CN108226130A - For the soft light Meta Materials laminated film and method of nitrite detection - Google Patents
For the soft light Meta Materials laminated film and method of nitrite detection Download PDFInfo
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- CN108226130A CN108226130A CN201711455014.2A CN201711455014A CN108226130A CN 108226130 A CN108226130 A CN 108226130A CN 201711455014 A CN201711455014 A CN 201711455014A CN 108226130 A CN108226130 A CN 108226130A
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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
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Abstract
The invention discloses a kind of soft light Meta Materials laminated films and method for nitrite detection.Single-layer metal nano-grain array is formed on soft transmitting substrate as metamaterial layer, then is covered with p-Mercaptoaniline self-assembled monolayer as nitrite sensitive membrane；Under Vis/NIR Spectroscopy excitation, metamaterial layer generates surface plasma body resonant vibration, under the surface plasmons of metamaterial layer and the common synergistic effect of The sub-salt nitrate ion, p-Mercaptoaniline in induction nitrite sensitive membrane is converted into azo biphenol compound, because the Raman spectrum of two kinds of molecules of azo biphenol compound and p-Mercaptoaniline has significant difference, this reaction directly is monitored by using Raman spectrum, and then realizes specific recognition and the detection to nitrite ion indirectly.The present invention is generated azo biphenyl with reference to catalysed aniline of the The sub-salt nitric acid in surface selectivity, is realized the detection of quick nitrite using special optical characteristic possessed by Meta Materials.
Description
Technical field
It detects film the present invention relates to a kind of and makes application method more particularly to a kind of for nitrite detection
Soft light Meta Materials laminated film and method.
Background technology
Nitrite is a kind of harmful substance being widely present in animals and plants food.The nitric acid being rich in vegetables and meat
Salt can also be transformed into nitrite in marinated, storage or mis-machined under the action of reductase.Simultaneously as
Nitrite has color development and anti-corrosive fresh-keeping effect to meat products, therefore makes meat products color development, enhancing wind frequently as additive
Taste, the effect of Antimicrobial preservative also are able to Shelf-life.But nitrite can make human body hemoglobin oxidation and lose fortune
The ability of oxygen therapy causes chronic, acute poisoning, moreover it is possible to which generation is reacted with the secondary-amine compound in food, in human body to be had by force
The nitrosamine compound of carcinogenicity.In addition to carcinogenic, nitrous acid can also generate teratogenesis to fetus through placenta and toxicity is made.With people
The enhancing of Consciousness of food security and the increasing of China's food security supervision dynamics, nitrite become food safety detection
One of big event.
National standard has result precision and essence for the assay method (hydrochloric acid-naphthalene-ethylenediamine method) of content of nitrite
The advantages of density is high, but operating process is more complicated, needs special instrument, is unsuitable for field quick detection.At present, to nitrous acid
Although salt content Fast Detection Technique has some reports, but need to further improve in terms of accuracy and sensitivity.
Meta Materials (Metamaterial) refer to it is a kind of by artificial structure's unit (artificial atom and artificial molecule) set and
Into special material, by the structurally ordered design on the key physical scale of material, certain apparent advise naturally can be broken through
The limitation of rule, so as to obtain the meta-materials function beyond the intrinsic common property of nature, such as " negative refraction ", " superparamagnetic
Property " etc..In the past 10 years, the great innovation for the design of material thought that Meta Materials are embodied causes global highest attention.The U.S.,
Japan, European Union sequentially activate the projects of Meta Materials, have caused information technology, national defense industry, new energy technology, microfabrication
Some row major transformations in the fields such as technology.
Invention content
In order to solve the problems, such as background technology, examined the object of the present invention is to provide one kind for nitrite
The soft light Meta Materials laminated film and method of survey prepare the side of meta-material thin film using autonomous dress technology on flexible parent metal
Special optical characteristic combination The sub-salt nitric acid possessed by method and utilization Meta Materials can be in the catalysed aniline of its surface selectivity
Azo biphenyl is generated, realizes the detection of quick nitrite.
