CN105675579A - Silver cubic nanoparticle-polyethylene flexible transparent film as well as preparation method and application thereof - Google Patents
Silver cubic nanoparticle-polyethylene flexible transparent film as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a silver cubic nanoparticle-polyethylene flexible transparent film as well as a preparation method and an application thereof. The transparent film comprises a polyethylene film and single layer silver cubic nanoparticles which covers on the polyethylene film, wherein the thickness of the polyethylene film is 18-25[mu]m, and the side length of the silver cubic nanoparticle is 50-60nm; the silver cubic nanoparticles are obtained by using a liquid phase method, an ethanol solution of the silver cubic nanoparticles and toluene are mixed, ultrasonic dispersion is carried out, dispersion liquid is obtained, the dispersion liquid is dropped into water, a single layer silver cubic nanoparticle film which suspends on water surface is obtained, the polyethylene film is used for peeling the silver cubic nanoparticle film on the water surface, and a target product is prepared. The film can be cut into any shapes and sizes, and has the advantages of light weight, portability and low cost; the film is easy to be bent and deformed randomly, the front side and the back side can be used as a SERS active substrate, a laser Raman spectrometer can be used for measuring rhodamine, or thiram, or methyl parathion, or polychlorinated biphenyl PCB-3 which are adhered to the film.
Description
Technical field
The present invention relates to a kind of nano particle-transparent film and preparation method and purposes, especially a kind of silver cubic nanometer particle-polyethylene flexible transparent film and its production and use.
Background technology
Surface phasmon nano particle has unique optical property, the fields such as phase, storage, near field optic, sensing, catalysis and surface enhanced Raman scattering (SERS) it are widely used for into, such as a kind of silver nanoparticle square-sodium polyacrylate laminated film of the applicant that Chinese invention patent CN102975454B announced on June 24th, 2015 and its production and use. The thickness of laminated film recorded in this patent of invention is 100nm, is coated with the silver nanoparticle square of sodium polyacrylate by it and sodium polyacrylate forms; Preparation method first adopts liquid phase method to obtain silver nanoparticle square, again by silver nanoparticle square ethanolic soln or silver nanoparticle square N, dinethylformamide solution and sodium polyacrylate aqueous solution and ultrasonic obtain mixed body fluid after, mixed body fluid is dripped and dries on substrate, obtained product. Though this kind of product can be used as SERS substrate to measure gas chromatography, but all there is shortcoming part with its preparation method, first, silver nanoparticle square is wrapped among sodium polyacrylate, have impact on giving full play to of effect of its relatively strong electromagnetic enhancing being generally suitable for, make its can only pollutent in adsorption aqueous solution, the determinand for other solution can not adsorb, and hinders testing molecule and enters into " focus "; Secondly, when it can be used as SERS substrate to use, because incidence exciting light is blocked effect by substrate, therefore its front can only be used, bringing inconvenience to the detection of some specific occasion; Again, preparation method can not obtain and have the SERS substrate that general suitable relatively strong electromagnetic strengthens effect.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming shortcoming part of the prior art, it is provided that a kind of structure is simple, has silver-colored cubic nanometer particle-polyethylene flexible transparent film that general suitable relatively strong electromagnetic strengthens effect.
Another technical problem that the present invention to be solved is for providing the preparation method of a kind of above-mentioned silver cubic nanometer particle-polyethylene flexible transparent film.
Another technical problem that the present invention to be solved is for providing the purposes of a kind of above-mentioned silver cubic nanometer particle-polyethylene flexible transparent film.
For solving the technical problem of the present invention, the technical scheme adopted is: silver cubic nanometer particle-polyethylene flexible transparent film comprises silver cubic nanometer particle, particularly,
By being covered with on polyethylene film, single silver cubic nanometer particle forms described flexible transparent film;
The thickness of described polyethylene film is 18～25 μm;
The length of side of described silver cubic nanometer particle is 50～60nm.
