric regulation and control object, acquires the Raman of R6G by adjustment microcobjective
Spectrum, the condition of acquisition are as follows: optical maser wavelength 633nm, laser power 10mW, sweep time 20s, Raman spectrum detect model
It encloses for 400-1800cm-1.Testing result using detection method of the invention as shown in Figure 1, it can be seen from the figure that can be obtained
The raman characteristic peak of the R6G of different solubility is realized to using R6G as the highly sensitive detection of the micro substance of representative.
Wherein, the synthetic method of silver nanowires is as follows:
(a) AgNO for being 0.1mol/L by 3mL concentration3Ethylene glycol solution is added to the poly- second that 3mL concentration is 0.6mol/L
In alkene pyrrolidone ethylene glycol solution, 10min is reacted；
(b) the above-mentioned solution of 6ml is taken to be added dropwise in 5ml ethylene glycol solution, temperature is 160 DEG C, reacts 6min；It is added dropwise
Afterwards, 1h is heated at 160 DEG C；
(c) solution that step (b) obtains is cooled to room temperature, primary, removing ethylene glycol solution is centrifuged using acetone, then use
Ethanol washing twice, removes remaining polyvinylpyrrolidonesolution solution, dries to get silver nanowires is arrived.
Embodiment 2
The Raman spectrum of melamine is detected, specific to detect as follows:
(1) it uses and cleans microchannel at high speeds containing mass fraction for the alcoholic solution of 0.15% tween；
(2) polyol process chemical synthesis silver nanowires is utilized, and silver nanowires is diluted 10 times with alcoholic solution；
(3) it takes certain deionized water to be heated to 90 DEG C, and melamine powder is added into deionized water, be configured to dense
Degree is the melamine aqueous solution of 0.1ppm, 10ppm and 500ppm；Similarly, above-mentioned melamine aqueous solution is taken, it is fixed using milk
Rongcheng concentration is the melamine milk soln of 1ppm and 10ppm, then by silver nanowires and above-mentioned melamine milk soln
It is mixed by volume for 1:1, and 25s is sufficiently stirred using vortex method, form mixture, then will be mixed using syringe pump
It closes object to be passed through in microflow channels in the case where flow velocity is 1 μ L/min, being passed through the time is 10min；
(4) mixture of silver nanowires and above-mentioned melamine milk soln is chosen as electric regulation and control object, and utilization is adjustable
The sine ac power supply of control captures the electric regulation and control object in microchannel, frequency 15MHz, voltage 8V, time 5min；
(5) micro-fluidic system that electric regulation and control object is captured in step (4) is placed in the objective table of confocal detection platform
On, laser spot is focused on electric regulation and control object at a distance from electric regulation and control object, acquires melamine by adjustment microcobjective
Raman spectrum, the condition of acquisition are as follows: optical maser wavelength 633nm, laser power 10mW, sweep time 20s.As a result such as Fig. 2
It is shown, since the miscellaneous peak of melamine milk soln is more, before measuring its Raman spectrum, first measure melamine aqueous amine
The Raman spectrum of solution to identify the peak position of melamine aqueous solution, and can obtain the trimerization under the enhancing of this substrate
The minimal detectable concentration of cyanamide aqueous solution is 0.1ppm, and well below national standard 1ppm, Fig. 4 left figure is the trimerization of various concentration
The Raman spectrogram of cyanamide aqueous solution, it can be seen from the figure that melamine aqueous solution peak position is in 678cm-1Place；Fig. 4 is right
Figure is the Raman spectrogram of the melamine milk soln of various concentration, it can be seen from the figure that in 678cm-1Place, various concentration
Melamine milk soln there is most strong characteristic peak, and when substrate is not added, in 678cm-1Place does not occur apparent feature
Peak, this explanation can obtain the raman characteristic peak of melamine using detection method of the invention.
Wherein, the synthetic method of silver nanowires is the same as embodiment 1.
Embodiment 3
Verify the repeatability of detection method
Raman characteristic peak is detected by the alternating to R6G and MB, there is repeatability to verify detection method of the invention.