The present invention is used for the measure to sample nitrite, has high sensitivity, specificity height, detection speed
Soon, without sample preprocessing the features such as.
Technical scheme is as follows：
First, a kind of soft light Meta Materials laminated film for nitrite detection：
Including base material, using flexible and transparent material；
Including metamaterial layer, be formed on base material, be by single metal nano particle be basic structural unit oldered array
It forms；
It including nitrite sensitive membrane, is formed on Meta Materials, is single point be made of p-Mercaptoaniline molecular self-assembling
Sub- film, the detected nitrite of nitrite sensitive membrane contact.
The present invention is to be equipped with single-layer metal nano-grain array, then be covered with p-Mercaptoaniline self assembly on soft base material
Monomolecular film, entire material show good flexible and translucency.The metamaterial layer is self-assembly of using interface, institute
The nitrite sensitive membrane molecular self-assembling stated is formed.
Under Vis/NIR Spectroscopy excitation, metamaterial layer generates surface plasma body resonant vibration, the metal on metamaterial layer surface
Nano particle can ionize generation surface plasma resonance, in the surface plasmons of metamaterial layer and The sub-salt nitrate ion
Under common synergistic effect, the p-Mercaptoaniline in nitrite sensitive membrane is induced to be converted into azo biphenol compound to carry out nitrous
Hydrochlorate detects, and because the Raman spectrum of two kinds of molecules of azo biphenol compound and p-Mercaptoaniline has significant difference, directly passes through profit
This reaction is monitored with Raman spectrum, and then realizes specific recognition and the detection to nitrite ion indirectly.
The drawing of surface plasma body resonant vibration amplification absorption molecule in nitrite sensitive membrane that the metamaterial layer generates
Graceful signal is to improve the sensitivity of detection, i.e. Surface enhanced Raman spectroscopy scattering effect.
Nitrite detection of the flexible and transparent meta-material thin film suitable for fluid sample and solid sample.The present invention
It can be not only used for nitrous acid in liquid sample to detect, the present invention can also be attached at irregular actual sample surface, for solid
Surface nitrous nitrification.
2nd, the production method of a kind of soft light Meta Materials laminated film for nitrite detection：
The metamaterial layer that structure is made of single metal nano particle for basic structural unit on flexibility, transmitting substrate,
The nitrite sensitive membrane being made of p-Mercaptoaniline is built on metamaterial layer.It is specifically first prepared on base material and forms list
A metal nanoparticle is the metamaterial layer that basic structural unit oldered array is formed, then by mercapto on metamaterial layer surface
Base aniline prepares to form self-assembled monolayer in a manner that molecule independently fills, as nitrite sensitive membrane.
The structure on base material forms single metal nano particle and surpasses for what basic structural unit oldered array was formed
Material layer is specially：It is first orderly in air/water boundary or organic solvent/aqueous phase interface structure using interface self assembly mode
Metal nanoparticle array, then metal nanoparticle array is transferred to flexible parent metal surface.
It builds and is specially by metamaterial layer mode of the single metal nano particle for basic structural unit：Using interface from group
Base material overlying last layer mounted in hard material is with the single-layer metal nano particle of the close ordered arrangement of single metal nano particle
Array, then flexible material is overlying on single-layer metal nano-grain array, by single-layer metal nano particle battle array after final stripping
In column jump to the base material of flexible material.
A kind of mode of the interface self assembly is：Hydrophilic treated after hard substrate is cleaned, is placed on horizontal plane,
Then water is added to form the moisture film for covering entire substrate surface in upper surface, the metal nanoparticle being scattered in organic solvent is delayed
In slow injection moisture film, one layer of close-packed arrays metal nanoparticle array is formed in the air liquid interface of moisture film, after water film evaporation
The metal nanoparticle array closely arranged.