Further improvement as silver cubic nanometer particle-polyethylene flexible transparent film:
Preferably, it is orderly dense arrangement between silver cubic nanometer particle.
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of above-mentioned silver cubic nanometer particle-polyethylene flexible transparent film comprises use liquid phase method and obtains silver cubic nanometer particle, and particularly completing steps is as follows:
Step 1, first is the ratio of 0.08～0.12:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 0.8～1.2g/L and the polyvinylpyrrolidone pentanediol solution of 14～18g/L, sodium-chlor ethylene glycol solution is added and polyvinylpyrrolidone pentanediol solution stirs evenly, obtain mixed solution, again according to the Silver Nitrate pentanediol solution of 14～18g/L, the weight ratio of mixed solution and pentanediol is the ratio of 3:3:4～6, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously under stirring, the pentanediol of 145～155 DEG C react at least after 3h, it is used frozen water cooling cancellation reaction, obtain reaction solution,
Step 2, after first using alcohol dilution reaction solution, it is carried out the process of solid-liquid separation and washing, obtain silver cubic nanometer particle, it is the ratio of 1:0.8～1.2 according to the silver-colored cubic nanometer particle ethanolic soln of 2.5～3.5g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse is 3min at least, obtains dispersion liquid;
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface, re-uses polyethylene film and peels off the silver-colored cubic nanometer membrana granulosa on the water surface, obtained silver cubic nanometer particle-polyethylene flexible transparent film.
Further improvement as the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film:
Preferably, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29.
Preferably, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min.
Preferably, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min.
Preferably, carrying out washing treatment be use successively ethanol and deionized water to be separated the solids obtained clean, during cleaning, separation solids is centrifugation.
Preferably, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with.
For solving another technical problem of the present invention, another technical scheme adopted is: the purposes of above-mentioned silver cubic nanometer particle-polyethylene flexible transparent film is,
Using silver cubic nanometer particle-polyethylene flexible transparent film as the active substrate of surface enhanced Raman scattering, using laser Raman spectrometer to measure the content of the organism of attachment on it, described organism is rhodamine, or Fu Meishuan, or parathion-methyl, or polychlorobiphenyl PCB-3.
Further improvement as the purposes of silver cubic nanometer particle-polyethylene flexible transparent film:
Preferably, the wavelength of the exciting light of laser Raman spectrometer to be 532nm, power be 0.05～0.25mW, integral time are 5～20s.
Relative to the useful effect of prior art it is:
Its one, use scanning electron microscope and X-ray diffractometer to characterize respectively obtained object product, by its result, it will be seen that object product is by being covered with on polyethylene film, individual layer cubic nanometer particle forms, wherein, the thickness of polyethylene film is 18～25 μm, and the length of side of cubic nanometer particle is 50～60nm. cubic nanometer particle is silver cubic nanometer particle. it is orderly dense arrangement between silver cubic nanometer particle. the object product that this kind is dressed up by the single silver cubic nanometer groups of grains being covered with on polyethylene film and its, both owing to silver cubic nanometer particle has extremely high SERS Electromagnetic enhancement effect, again because silver cubic nanometer particle is directly in the face of determinand, also owing to the exciting light of incidence is hyalosome by polyethylene film, more because polyethylene film is flexible material, thus it is active to make object product not only have high SERS, also it is convenient to directly be affixed on or be wrapped on the determinand with complex surface, laser Raman spectrometer is used to detect the organic pollutant of solid surface to be measured by the back side of polyethylene film.
Its two, using obtained object product as SERS active-substrate, the tests of the repeatedly many batches under rhodamine, Fu Meishuan, parathion-methyl and polychlorobiphenyl PCB-3 carry out different concns respectively, when the concentration of analyte rhodamine is low to moderate 10-16The concentration of mol/L, Fu Meishuan is low to moderate 10-8The concentration of mol/L, parathion-methyl is low to moderate 10-8The concentration of mol/L, polychlorobiphenyl PCB-3 is low to moderate 10-6During mol/L, still it can be detected effectively, and consistence of its detection and the multiple spot of repeatability on object product and any point all very good.
