CN104195551B - The CNT of modified by silver nanoparticles-eggshell membrane composite S ERS substrate and its production and use - Google Patents
The CNT of modified by silver nanoparticles-eggshell membrane composite S ERS substrate and its production and use Download PDFInfo
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- CN104195551B CN104195551B CN201410451960.XA CN201410451960A CN104195551B CN 104195551 B CN104195551 B CN 104195551B CN 201410451960 A CN201410451960 A CN 201410451960A CN 104195551 B CN104195551 B CN 104195551B
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Abstract
The invention discloses the CNT of a kind of modified by silver nanoparticles-eggshell membrane composite S ERS substrate and its production and use. SERS substrate is by the CNT being carried on eggshell membrane, and modifies the silver nano-grain composition on CNT, and CNT length is 0.5～2 μm, pipe diameter is 30～50nm, and the particle diameter of silver nano-grain is 5～10nm; Method dissolves to obtain eggshell membrane for being first placed in acetum by Ovum crusta Gallus domesticus, it is placed in ammonia spirit by eggshell membrane the ultrasonic eggshell membrane that must have alkalized again, afterwards, first carboxylated CNT is scattered in deionized water for ultrasonic and obtains carbon nano-tube solution, to be placed in carbon nano-tube solution by the eggshell membrane alkalized again ultrasonic, and area load has the eggshell membrane of CNT, finally, it is placed in sputter sputtering silver, prepares purpose product. It as the active substrate of surface enhanced raman spectroscopy, can use laser Raman spectrometer to measure the rhodamine of attachment on it or the content of parathion-methyl or Polychlorinated biphenyls PCB-3 or bovine serum albumin.
Description
Technical field
The present invention relates to a kind of SERS substrate and preparation method and purposes, the CNT of especially a kind of modified by silver nanoparticles-eggshell membrane composite S ERS substrate and its production and use.
Background technology
Relevant Theoretical Calculation and experimentation show, surface enhanced raman spectroscopy (SERS) substrate being construction unit with nano materials such as noble metal gold, silver, copper, when gap between noble metal nano structure is less than 10nm, substrate has high SERS activity, meanwhile, if base material has great specific surface area and the characterization of adsorption that target molecule has been had, it is beneficial to target molecule in the absorption of substrate surface and enrichment, improves the sensitivity of detection. furthermore, the repeatability of signal uniformity and measurement result in order to ensure substrate, it is desirable to suprabasil nanostructured is evenly distributed in large-area scope. at present, people are in order to obtain equally distributed nanostructured substrate, often by electro-deposition, photoetching, the technology such as electron beam lithography, as being entitled as " InvertedSize-dependenceofSurface-enhancedRamanScattering onGoldNanoholeandNanodiskArrays ", Yu, Q.etal, NanoLett., 2008, 8 (7), 1923-1928 (" surface-enhanced Raman signals of the gold nano hole/nanometer plate array dependency to substrate nano-scale ", " nanometer periodical " the 8th volume the 7th phase 1923～1928 pages in 2008) and " Nanohole-EnhancedRamanScattering. " Brolo, A.G.etal, NanoLett., 2004, 4 (10), (Raman signal that nano aperture causes strengthens 2015-2018, " nanometer periodical " the 4th volume the 10th phase 2015～2018 pages in 2004) article is introduced.Though using the various technological means mentioned in these articles also can obtain the nanostructured substrate being evenly distributed in wide area, but it being expensive to there is required instrument and equipment, complicated process of preparation, cost are high, the defect being difficult to overcome of time-consuming power consumption.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming weak point of the prior art, it is provided that a kind of carrier is economic and environment-friendly, and the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles that nanostructured thereon is evenly distributed.
Another technical problem that the invention solves the problems that preparation method for providing the CNT-eggshell membrane composite S ERS substrate of a kind of above-mentioned modified by silver nanoparticles.
Another technical problem that the invention solves the problems that is for providing the purposes of the CNT-eggshell membrane composite S ERS substrate of a kind of above-mentioned modified by silver nanoparticles.
For solving the technical problem of the present invention, the technical scheme adopted is: the CNT of modified by silver nanoparticles-eggshell membrane composite S ERS substrate includes silver nano-grain, particularly,
Described composite S ERS substrate is by the CNT being carried on eggshell membrane, and modifies the silver nano-grain composition on CNT;
The pipe range of described CNT is 0.5～2 μm, pipe diameter is 30～50nm;
The particle diameter of described silver nano-grain is 5～10nm.