As a result as shown in Figure 3: comparative analysis R6G and MB Raman spectrum characteristic peak is followed and is badly repeated several times, the raman characteristic peak of R6G and MB
It has not undergone great changes and is displaced, also without other spectra1 interfer-s, this explanation detection method provided by the invention has can
Repeatability.
Embodiment 4
Quantitative analysis can be carried out by verifying detection method of the invention
To further decrease influence of the testing conditions variation to testing result, overlap of peaks, peak intensity and inspection are comprehensively considered
After surveying the factors such as stability, R6G molecule is chosen in 1505cm-1Locate spectral peak as characteristic peak；Successively detect R6G under various concentration
Raman scattering intensity is drawn using origin software.It goes forward side by side line matched curve, as a result as shown in Figure 4；With the concentration of R6G molecule
For independent variable, characteristic peak 1505cm-1The raman scattering intensity at place is dependent variable, and R6G various concentration is successively established using least square method
Under Quantitative Analysis Model.R6G molecular method quantification linearity curve are as follows: y=2603.8x+34357.1, goodness of fit R2=0.96.
It can be seen that detection method provided by the invention can carry out quantitative analysis to sample to be tested, to improve detection side of the invention
The accuracy of method.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (4)
1. a kind of material composition Raman spectra detection process based on the reunion enhancing of automatically controlled nano wire, which is characterized in that including such as
Lower step:
(1) it uses and cleans microchannel at high speeds containing mass fraction for the alcoholic solution of 0.05-0.15% tween；
(2) polyol process chemical synthesis silver nanowires is utilized, and silver nanowires is diluted 10 times with alcoholic solution；
(3) sample to be tested is first configured to solution, is by volume then that 1:1 is mixed with solution to be measured by silver nanowires,
And 25-50s is sufficiently stirred, mixture is formed, is then passed through mixture in microflow channels in the case where flow velocity is 1 μ L/min, when being passed through
Between be 10min；
(4) mixture of silver nanowires and sample to be tested is chosen as electric regulation and control object, utilizes regulatable sine ac power supply
Capture the electric regulation and control object in microchannel, frequency 15-25MHz, voltage 8-10V, time 5-7min；
(5) micro-fluidic system for capturing electric regulation and control object in step (4) is placed on the objective table of confocal detection platform, is adjusted
Laser spot is focused on electric regulation and control object at a distance from electric regulation and control object, acquires the Raman of sample to be tested by whole microcobjective
Spectrum.
2. the material composition Raman spectra detection process according to claim 1 based on the reunion enhancing of automatically controlled nano wire,
It is characterized in that, the synthetic method of silver nanowires is as follows in step (2):
(a) AgNO for being 0.1mol/L by 3mL concentration3Ethylene glycol solution is added to the polyvinyl pyrrole that 3mL concentration is 0.6mol/L
In alkanone ethylene glycol solution, 10min is reacted；
(b) the above-mentioned solution of 6ml is taken to be added dropwise in 5ml ethylene glycol solution, temperature is 160 DEG C, reacts 6min；After being added dropwise,
1h is heated at 160 DEG C；
(c) solution that step (b) obtains is cooled to room temperature, is centrifuged, washs, dries to get silver nanowires is arrived.
3. the material composition Raman spectra detection process according to claim 1 based on the reunion enhancing of automatically controlled nano wire,
It is characterized in that, frequency is 20MHz, voltage 10V, time 6min in step (4).
4. the material composition Raman spectra detection process according to claim 1 based on the reunion enhancing of automatically controlled nano wire,
It is characterized in that, the condition of acquisition sample Raman spectrum in step (5) are as follows: optical maser wavelength 633nm, laser power 10mW are adopted
Integrate the time as 20s, Raman spectrum detection range is 400-1800cm-1。
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| CN113418905A (en) * | 2021-07-28 | 2021-09-21 | 中国药科大学 | Surface enhanced Raman spectroscopy detection method for detecting marine toxin GYM based on crossed mesh silver nanowire AgNW |
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Application publication date: 20190621 |