Its three, preparation method is simple, science, efficient. not only obtain structure simple, there is object product silver cubic nanometer particle-polyethylene flexible transparent film that general suitable relatively strong electromagnetic strengthens effect, also make it have and can arbitrarily bend and distortion, and positive and negative two sides all can be used as the performance of SERS active-substrate use, more there is manufacture craft simple, the feature that cost is low, make use of the not capacitive of toluene and water particularly ingeniously, the surface tension of the capillary force that silver cubic nanometer particle exists in solution surface and water, achieve the self-assembly to silver cubic nanometer particle, make it be self-assembled into one layer in the interface of air/water to be evenly distributed, compact arranged silver cubic nanometer granular cell layer film, thus be to flexible and transparent by silver cubic nanometer transfer of granules, surface has lays a good foundation on the polyethylene film of certain viscosity, and obtain therefrom and there is the active height of SERS, the uniform flexible and transparent SERS substrate of signal. this kind of air/water interface self-assembly method, except the self-assembly for nano particle provides a kind of assembling thinking newly, also provides a kind of effective method for preparing the transparent SERS substrate of large area flexible, thus make object product can be tailored to arbitrary shape and size, and there is light weight, portable and inexpensive advantage, very easily in being widely used in fast detection of trace environmental pollutant field, and the practical application promoting SERS technology is had important meaning.
Accompanying drawing explanation
Fig. 1 is one of the object product that preparation method obtained result of using scanning electron microscope (SEM) and laser Raman spectrometer to characterize.Wherein, the SEM image of product for the purpose of Fig. 1 a; The SERS spectrogram of product for the purpose of Fig. 1 b, for the purpose of the upper curve in figure, the SERS in product front composes the SERS spectrum line at the product back side for the purpose of line, lower curve.
Fig. 2 is respectively to one of result that the object product use laser Raman spectrometer containing different concns rhodamine, Fu Meishuan characterizes. Wherein, Fig. 2 a is the SERS spectrogram of the object product containing different concns rhodamine; Fig. 2 b is the SERS spectrogram containing the rich U.S. two object product of different concns, and the standard SERS that the curve bottom spectrogram is rich U.S. two powder composes line.
Fig. 3 is respectively to one of result that the object product use laser Raman spectrometer containing different concns parathion-methyl, polychlorobiphenyl PCB-3 characterizes. Wherein, Fig. 3 a is the SERS spectrogram of the object product containing different concns parathion-methyl, and the standard SERS that the curve bottom it is parathion-methyl powder composes line; Fig. 3 b is the SERS spectrogram of the object product containing different concns polychlorobiphenyl PCB-3, and the standard SERS that the curve bottom it is polychlorobiphenyl PCB-3 powder composes line.
Embodiment
Below in conjunction with accompanying drawing, the optimal way of the present invention is described in further detail.
First buy from market or obtain voluntarily:
Sodium-chlor; Ethylene glycol; Polyvinylpyrrolidone; Pentanediol; Silver Nitrate; Ethanol; Toluene; Thickness is the polyethylene film of 0.5～1.5mm.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, first is the ratio of 0.08:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 0.8g/L and the polyvinylpyrrolidone pentanediol solution of 18g/L, is added by sodium-chlor ethylene glycol solution and stirs evenly in polyvinylpyrrolidone pentanediol solution; Wherein, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29, obtain mixed solution. It is the ratio of 3:3:4 according to the weight ratio of the Silver Nitrate pentanediol solution of 14g/L, mixed solution and pentanediol again, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously and stirs after pentanediol lower, 145 DEG C reacts 4h, it uses frozen water cooling cancellation react; Wherein, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min, obtain reaction solution.