Further improvement as the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles:
Preferably, eggshell membrane is the porous network of the eggshell membrane fiber composition of diameter 300～2000nm.
For solving another technical problem of the present invention, another technical scheme adopted is: the preparation method of the CNT of above-mentioned modified by silver nanoparticles-eggshell membrane composite S ERS substrate includes sputtering method, and particularly key step is as follows:
Step 1, first the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk is placed in the eggshell dissolving sclerotin in the acetum that concentration is 8～12wt%, obtain eggshell membrane, then eggshell membrane is placed in the ammonia spirit that concentration is 1～3vol% ultrasonic at least 3min, obtain the eggshell membrane alkalized;
Step 2, first carboxylated CNT is scattered in deionized water for ultrasonic at least 30min, obtain finely dispersed carbon nano-tube solution, the eggshell membrane alkalized is placed in ultrasonic at least 3min again in the carbon nano-tube solution that concentration is 400～600g/L, and obtaining area load has the eggshell membrane of CNT;
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 4～18min under 30～50mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles.
The further of preparation method as the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles is improved:
Preferably, before being placed in acetum by Ovum crusta Gallus domesticus, deionized water ultrasonic cleaning twice first it is used for.
Preferably, before to be placed in ammonia spirit by eggshell membrane ultrasonic, deionized water ultrasonic cleaning first it is used for.
Preferably, before to be placed in carbon nano-tube solution by the eggshell membrane alkalized ultrasonic, first it be used for deionized water ultrasonic cleaning and dry.
Preferably, when to be placed in by the eggshell membrane alkalized in the carbon nano-tube solution that concentration is 400～600g/L ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL; Ensure that the eggshell membrane alkalized can fully immerse in carbon nano-tube solution, lay a good foundation for making CNT be distributed evenly on eggshell membrane.
For solving another technical problem of the present invention, another technical scheme adopted is: the purposes of the CNT of above-mentioned modified by silver nanoparticles-eggshell membrane composite S ERS substrate is,
Using the CNT of the modified by silver nanoparticles-eggshell membrane composite S ERS substrate active substrate as surface enhanced raman spectroscopy, laser Raman spectrometer is used to measure the content of rhodamine (R6G) or parathion-methyl or Polychlorinated biphenyls PCB-3 or the bovine serum albumin adhered to it on.
The further of purposes as the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles is improved:
Preferably, the excitation wavelength of laser Raman spectrometer to be 532nm, output be 0.3～0.7mW, the time of integration are 3～7s; Not only ensure the accuracy of detection, be also easy to purpose product and measure on it giving full play to of rhodamine of attachment or parathion-methyl or Polychlorinated biphenyls PCB-3 or bovine serum albumin performance.
Provide the benefit that relative to prior art:
One, uses scanning electron microscope to characterize prepared purpose product, by its result it can be seen that purpose product is the numerous tubules being modified with nano-particle is carried on sturdy fiber; Wherein, sturdy fiber is the fiber of composition porous network shape eggshell membrane, and its diameter is 300～2000nm, and tubule is CNT, and its pipe range is 0.5～2 μm, pipe diameter is 30～50nm, and nano-particle is silver nano-grain, and its particle diameter is 5～10nm. This purpose product being assembled into by eggshell membrane, CNT and silver nano-grain, both due to as a kind of biological semi-permeable film, eggshell membrane has distribution rule, uniform nanoporous network structure in large-area scope, so making it have great specific surface area and to micromolecular characterization of adsorption, it it is the perfect carrier constructing D S ERS substrate; Again because being assembled into the CNT of fiber surface of composition eggshell membrane, and further increasing the uniformity of substrate, specific surface area and to micromolecular characterization of adsorption; Due also to CNT is modified with the silver nano-grain with high SERS activity and further makes SERS substrate become the composite S ERS three-dimensional substrates possessing higher SERS activity and uniformity.