The another way of the interface self assembly is：By organic solvent and the metal nanoparticle being scattered in water phase
Mutual exclusive interface is mixed to form, ethyl alcohol is slowly injected into water phase, inducing metal nano particle is in organic solvent/water phase circle
One layer of close-packed arrays metal nanoparticle array is formed at face, is delayed after hard substrate after hydrophilic treated is slowly inserted into below interface
It is slow to propose, the metal nanoparticle array closely arranged.
Structure nitrite sensitive membrane mode be specially：One is formed in metamaterial layer using the technology of molecular self-assembling
The fine and close p-Mercaptoaniline monomolecular film of layer, forms the sensitive membrane for having response to nitrite ion.It particularly will be to sulfydryl
Aniline solution is added drop-wise to the self-assembled monolayer formed described in acquisition by p-Mercaptoaniline after standing on metamaterial layer surface.
A kind of methods that nitrite detection is used for using flexible and transparent meta-material thin film of three,：
Detected sample is placed in the nitrite sensitive membrane of flexible and transparent meta-material thin film, with visible/near infrared
Laser is irradiated, and the testing result of sample to be tested nitrite ion is obtained by Raman spectroscopy instrument acquisition signal.
The surface that the present invention is generated by the metal Nano structure in metamaterial layer under the action of visible/near infrared laser
Plasma resonance, and The sub-salt nitrate ion collective effect is combined, selectively aniline is converted into sensitive membrane is catalyzed
Azo biphenyl, due to the Raman spectrum of aniline and azo biphenyl, there were significant differences, by Raman light instrument realize to nitrite from
The specific recognition of son and detection；Meanwhile the surface plasma in metamaterial layer is to adsorbing the Raman light of the molecule on its surface
Amplification of the spectrum with enhancing intensity plays the role of improving detection sensitivity.
The detected sample is fluid sample or solid sample.
It is fluid sample for detected sample, nitrite detection mode is：Liquid to be detected sample is placed directly within
On meta-material thin film, after laser excitation, signal, the detection to nitrite ion are acquired with Raman spectrum.
It is solid sample for detected sample, nitrite detection mode is：Meta Materials are placed in solid sample to be measured
After laser excitation, signal, specific recognition and detection to nitrite ion are acquired with Raman spectrum for surface.
The material of the metal nanoparticle is gold, silver, the alloy of one or more kinds of mixing of platinum, copper.
The grain size of the metal nanoparticle is 10nm to 200nm.
The pattern of the metal nanoparticle is ball, ellipsoid, stick, cube, polygon and irregular shape.
The base material of the hard material uses glass, silicon chip or sheet metal.
The base material of the flexible material is the polymer of flexible and transparent, using polyacrylamide, dimethyl silicone polymer, is gathered
Acrylate, polyethylene tape or polyimides glue.
The beneficial effects of the invention are as follows：
The present invention is by under the action of the surface plasma that is formed in metal nano metamaterial structure, The sub-salt nitrate ion
The principle of azo biphenyl and the Raman light of catalysate (azo biphenyl) and substrate (aniline) can be generated with efficient catalytic aniline
The characteristic there are significant difference is composed, it can be achieved that specific recognition and detection to nitrite ion.
The metal nano Meta Materials that the present invention is built in flexible clear materials, except containing available for nitrous acid in fluid sample
The detection of amount, can also attach with solid sample surface, for actual sample surface nitrite detect.
The present invention has sensitivity, specificity high as a result, without sample preprocessing, it is easy to use the features such as, can be extensive
As various food, drug, environmental contaminants nitrite detection method.
Description of the drawings
Fig. 1 is the structure diagram of the present invention.
Fig. 2 is a kind of embodiment flow diagram of manufacturing method of the present invention.
Fig. 3 is another embodiment flow diagram of manufacturing method of the present invention.
Fig. 4 is the typical metal nano-array Meta Materials scanning electron microscope (SEM) photograph of the present invention.