Step 2, after first using alcohol dilution reaction solution, carries out the process of solid-liquid separation and washing to it; Wherein, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min, carrying out washing treatment be use successively ethanol and deionized water to being separated the solids obtained clean, being separated solids during cleaning is centrifugation, obtains silver cubic nanometer particle. Being the ratio of 1:0.8 according to the silver-colored cubic nanometer particle ethanolic soln of 2.5g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse 5min, obtains dispersion liquid.
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface. Re-use polyethylene film and peel off the silver-colored cubic nanometer membrana granulosa on the water surface; Wherein, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with. Obtain and it is similar to shown in Fig. 1 a, and the silver-colored cubic nanometer particle-polyethylene flexible transparent film as shown in the curve in Fig. 1 b.
Embodiment 2
The concrete steps of preparation are:
Step 1, first is the ratio of 0.09:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 0.9g/L and the polyvinylpyrrolidone pentanediol solution of 17g/L, is added by sodium-chlor ethylene glycol solution and stirs evenly in polyvinylpyrrolidone pentanediol solution;Wherein, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29, obtain mixed solution. It is the ratio of 3:3:4.5 according to the weight ratio of the Silver Nitrate pentanediol solution of 15g/L, mixed solution and pentanediol again, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously and stirs after pentanediol lower, 148 DEG C reacts 3.8h, it uses frozen water cooling cancellation react; Wherein, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min, obtain reaction solution.
Step 2, after first using alcohol dilution reaction solution, carries out the process of solid-liquid separation and washing to it; Wherein, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min, carrying out washing treatment be use successively ethanol and deionized water to being separated the solids obtained clean, being separated solids during cleaning is centrifugation, obtains silver cubic nanometer particle. Being the ratio of 1:0.9 according to the silver-colored cubic nanometer particle ethanolic soln of 2.8g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse 4.5min, obtains dispersion liquid.
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface. Re-use polyethylene film and peel off the silver-colored cubic nanometer membrana granulosa on the water surface; Wherein, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with. Obtain and it is similar to shown in Fig. 1 a, and the silver-colored cubic nanometer particle-polyethylene flexible transparent film as shown in the curve in Fig. 1 b.
Embodiment 3
The concrete steps of preparation are:
Step 1, first is the ratio of 0.1:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 1g/L and the polyvinylpyrrolidone pentanediol solution of 16g/L, is added by sodium-chlor ethylene glycol solution and stirs evenly in polyvinylpyrrolidone pentanediol solution; Wherein, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29, obtain mixed solution. It is the ratio of 3:3:5 according to the weight ratio of the Silver Nitrate pentanediol solution of 16g/L, mixed solution and pentanediol again, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously and stirs after pentanediol lower, 150 DEG C reacts 3.5h, it uses frozen water cooling cancellation react; Wherein, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min, obtain reaction solution.
Step 2, after first using alcohol dilution reaction solution, carries out the process of solid-liquid separation and washing to it; Wherein, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min, carrying out washing treatment be use successively ethanol and deionized water to being separated the solids obtained clean, being separated solids during cleaning is centrifugation, obtains silver cubic nanometer particle. Being the ratio of 1:1 according to the silver-colored cubic nanometer particle ethanolic soln of 3g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse 4min, obtains dispersion liquid.
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface. Re-use polyethylene film and peel off the silver-colored cubic nanometer membrana granulosa on the water surface; Wherein, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with. Obtain as shown in Figure 1a, and the silver-colored cubic nanometer particle-polyethylene flexible transparent film as shown in the curve in Fig. 1 b.
Embodiment 4
The concrete steps of preparation are:
Step 1, first is the ratio of 0.11:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 1.1g/L and the polyvinylpyrrolidone pentanediol solution of 15g/L, is added by sodium-chlor ethylene glycol solution and stirs evenly in polyvinylpyrrolidone pentanediol solution; Wherein, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29, obtain mixed solution. It is the ratio of 3:3:5.5 according to the weight ratio of the Silver Nitrate pentanediol solution of 17g/L, mixed solution and pentanediol again, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously and stirs after pentanediol lower, 153 DEG C reacts 3.3h, it uses frozen water cooling cancellation react; Wherein, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min, obtain reaction solution.
