CN102095711A - Double colour fluorescent chemical sensor used for visually detecting explosive and manufacturing method thereof - Google Patents
Double colour fluorescent chemical sensor used for visually detecting explosive and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a double colour fluorescent chemical sensor used for visually detecting explosive, in particular to a paper-based or membrane-based sensor comprising a filter paper or glass slide substrate and double colour quantum dot superstructure silicon oxide nano particles uniformly distributed on the substrate. The method for manufacturing the sensor comprises the following steps of: firstly embedding red or green quantum dots into silicon oxide nano particles, aminating the surface of silicon oxide, then carrying out covalence coupling and coating a green or red quantum dot sensitive layer to obtain the double colour quantum dot superstructure silicon oxide nano particles, and finally processing to obtain the fluorescent chemical sensor. By applying the sensor, explosive residue with the trace of 5nanogram/mm<2> can be visually and rapidly detected online in real time. The fluorescence intensity of outer quantum dots is 2-10 times that of inner quantum dots.
Description
One, technical field
The present invention relates to a kind of fluorescence chemical sensor and preparation method thereof, the visual analyzing that is particularly related to a kind of trace explosive detects fluorescence chemical sensor and preparation method thereof, sensor of the visual detection of the two emitting fluorescence signals of specifically a kind of color quantum point TNT explosive and preparation method thereof.
Two, background technology
The frequent in recent years terrorist incident that occurs is threatening the people's lives and property safety constantly, has had a strong impact on social harmony with stable.These terrorist incidents normally utilize explosive to carry out the attack of terrorism, will prevent that therefore similar incidents from taking place, and must carry out narrow examination and detection to explosive.On the other hand, survey and to spread all over not detonating a mine all over the world, eliminate safe hidden trouble and also will place hope on the raising of explosive detection method fundamentally.Current common method has: imaging technique, nuclear technology, ion mobility spectrometry method, electrochemical analysis method, chemical-biological sensing method, optical analysis method etc.These methods need that large scientific instrument is auxiliary, the data acquisition and processing (DAP) process of very complicated, detect the cost height, and the technician that need be subjected to special training, limited greatly in real time on-the-spot detect and daily life in application.
People (Angew.Chem.Int.Ed.2008,47:8601～8604.) such as Beijing chemistry hair orchid group of institute of the Chinese Academy of Sciences have been developed a kind of simple visual explosive detection method.2,4,6-trinitro-toluene (TNT) can make amido modified golden nanometer particle assemble, and produces by the change color of claret to blueness, can optionally detect the TNT of trace.But the instability of solution of gold nanoparticles self has limited the realization of this visual approach greatly.People (J.Am.Chem.Soc.2009,131:1390～1391.) such as department of chemistry, tsinghua university, Li Jing rainbow have reported a kind of platform of novel colorimetric detection nitryl aromatic class explosive.Because change color is corresponding with the explosive decomposition product complicated, still needs complicated data handling procedure, and needs optical imaging device.The realization of the visual detection of real-time online still faces very big challenge.
The semi-conductor nano particles that quantum dot mainly is made up of II-VI family element or III-V family element.As a kind of fluorescence probe with potential using value, to compare with traditional organic fluorescent dye, the photoluminescent property of quantum dot is very superior: excite wide ranges, emission peak is narrow and symmetrical, and Stokes shift is big, the quantum yield height, brightness is strong, the light stability height.Particularly the quantum dot of different colours can be excited simultaneously by the light source of single wavelength, and this characteristic can be used to design visual fluorescence chemical sensor.At present, quantum dot yet there are no report in the visual context of detection of explosive.
Three, summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, the quick visualization that aims to provide a kind of real-time scene detects the fluorescence chemical sensor of trace explosive, and technical matters to be solved utilizes the photoluminescent property design of color quantum point to realize the method for visual explosive detection.
The character that the present invention utilizes the quantum dot of different colours to be excited simultaneously by the light source of single wavelength designs the sensor of visual detection TNT, develops a kind of novel two emissive quantum dots fluorescence chemical sensors and preparation method thereof.