Fig. 5 is the The sub-salt nitric acid testing principle schematic diagram of the present invention.
Fig. 6 is the Surface enhanced Raman spectroscopy comparison diagram of p-Mercaptoaniline and azo biphenyl.
Fig. 7 is a kind of implementation process diagram that the present invention is used to detect fluid sample nitrite.
Fig. 8 is response response Raman spectrogram of the present invention under different nitrite concentrations.
Fig. 9 is response Raman spectrogram of the present invention to interference anion typical in water.
Figure 10 is a kind of implementation process diagram that the present invention is used to detect nitrite on solid sample surface
Figure 11 is the obverse and reverse sides response Raman spectrogram of the present invention.
In figure：1st, flexible parent metal, 2, metamaterial layer, 3, nitrite ion sensitive membrane, 4, hard substrate, 5, moisture film, 6,
Syringe pump, 7, syringe, 8, metal nanoparticle array, 9, container, 10, metal nanoparticle colloidal sol, 11, toluene, 12, liquid
Sample, 13, laser, 14, Raman spectroscopy instrument, 15, optical fiber, 16, solid sample.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
It is of the invention mainly using interface self assembly on hard material surface, it is basic to prepare by single metal nano particle
The Meta Materials that structural unit is formed；Flexible material is overlying on above-mentioned Meta Materials again, flexible material can be transferred into after stripping
On the base material of material；Form one layer of p-Mercaptoaniline self-assembled film, shape on metal nano array in a manner of molecular self-assembling again
Pairs of nitrite ion has the sensitive membrane of response, is detected for nitrite.
As shown in Figure 1, the Meta Materials laminated film of the present invention is mainly by soft light base material, single metal nano particle
The metamaterial layer 2 and nitrite ion sensitive membrane 3 of basic structural unit are composed, and specific embodiments of the present invention are as follows：
Embodiment one (as shown in Figure 2)：Air liquid interface independently fills mode
(1) hard substrate 4 cleans：It is dry by sheet glass, silicon chip or sheet metal after water, acetone, water are cleaned by ultrasonic.
(2) preparation of metamaterial layer：The metal nano of various unlike materials, size and pattern is synthesized using wet chemistry method
Grain colloidal sol 10, then be scattered in metal nanoparticle in water phase by above-mentioned and be transferred in organic solvent, specific method is as follows：By 5mL
Metal nanoparticle colloidal sol is mixed with dissolved with the chloroformic solution of 0.1mg/mL sulfydryls-polyethylene glycol (average molecular weight 5000)；It is molten
After liquid layering, 1mL methanol is rapidly joined in water phase, inducible metal nanoparticle is transferred in chloroformic solution；Gained disperses
The metal nanoparticle in chloroform removes sulfydryl-polyethylene glycol excessive in solution through washing repeatedly, is concentrated into 50 μ L chloroforms
For use.
By above-mentioned cleaned hard substrate 4 as on levelling bench, adding in a certain amount of water, the entire base of covering of formation
The moisture film 5 on material surface.Using syringe pump 6 and syringe 7, on moisture film gas liquid interface injecting above-mentioned metal nanoparticle has
Machine colloidal sol until metal nanoparticle is paved with entire moisture film, forms orderly metal nanoparticle array 8.After water film evaporation,
It can be formed by super material layer 2 of the single metal nano particle for basic structural unit；
(3) preparation of meta-material thin film：Polymer precursor is spun on above-mentioned metal nanoparticle array surface, is heated
It is removed after curing, metal nanoparticle array can be transferred on flexible parent metal 1, form the meta-material thin film of soft light.
(4) preparation of nitrite ion sensitive membrane 3：100 μM of p-Mercaptoaniline solution of 1mL is placed in above-mentioned super material
Expect on film, after static 1 hour, wash with water repeatedly, one layer of p-Mercaptoaniline monomolecular film can be formed on Meta Materials surface.