Its two, using prepared purpose product as SERS active-substrate, through respectively rhodamine, parathion-methyl, Polychlorinated biphenyls PCB-3 and bovine serum albumin being carried out the tests of the repeatedly many batches under variable concentrations, when the concentration of measured object rhodamine is low to moderate 10-13Mol/L, parathion-methyl concentration be low to moderate 10-11Mol/L, Polychlorinated biphenyls PCB-3 concentration be low to moderate 10-6Mol/L, bovine serum albumin concentration when being low to moderate 0.1ppb, remain to effectively detect it, and multiple spot on purpose product of the concordance of its detection and repeatability and any point all very good.
Purpose product has so big Raman enhancer, and its reason is, one is pattern is the eggshell membrane of porous network and being assembled of CNT so that substrate has great specific surface area; CNT is to micromolecular adsorption simultaneously, it is achieved that target molecule, in suprabasil enrichment, improves sensitivity and the enhancer of detection; Two is that the silver nano-grain modified in carbon nano tube surface defines substantial amounts of SERS active site, in addition, except the Electromagnetic enhancement effect that the interaction between adjacent silver nano-grain causes, the enhancing of Raman signal is also served certain effect by the electromagnetic coupled enhancing between silver nano-grain on the eggshell membrane fiber not even together of the silver nano-grain on different CNTs.
They are three years old, preparation method is simple, science, efficiently, not only prepare carrier economic and environment-friendly, and the CNT-eggshell membrane composite S ERS substrate of purpose product modified by silver nanoparticles that nanostructured thereon is evenly distributed, after also making it coordinate with laser Raman spectrometer, possess the rhodamine or parathion-methyl or Polychlorinated biphenyls PCB-3 that adhere on which or bovine serum albumin has carried out the quick trace SERS function detected; More have technique simple, device simple, the required prices of raw materials are cheap, wide material sources, environmental protection feature; So that purpose product has extremely wide commercial application prospect in fields such as environment, chemistry, biologies.
Accompanying drawing explanation
Fig. 1 is respectively to one of result that the Primary product made in purpose product process, intermediate product and purpose product use scanning electron microscope (SEM) characterize. Wherein, Fig. 1 a is the SEM image of Primary product eggshell membrane, and Fig. 1 b is the SEM image after intermediate product eggshell membrane fibers adsorption CNT, the SEM image of product for the purpose of Fig. 1 c.
Fig. 2 is that the purpose product being attached with rhodamine on which uses laser Raman spectrometer to carry out one of result of characterizing. Wherein, Fig. 2 a is the SERS spectrogram of the purpose product that the time the is 12min detection variable concentrations rhodamine of sputtering silver; Fig. 2 b is 10 for taking 6 some detectable concentrations on purpose product at random-8The SERS spectrogram of the rhodamine of mol/L.
Fig. 3 is respectively to one of result that the purpose product being attached with variable concentrations parathion-methyl, Polychlorinated biphenyls PCB-3 and bovine serum albumin uses laser Raman spectrometer to characterize. Wherein, Fig. 3 a is SERS spectrogram during detection parathion-methyl; Fig. 3 b is SERS spectrogram during detection Polychlorinated biphenyls PCB-3; Fig. 3 c is SERS spectrogram during detection bovine serum albumin.
Detailed description of the invention
Below in conjunction with accompanying drawing, the optimal way of the present invention is described in further detail.
First buy from market or prepare by conventional method:
Egg; Acetic acid; Ammonia; Carboxylated CNT; Deionized water.
Then,
Embodiment 1
Concretely comprising the following steps of preparation:
Step 1, after the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk first uses deionized water ultrasonic cleaning twice, is placed on the eggshell dissolving sclerotin in the acetum that concentration is 8wt%, obtains eggshell membrane. After again eggshell membrane being used deionized water ultrasonic cleaning, it is placed on ultrasonic 3min in the ammonia spirit that concentration is 1vol%, obtains being similar to the eggshell membrane of the alkalization shown in Fig. 1 a.
Step 2, is first scattered in deionized water for ultrasonic 30min by carboxylated CNT, obtains finely dispersed carbon nano-tube solution. After the eggshell membrane alkalized using deionized water ultrasonic cleaning again and drying, being placed on ultrasonic 7min in the carbon nano-tube solution that concentration is 400g/L, obtaining being similar to the area load shown in Fig. 1 b has the eggshell membrane of CNT; Wherein, time ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 18min under 30mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate being similar to the modified by silver nanoparticles shown in Fig. 1 c.