Two emitting fluorescence chemical sensors that the present invention is alleged, be to be substrate with filter paper or microslide, by substrate be evenly distributed on filter paper base or the film based sensor that suprabasil pair of color development quantum dot superstructure silicon oxide nanoparticle formed, the described pair of color development quantum dot superstructure silicon oxide nanoparticle be by silicon oxide nanoparticle in it behind red or green quantum dot of embedding, its surface amination covalent coupling coat green or the formed superstructure silicon oxide nanoparticle of red quantum dot sensitive layer.
Described redness or green quantum dot are meant at quantum dot can launch redness or green fluorescence when single wavelength light source excites simultaneously.
Described quantum dot is selected from any transmitting green of carboxyl-functionals such as CdTe, CdTe/CdS, CdSe, CdSe/ZnS, CdSe/CdS or CdS or the quantum dot of red fluorescence.
The preparation method of this sensor at first is embedded in redness or green quantum dot in the silicon oxide nanoparticle, after the silicon oxide surface amination, covalent coupling coats green or red quantum dot sensitive layer again, obtain the two color development quantum dot superstructure silicon oxide nanoparticles of a class, be processed into fluorescence chemical sensor at last.Such sensor is can visual detection trace explosive residual.
Technical scheme of the present invention comprises the structure of silicon oxide nanoparticle surface-sensitive quantum dot layer of silicon oxide nanoparticle, embedded quantum dots of the luminous stable embedded quantum dots of preparation and the visual sensing of fixing two color development quantum dot superstructure silicon oxide nanoparticles, the silicon oxide nanoparticle of the luminous stable embedded quantum dots of described preparation is embedded in quantum dot in the silicon oxide nanoparticle exactly, forms the silicon oxide layer of transparent passivation on quantum dot.Because quantum dot is embedded in the middle of the monox, its photoluminescent property is not subjected to the interference of foreign matter substantially.Make up the quantum dot layer to the explosive sensitivity then on the silicon oxide particle surface of embedded quantum dots, inside is interference-free because outer field quantum dot is relatively more responsive, thus colorific orderly variation; The visual sensing of described fixing two color development quantum dot superstructure silicon oxide nanoparticles, two color development quantum dot superstructure silicon oxide nanoparticle sensors that will obtain exactly are fixed in filter paper or the polymeric material, make test paper or drying and forming-film, be convenient to the visual explosive detection of on-the-spot real-time online.
The concrete operations step is as follows:
1, the silicon oxide nanoparticle of the luminous stable embedded quantum dots of preparation
Synthetic glow (or green glow) quantum dot stoste, ultrapure water, ammoniacal liquor and 3-mercaptopropyl trimethoxysilane (MPS) are mixed in the container, stirred 4-24 hour, modify quantum dot earlier, add positive tetraethyl orthosilicate (TEOS) then, then stir and add 3-aminopropyl triethoxysilane (APTS) after 4-24 hour again, continue to mix liquid.The silicon oxide nanoparticle centrifuge washing of the embedded quantum dots that finally obtains is scattered in the ultrapure water for several times more again, and is standby.
2, the structure of the silicon oxide nanoparticle surface-sensitive quantum dot layer of embedded quantum dots
The silicon oxide nanoparticle of getting embedded quantum dots is in the 10mL ultrapure water, the quantum dot solution that adds green light (or ruddiness), under the effect of condensation agent 1-(3-dimethyl aminopropyl)-3-ethyl carbon diamines/N-maloyl imines (EDC/NHS), stirred 0.5～5 hour, successfully make up the responsive quantum dot layer on embedded quantum dots silicon oxide nanoparticle surface.Mixed liquor is centrifugal, abandoning supernatant, and the two color development quantum dot superstructure silicon oxide nanoparticles that obtain are scattered in the ultrapure water again, and are standby.