Embodiment two (as shown in Figure 3)：Liquid/liquid interface independently fills mode
The mode that liquid/liquid interface can also be utilized independently to fill prepares metal nanoparticle array, and concrete operations are as follows：Holding
In device 9, by 5mL metal nanoparticles colloidal sol 10 and 5mL toluene 11；After solution layering, using syringe pump 6 and syringe 7,
With the rate of 100 μ L/min injection 12mL, alcohol, inducible metal nanoparticle are formed in toluene/water boundary in metal-sol
Compact arranged metal nanoparticle array 8 can be fished for the hard substrate 4 through over cleaning, after being completely dried, can be formed by
Single metal nano particle be basic structural unit Meta Materials material layer 2 (as shown in Figure 4), remaining operations step with above-mentioned (3)-
(4)。
Metal Nano structure can generate surface plasma body resonant vibration and show under Vis/NIR Spectroscopy excitation in metamaterial layer
As with that under the synergistic effect of sample Central Asia salt nitrate ion, can be joined with p-Mercaptoaniline generation azo in efficient catalytic sensitive membrane
Benzene class chemicals (see Fig. 5).It, can because the Raman spectrum of azo biphenyl class chemicals has notable area (see Fig. 6) with p-Mercaptoaniline
This reaction directly is monitored using Raman spectrum, and then realizes specific recognition and the detection to nitrite ion indirectly, specifically
Embodiment is as follows：
Embodiment three：Nitrous acid detects in liquid sample
As shown in fig. 7, adding in the hydrochloric acid of 1 μ L 1M in fluid sample 12 to be detected 20 μ L, sample 12 is placed in after mixing
It is uniformly placed on above-mentioned film, acquisition visible/near infrared band laser 13 utilizes Raman spectrometer 14 and light as light source
Fibre 15 acquires the Raman spectrum of film surface, can measure the content of nitrite in fluid sample 12 (see Fig. 8).Above-mentioned detection side
Method has very high selectivity and antijamming capability (see Fig. 9).
Example IV：Nitrous acid detects in solid sample surface
As shown in Figure 10, because the Meta Materials laminated film of the present invention have good flexibility and translucency (see Figure 11,
Raman signal can be all collected from obverse and reverse sides), it of the invention can also be detected for solid sample surface nitrite, specifically
Operation is as follows：The hydrochloric acid solution of 10 μ L 10mM is placed in 16 surface of solid sample to be detected, dissolves the nitrite on surface,
Meta-material thin film is attached and solid sample surface again.
Then in a manner that embodiment three is identical, acquisition visible/near infrared band laser 13 is as light source, from super material
The material laminated film back side is irradiated to solid sample surface through Meta Materials laminated film, is adopted using Raman spectrometer 14 and optical fiber 15
Collect the Raman spectrum of film surface, the content of nitrite in fluid sample can be measured.Since the meta-material thin film of the present invention has
There is good translucency, therefore Raman spectrum can be acquired from the Meta Materials laminated film back side and detected for nitrite.
Although the present invention is disclosed with specific embodiment, it is not limited to the present invention, the technology of any this field
Personnel, the displacement of made equivalent assemblies or according to patent of the present invention under the premise of the spirit and scope of the present invention are not departed from
The equivalent variations and modification that protection domain is made all should still belong to the scope that this patent is covered.
Claims (10)
1. a kind of soft light Meta Materials laminated film for nitrite detection, it is characterised in that：
Including base material (1), using flexible and transparent material；
Including metamaterial layer (2), be formed on base material (1), be by single metal nano particle be the orderly battle array of basic structural unit
Row are formed；
It including nitrite sensitive membrane (3), is formed on Meta Materials (2), is the list being made of p-Mercaptoaniline molecular self-assembling
Molecular film, the detected nitrite of nitrite sensitive membrane (3) contact.