Embodiment 2
Concretely comprising the following steps of preparation:
Step 1, after the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk first uses deionized water ultrasonic cleaning twice, is placed on the eggshell dissolving sclerotin in the acetum that concentration is 9wt%, obtains eggshell membrane.After again eggshell membrane being used deionized water ultrasonic cleaning, it is placed on ultrasonic 4min in the ammonia spirit that concentration is 1.5vol%, obtains being similar to the eggshell membrane of the alkalization shown in Fig. 1 a.
Step 2, is first scattered in deionized water for ultrasonic 33min by carboxylated CNT, obtains finely dispersed carbon nano-tube solution. After the eggshell membrane alkalized using deionized water ultrasonic cleaning again and drying, being placed on ultrasonic 6min in the carbon nano-tube solution that concentration is 450g/L, obtaining being similar to the area load shown in Fig. 1 b has the eggshell membrane of CNT; Wherein, time ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 15min under 35mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate being similar to the modified by silver nanoparticles shown in Fig. 1 c.
Embodiment 3
Concretely comprising the following steps of preparation:
Step 1, after the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk first uses deionized water ultrasonic cleaning twice, is placed on the eggshell dissolving sclerotin in the acetum that concentration is 10wt%, obtains eggshell membrane. Again eggshell membrane is used after deionized water ultrasonic cleaning, be placed on ultrasonic 5min in the ammonia spirit that concentration is 2vol%, obtain the eggshell membrane of alkalization as shown in Figure 1a.
Step 2, is first scattered in deionized water for ultrasonic 35min by carboxylated CNT, obtains finely dispersed carbon nano-tube solution. After the eggshell membrane alkalized using deionized water ultrasonic cleaning again and drying, being placed on ultrasonic 5min in the carbon nano-tube solution that concentration is 500g/L, obtaining area load as shown in Figure 1 b has the eggshell membrane of CNT; Wherein, time ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 12min under 40mA in electric current, the CNT-eggshell membrane composite S ERS substrate of prepared modified by silver nanoparticles as illustrated in figure 1 c.
Embodiment 4
Concretely comprising the following steps of preparation:
Step 1, after the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk first uses deionized water ultrasonic cleaning twice, is placed on the eggshell dissolving sclerotin in the acetum that concentration is 11wt%, obtains eggshell membrane. After again eggshell membrane being used deionized water ultrasonic cleaning, it is placed on ultrasonic 6min in the ammonia spirit that concentration is 2.5vol%, obtains being similar to the eggshell membrane of the alkalization shown in Fig. 1 a.
Step 2, is first scattered in deionized water for ultrasonic 38min by carboxylated CNT, obtains finely dispersed carbon nano-tube solution. After the eggshell membrane alkalized using deionized water ultrasonic cleaning again and drying, being placed on ultrasonic 4min in the carbon nano-tube solution that concentration is 550g/L, obtaining being similar to the area load shown in Fig. 1 b has the eggshell membrane of CNT; Wherein, time ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 8min under 45mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate being similar to the modified by silver nanoparticles shown in Fig. 1 c.
Embodiment 5
Concretely comprising the following steps of preparation:
Step 1, after the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk first uses deionized water ultrasonic cleaning twice, is placed on the eggshell dissolving sclerotin in the acetum that concentration is 12wt%, obtains eggshell membrane.After again eggshell membrane being used deionized water ultrasonic cleaning, it is placed on ultrasonic 7min in the ammonia spirit that concentration is 3vol%, obtains being similar to the eggshell membrane of the alkalization shown in Fig. 1 a.
Step 2, is first scattered in deionized water for ultrasonic 40min by carboxylated CNT, obtains finely dispersed carbon nano-tube solution. After the eggshell membrane alkalized using deionized water ultrasonic cleaning again and drying, being placed on ultrasonic 3min in the carbon nano-tube solution that concentration is 600g/L, obtaining being similar to the area load shown in Fig. 1 b has the eggshell membrane of CNT; Wherein, time ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 4min under 50mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate being similar to the modified by silver nanoparticles shown in Fig. 1 c.