3, the visual sensing of fixing two color development quantum dot superstructure silicon oxide nanoparticles
The two color development quantum dot superstructure silicon oxide nanoparticles that obtain are scattered in the ultrapure water, get filter paper and immerse in the mixed liquor.Ultrasonic some time is taken out filter paper after disperseing, and drying obtains the visual sensor of test paper base; The two color development quantum dot superstructure silicon oxide nanoparticles that obtain are scattered in the high molecular polymer aqueous solution, and drying and forming-film in the substrates such as dropping in microslide of taking a sample obtains the visual sensor of film base.The test paper or the film that obtain are stored in the darkroom.
Described high molecular polymer is selected from one or both polymkeric substance to mix in polyvinyl alcohol (PVA), polyglycol, polyvinylpyrrolidone, polyacrylic acid, polymethyl or the gum arabic etc.
Advantage of the present invention and good effect:
The present invention utilizes the quantum dot of different colours to be designed visual fluorescence chemical sensor by the light source of single wavelength while excited fluorescent characteristic first.Specifically invented sensor of the visual detection of the two emitting fluorescence signals of class color quantum point TNT explosive and preparation method thereof.The sensor of preparation can be designed to the test paper or the film that are easy to carry and operate, is convenient to the visual explosive detection of on-the-spot real-time online.The test paper sensor that obtains successfully is used for the TNT trace residue on the visual detection material object, and the trace TNT that can visually detect every square millimeter of 5 nanogram is residual.The outer quantum dot fluorescence intensity of monox is inner 2～10 times.Excitation wavelength is at 365nm.
The inventive method can avoid using large-scale instrument to a certain extent, only needs a hand-held uviol lamp just can carry out visual detection, and simple to operate, fast convenient, highly sensitive, effect is remarkable; This method can effectively be avoided the interference of other impurity in the sample, so selectivity is good, has also omitted preprocessing process.The two emitting fluorescence chemical sensors of the color quantum point of preparation can the visual explosive detection of on-the-spot real-time online.
Four, description of drawings
Fig. 1 is two color development quantum dot superstructure silicon oxide nanoparticle shape appearance figures.
Fig. 2 is two color development quantum dot superstructure silicon oxide nanoparticles (c) and red (b), green (a) quantum dot fluorescence figure.
Fig. 3 is the visual photo of TNT explosive detection in the waste water.
Fig. 4 is the visual photo of TNT explosive detection.
Fig. 5 is the visual photo of the portable detection trace of test paper base TNT.
Five, embodiment
Now be described below for the example non-limiting examples with the cadmium telluride quantum dot:
Embodiment 1
1, the silicon oxide nanoparticle of the luminous stable embedded quantum dots of preparation
With 0.2284g caddy (CdCl
22.5H
2O) join in the ultrapure water of 250mL deoxygenation, add the 0.21mL mercaptopropionic acid subsequently, with 1M NaOH solution its pH value is transferred to 11.2 again, form the solution that contains sulfhydryl compound and cadmium ion.On the other hand, get 0.0319g tellurium powder and 0.05g sodium borohydride in the 2mL ultrapure water, under nitrogen protection, ice bath reacts more than 8 hours.The 5mL0.5M dilution heat of sulfuric acid is injected in the sodium hydrogen telluride solution of generation.With the H that generates
2Te all feeds in the above-mentioned cadmium-ion solution, stirs after 20 minutes reflux.The control return time, can obtain mercaptopropionic acid stable, the fluorescent emission peak position is in the cadmium telluride quantum dot aqueous solution of 490～680nm.The quantum dot original solution that makes shines 15 days to improve fluorescence quantum yield under the uviol lamp of 15W, standby.
Get red quantum dot (emission peak is at 630nm) solution 20mL, add dilution of 20mL ultrapure water and 1mL ammoniacal liquor, add 80mL ethanol again, under agitation add 0.05mL MPS, after stirring 12h, add positive tetraethyl orthosilicate 2mL, then stir 12h after, add 3-aminopropyl triethoxysilane 0.1mL again, continue to mix liquid 12h.The silicon oxide nanoparticle centrifuge washing of the embedded quantum dots that finally obtains is scattered in the ultrapure water for several times more again, and is standby.