Step 2, after first using alcohol dilution reaction solution, carries out the process of solid-liquid separation and washing to it; Wherein, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min, carrying out washing treatment be use successively ethanol and deionized water to being separated the solids obtained clean, being separated solids during cleaning is centrifugation, obtains silver cubic nanometer particle. Being the ratio of 1:1 according to the silver-colored cubic nanometer particle ethanolic soln of 3.3g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse 3.5min, obtains dispersion liquid.
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface. Re-use polyethylene film and peel off the silver-colored cubic nanometer membrana granulosa on the water surface; Wherein, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with. Obtain and it is similar to shown in Fig. 1 a, and the silver-colored cubic nanometer particle-polyethylene flexible transparent film as shown in the curve in Fig. 1 b.
Embodiment 5
The concrete steps of preparation are:
Step 1, first is the ratio of 0.12:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 1.2g/L and the polyvinylpyrrolidone pentanediol solution of 14g/L, is added by sodium-chlor ethylene glycol solution and stirs evenly in polyvinylpyrrolidone pentanediol solution; Wherein, polyvinylpyrrolidone to be molecular weight be 58000 polyvinylpyrrolidone K29, obtain mixed solution. It is the ratio of 3:3:6 according to the weight ratio of the Silver Nitrate pentanediol solution of 18g/L, mixed solution and pentanediol again, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously and stirs after pentanediol lower, 155 DEG C reacts 3h, it uses frozen water cooling cancellation react; Wherein, the Silver Nitrate pentanediol solution of injection pentanediol, the speed of mixed solution are 600 μ L/min, obtain reaction solution.
Step 2, after first using alcohol dilution reaction solution, carries out the process of solid-liquid separation and washing to it; Wherein, solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min, carrying out washing treatment be use successively ethanol and deionized water to being separated the solids obtained clean, being separated solids during cleaning is centrifugation, obtains silver cubic nanometer particle. Being the ratio of 1:1.2 according to the silver-colored cubic nanometer particle ethanolic soln of 3.5g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse 3min, obtains dispersion liquid.
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface. Re-use polyethylene film and peel off the silver-colored cubic nanometer membrana granulosa on the water surface; Wherein, peel off as first polyethylene film being overlying on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with. Obtain and it is similar to shown in Fig. 1 a, and the silver-colored cubic nanometer particle-polyethylene flexible transparent film as shown in the curve in Fig. 1 b.
The purposes of silver cubic nanometer particle-polyethylene flexible transparent film is,
Using silver cubic nanometer particle-polyethylene flexible transparent film as the active substrate of surface enhanced Raman scattering, it may also be useful to laser Raman spectrometer measures it on the content of the organism adhered to; Wherein, the wavelength of the exciting light of laser Raman spectrometer to be 532nm, power be 0.05～0.25mW, integral time are 5～20s.
When organism is rhodamine, the result of detection is as shown in the curve in Fig. 2 a.
When organism is rich beautiful pair, the result of detection is as shown in the curve in Fig. 2 b.
When organism is parathion-methyl, the result of detection is as shown in the curve in Fig. 3 a.
When organism is polychlorobiphenyl PCB-3, the result of detection is as shown in the curve in Fig. 3 b.
Obviously, silver-colored cubic nanometer particle-polyethylene flexible transparent film of the present invention and its production and use can be carried out various change and modification and not depart from the spirit and scope of the present invention by the technician of this area. Like this, if these amendments and modification to the present invention belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these and changes and modification.
Claims (10)
1. silver-colored cubic nanometer particle-polyethylene flexible transparent film, comprises silver cubic nanometer particle, it is characterised in that:
By being covered with on polyethylene film, single silver cubic nanometer particle forms described flexible transparent film;
The thickness of described polyethylene film is 18～25 μm;
The length of side of described silver cubic nanometer particle is 50～60nm.