2. a kind of making side of soft light Meta Materials laminated film for nitrite detection as described in claim 1
Method, it is characterised in that：It is first prepared on base material (1) and forms single metal nano particle as basic structural unit oldered array composition
Metamaterial layer (2), then prepared in a manner that molecule independently fills by p-Mercaptoaniline on metamaterial layer (2) surface formed from
Monomolecular film is assembled, as nitrite sensitive membrane (3).
3. a kind of making side of soft light Meta Materials laminated film for nitrite detection according to claim 2
Method, it is characterised in that：Described being prepared on base material forms single metal nano particle as basic structural unit oldered array structure
Into metamaterial layer (2) be specially：
(1) orderly metal is first built in air/water boundary or organic solvent/aqueous phase interface using interface self assembly mode
Nano-grain array；
(2) metal nanoparticle array is transferred to flexible parent metal surface again.
4. a kind of making side of soft light Meta Materials laminated film for nitrite detection according to claim 2
Method, it is characterised in that：P-Mercaptoaniline solution is added drop-wise to after being stood on metamaterial layer (2) surface described in obtaining by sulfydryl benzene
The self-assembled monolayer that amine is formed.
5. a kind of nitrite detection method, it is characterised in that：Detected sample is placed on flexible and transparent described in claim 1 and surpasses
Material film or the nitrite based on flexible and transparent meta-material thin film made of any production methods of claim 2-4
It in sensitive membrane (3), is irradiated with the laser of visible/near infrared, is obtained in sample to be tested by Raman spectroscopy instrument acquisition signal
The testing result of nitrite ion.
6. soft light Meta Materials laminated film according to claim 1 or any making sides of claim 2-4
A kind of nitrite detection method described in flexible and transparent meta-material thin film made of method or claim 5, it is characterised in that：
Under Vis/NIR Spectroscopy excitation, metamaterial layer (2) generates surface plasma body resonant vibration, the surface ion in metamaterial layer (2)
Under the common synergistic effect of body and The sub-salt nitrate ion, the p-Mercaptoaniline in nitrite sensitive membrane (3) is induced to be converted into idol
Nitrogen biphenol compound is to carry out nitrite detection.
7. soft light Meta Materials laminated film according to claim 1 or any making sides of claim 2-4
A kind of nitrite detection method described in flexible and transparent meta-material thin film made of method or claim 5, it is characterised in that：
The Raman of surface plasma body resonant vibration amplification absorption molecule in nitrite sensitive membrane (3) that the metamaterial layer (2) generates
Signal is to improve the sensitivity of detection.
8. soft light Meta Materials laminated film according to claim 1 or any making sides of claim 2-4
A kind of nitrite detection method described in flexible and transparent meta-material thin film made of method or claim 5, it is characterised in that：
Nitrite detection of the flexible and transparent meta-material thin film suitable for fluid sample and solid sample.
9. a kind of nitrite detection method according to claim 5, it is characterised in that：The detected sample is liquid
Body sample or solid sample are fluid sample for detected sample, then fluid sample are added dropwise in flexible and transparent Meta Materials
Nitrite sensitive membrane (3) surface that film is placed；Be fluid sample for detected sample, then it is flexible and transparent Meta Materials are thin
Nitrite sensitive membrane (3) surface that film is placed is attached on solid sample.
10. soft light Meta Materials laminated film according to claim 1 or any making sides of claim 2-4
Flexible and transparent meta-material thin film made of method, it is characterised in that：The material of the metal nanoparticle for gold, silver, platinum, copper one
Kind or the alloy of a variety of mixing.
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| CN109856134B (en) * | 2019-02-21 | 2021-04-27 | 上海历思实业有限公司 | Copper ion detection reagent, test paper, preparation method and application in copper ion detection |
| CN114199854A (en) * | 2021-12-15 | 2022-03-18 | 曲阜师范大学 | Preparation method of SERS substrate constructed by flexible transparent cone ordered array |
| CN114199854B (en) * | 2021-12-15 | 2024-01-12 | 曲阜师范大学 | Preparation method of SERS substrate constructed by flexible transparent cone ordered array |
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