2, the structure of the silicon oxide nanoparticle surface-sensitive quantum dot layer of embedded quantum dots
The silicon oxide nanoparticle of getting embedded quantum dots is in the 10mL ultrapure water, quantum dot (emission peak is at the 520nm) solution that adds green light, stirred for several hour under the effect of condensation agent EDC/NHS successfully makes up the responsive quantum dot layer (pattern is seen accompanying drawing 1) on embedded quantum dots silicon oxide nanoparticle surface.Mixed liquor is centrifugal, abandoning supernatant, and the two color development quantum dot superstructure silicon oxide nanoparticle sensors that obtain are scattered in (fluorescence spectrum is seen accompanying drawing 2) in the ultrapure water again, and are standby.
3, trace TNT in the visual detection waste water of two color development quantum dot superstructure silicon oxide nanoparticle sensors
TNT solution to be detected joins in two color development quantum dot superstructure silicon oxide nanoparticle solution and carries out the fluorescent visual detection.At 2ppb content response is just arranged, detect very sensitive.Along with the amount of TNT strengthens gradually, fluorescence color changes to redness at last by yellow green flavescence look gradually.Can see the stepped change of color this moment under uviol lamp, realize visual detection.Visual photo is seen accompanying drawing 3.
Embodiment 2
1, the silicon oxide nanoparticle of the luminous stable embedded quantum dots of preparation
With 0.2284g caddy (CdCl
22.5H
2O) join in the ultrapure water of 250mL deoxygenation, add the 0.21mL mercaptopropionic acid subsequently, with 1M NaOH solution its pH value is transferred to 11.2 again, form the solution that contains sulfhydryl compound and cadmium ion.On the other hand, get 0.0319g tellurium powder and 0.05g sodium borohydride in the 2mL ultrapure water, under nitrogen protection, ice bath reacts more than 8 hours.5mL 0.5M dilution heat of sulfuric acid is injected in the sodium hydrogen telluride solution of generation.With the H that generates
2Te all feeds in the above-mentioned cadmium-ion solution, stirs after 20 minutes reflux.The control return time, can obtain mercaptopropionic acid stable, the fluorescent emission peak position is in the cadmium telluride quantum dot aqueous solution of 490～680nm.The quantum dot original solution that makes shines 15 days to improve fluorescence quantum yield under the uviol lamp of 15W, standby.
Get green light quantum dot (emission peak is at 540nm) solution 10mL, add dilution of 10mL ultrapure water and 1mL ammoniacal liquor, add 40mL ethanol again, under agitation add 0.1mL MPS, after stirring 24h, add positive tetraethyl orthosilicate 2mL, then stir 12h after, add positive tetraethyl orthosilicate of 0.5mL and 0.1mL 3-aminopropyl triethoxysilane again, continue to mix liquid 12h.The silicon oxide nanoparticle centrifuge washing of the embedded quantum dots that finally obtains is scattered in the ultrapure water for several times more again, and is standby.
2, the structure of the silicon oxide nanoparticle surface-sensitive quantum dot layer of embedded quantum dots
The silicon oxide nanoparticle of getting embedded quantum dots is in the 10mL ultrapure water, add quantum dot (emission peak is at the 610nm) solution that glows, stirred for several hour under the effect of condensation agent EDC/NHS successfully makes up the responsive quantum dot layer (pattern is seen accompanying drawing 1) on embedded quantum dots silicon oxide nanoparticle surface.Mixed liquor is centrifugal, abandoning supernatant, and the two color development quantum dot superstructure silicon oxide nanoparticle sensors that obtain are scattered in the ultrapure water again, and are standby.