2. silver cubic nanometer particle-polyethylene flexible transparent film according to claim 1, is characterized in that being orderly dense arrangement between silver cubic nanometer particle.
3. a preparation method for silver cubic nanometer particle-polyethylene flexible transparent film described in claim 1, comprises and uses liquid phase method to obtain silver cubic nanometer particle, it is characterised in that completing steps is as follows:
Step 1, first is the ratio of 0.08～0.12:3 according to the weight ratio of the sodium-chlor ethylene glycol solution of 0.8～1.2g/L and the polyvinylpyrrolidone pentanediol solution of 14～18g/L, sodium-chlor ethylene glycol solution is added and polyvinylpyrrolidone pentanediol solution stirs evenly, obtain mixed solution, again according to the Silver Nitrate pentanediol solution of 14～18g/L, the weight ratio of mixed solution and pentanediol is the ratio of 3:3:4～6, Silver Nitrate pentanediol solution and mixed solution are injected simultaneously under stirring, the pentanediol of 145～155 DEG C react at least after 3h, it is used frozen water cooling cancellation reaction, obtain reaction solution,
Step 2, after first using alcohol dilution reaction solution, it is carried out the process of solid-liquid separation and washing, obtain silver cubic nanometer particle, it is the ratio of 1:0.8～1.2 according to the silver-colored cubic nanometer particle ethanolic soln of 2.5～3.5g/L and the volume ratio of toluene again, after silver cubic nanometer particle ethanolic soln and toluene being mixed, ultrasonic disperse is 3min at least, obtains dispersion liquid;
Step 3, first enters in water by dispersant liquid drop, obtains the single silver cubic nanometer membrana granulosa being suspended on the water surface, re-uses polyethylene film and peels off the silver-colored cubic nanometer membrana granulosa on the water surface, obtained silver cubic nanometer particle-polyethylene flexible transparent film.
4. the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 3, is characterized in that polyvinylpyrrolidone to be molecular weight is the polyvinylpyrrolidone K29 of 58000.
5. the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 3, it is characterized in that injecting the Silver Nitrate pentanediol solution of pentanediol, the speed of mixed solution be 600 μ L/min.
6. the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 3, is characterized in that solid-liquid separation is treated to centrifugation, and its rotating speed is 14000r/min, time is 15min.
7. the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 3, it is characterized in that carrying out washing treatment be use successively ethanol and deionized water to be separated the solids obtained clean, during cleaning, separation solids is centrifugation.
8. the preparation method of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 3, it is characterized in that peeling off as to be first overlying on by polyethylene film on the silver-colored cubic nanometer membrana granulosa on the water surface, then the polyethylene film lift-off water surface of silver cubic nanometer particle will be stained with.
9. the purposes of silver cubic nanometer particle-polyethylene flexible transparent film described in a claim 1, it is characterised in that:
Using silver cubic nanometer particle-polyethylene flexible transparent film as the active substrate of surface enhanced Raman scattering, using laser Raman spectrometer to measure the content of the organism of attachment on it, described organism is rhodamine, or Fu Meishuan, or parathion-methyl, or polychlorobiphenyl PCB-3.
10. the purposes of silver cubic nanometer particle-polyethylene flexible transparent film according to claim 9, is characterized in that the wavelength of the exciting light of laser Raman spectrometer to be 532nm, power is that 0.05～0.25mW, integral time are 5～20s.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107478638A (en) * | 2017-07-17 | 2017-12-15 | 中国科学院合肥物质科学研究院 | Individual layer counter opal structure of silver nano-grain assembling and its production and use |
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| CN109030453A (en) * | 2018-07-04 | 2018-12-18 | 浙江工业大学 | A kind of preparation method and application of flexible and transparent SERS substrate |
| CN109253998A (en) * | 2018-10-25 | 2019-01-22 | 珠海彩晶光谱科技有限公司 | Metal-wrappage-antibody composite nanoparticle quantitative detection tumor marker method based on Raman enhancing |
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