The purposes of the CNT of modified by silver nanoparticles-eggshell membrane composite S ERS substrate is,
Using the CNT of the modified by silver nanoparticles-eggshell membrane composite S ERS substrate active substrate as surface enhanced raman spectroscopy, use laser Raman spectrometer to measure the rhodamine of attachment on it or the content of parathion-methyl or Polychlorinated biphenyls PCB-3 or bovine serum albumin, obtain result as shown in Figure 2 or Figure 3; Wherein, the excitation wavelength of laser Raman spectrometer to be 532nm, output be 0.3～0.7mW, the time of integration are 3～7s.
Obviously, the CNT of the modified by silver nanoparticles of the present invention-eggshell membrane composite S ERS substrate and its production and use can be carried out various change and modification without deviating from the spirit and scope of the present invention by those skilled in the art. So, 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 is also intended to comprise these and changes and modification.
Claims (5)
1. a preparation method for the CNT of modified by silver nanoparticles-eggshell membrane composite S ERS substrate, including sputtering method, it is characterised in that key step is as follows:
Step 1, first the Ovum crusta Gallus domesticus removing Ovum Gallus domesticus album and egg yolk is placed in the eggshell dissolving sclerotin in the acetum that concentration is 8～12wt%, obtain eggshell membrane, then eggshell membrane is placed in the ammonia spirit that concentration is 1～3vol% ultrasonic at least 3min, obtain the eggshell membrane alkalized;
Step 2, first carboxylated CNT is scattered in deionized water for ultrasonic at least 30min, obtain finely dispersed carbon nano-tube solution, the eggshell membrane alkalized is placed in ultrasonic at least 3min again in the carbon nano-tube solution that concentration is 400～600g/L, and obtaining area load has the eggshell membrane of CNT;
Step 3, has the eggshell membrane of CNT to be placed in sputter by area load, is sputtering silver 4～18min under 30～50mA in electric current, prepares the CNT-eggshell membrane composite S ERS substrate of modified by silver nanoparticles;
The CNT of described modified by silver nanoparticles-eggshell membrane composite S ERS substrate is by the CNT being carried on eggshell membrane, and modify the silver nano-grain composition on CNT, wherein, the pipe range of CNT is 0.5～2 μm, pipe diameter is 30～50nm, and the particle diameter of silver nano-grain is 5～10nm.
2. the preparation method of the CNT of modified by silver nanoparticles according to claim 1-eggshell membrane composite S ERS substrate, is characterized in that, before being placed in acetum by Ovum crusta Gallus domesticus, being first used for deionized water ultrasonic cleaning twice.
3. the preparation method of the CNT of modified by silver nanoparticles according to claim 1-eggshell membrane composite S ERS substrate, is characterized in that, before to be placed in ammonia spirit by eggshell membrane ultrasonic, being first used for deionized water ultrasonic cleaning.
4. the preparation method of the CNT of modified by silver nanoparticles according to claim 1-eggshell membrane composite S ERS substrate, it is characterized in that, before to be placed in carbon nano-tube solution by the eggshell membrane alkalized ultrasonic, being first used for deionized water ultrasonic cleaning and drying.
5. the preparation method of the CNT of modified by silver nanoparticles according to claim 1-eggshell membrane composite S ERS substrate, is characterized in that when to be placed in by the eggshell membrane alkalized in the carbon nano-tube solution that concentration is 400～600g/L ultrasonic, its every cm2The eggshell membrane alkalized is placed in the carbon nano-tube solution of at least 5mL.
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| CN105482803B (en) * | 2015-11-26 | 2017-10-03 | 东南大学 | A kind of double mode super-resolution imaging probes of fluorescence SERS and preparation method thereof and application method |
| CN105717091B (en) * | 2016-01-29 | 2019-01-18 | 南京理工大学 | A kind of SERS substrate of persistent high efficiency and preparation method thereof |
| CN106568751A (en) * | 2016-11-01 | 2017-04-19 | 广西壮族自治区林业科学研究院 | CNTs-modified 1,4-dioxyanthraquinone doped cellulose-combined porous membrane and preparation method and application thereof |
| CN108341407B (en) * | 2017-01-24 | 2021-06-29 | 北京大学 | Gold nanoparticle modified carbon nanotube and preparation method and application thereof |
| CN107617344B (en) * | 2017-09-01 | 2020-10-16 | 中国科学院宁波材料技术与工程研究所 | Nanowire-loaded polymer microporous membrane and preparation method thereof |
| CN111060488A (en) * | 2019-12-19 | 2020-04-24 | 江汉大学 | Chlorbenzuron detection method |
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