3, trace TNT in the visual detection waste water of two color development quantum dot superstructure silicon oxide nanoparticle sensors
TNT solution to be detected joins in two color development quantum dot superstructure silicon oxide nanoparticle solution and carries out the fluorescent visual detection.At 2ppb content response is just arranged, detect very sensitive.Along with the amount of TNT strengthens gradually, fluorescence color changes to green at last by redness flavescence look gradually.Can see the stepped change of color this moment under uviol lamp, realize visual detection.Visual photo is seen accompanying drawing 4.
Embodiment 3
1, the silicon oxide nanoparticle of the luminous stable embedded quantum dots of preparation
With 0.2284g caddy (CdCl
22.5H
2O) join in the ultrapure water of 250mL deoxygenation, add the 0.21mL mercaptopropionic acid subsequently, with 1M NaOH solution its pH value is transferred to 11.2 again, form the solution that contains sulfhydryl compound and cadmium ion.On the other hand, get 0.0319g tellurium powder and 0.05g sodium borohydride in the 2mL ultrapure water, under nitrogen protection, ice bath reacts more than 8 hours.The 5mL0.5M dilution heat of sulfuric acid is injected in the sodium hydrogen telluride solution of generation.With the H that generates
2Te all feeds in the above-mentioned cadmium-ion solution, stirs after 20 minutes reflux.The control return time, can obtain mercaptopropionic acid stable, the fluorescent emission peak position is in the cadmium telluride quantum dot aqueous solution of 490～680nm.The quantum dot original solution that makes shines 15 days to improve fluorescence quantum yield under the uviol lamp of 15W, standby.
Get red quantum dot (emission peak is at 650nm) solution 10mL, add dilution of 10mL ultrapure water and 1mL ammoniacal liquor, add 60mL ethanol again, under agitation add 0.04mL MPS, after stirring 24h, add positive tetraethyl orthosilicate 2mL, then stir 12h after, add 3-aminopropyl triethoxysilane 0.1mL again, continue to mix liquid 6h.The silicon oxide nanoparticle centrifuge washing of the embedded quantum dots that finally obtains is scattered in the ultrapure water for several times more again, and is standby.
2, the structure of the silicon oxide nanoparticle surface-sensitive quantum dot layer of embedded quantum dots
The silicon oxide nanoparticle of getting embedded quantum dots is in the 10mL ultrapure water, quantum dot (emission peak is at the 510nm) solution that adds green light, stirred for several hour under the effect of condensation agent EDC/NHS successfully makes up the responsive quantum dot layer (pattern is seen accompanying drawing 1) on embedded quantum dots silicon oxide nanoparticle surface.Mixed liquor is centrifugal, abandoning supernatant, and the two color development quantum dot superstructure silicon oxide nanoparticle sensors that obtain are scattered in (fluorescence spectrum is seen accompanying drawing 2) in the ultrapure water again, and are standby.
3, the visual detection trace of two color development quantum dot superstructure silicon oxide nanoparticle sensor test paper TNT
TNT solution to be detected joins on the test paper that contains two color development quantum dot superstructure silicon oxide nanoparticles and carries out the fluorescent visual detection.At every square millimeter of content of 5 nanograms response is just arranged, detect very sensitive.Realize visual detection.Visual photo is seen accompanying drawing 5.
Claims (4)
1. two emitting fluorescence chemical sensors of a visual explosive detection, it is characterized in that: this sensor is equally distributed pair of paper substrate or film based sensor that color development quantum dot superstructure silicon oxide nanoparticle is formed in substrate and the substrate by filter paper or microslide, the described pair of color development quantum dot superstructure silicon oxide nanoparticle be by silicon oxide nanoparticle in it behind red or green quantum dot of embedding, its surface amination covalent coupling coat superstructure silicon oxide nanoparticle green or that red quantum dot sensitive layer is constituted.
2. sensor according to claim 1 is characterized in that: described quantum dot is selected from any transmitting green of CdTe, CdTe/CdS, CdSe, CdSe/ZnS, CdSe/CdS or CdS carboxyl-functional and the quantum dot of red fluorescence.
3. the preparation method of two emitting fluorescence chemical sensors of visual explosive detection as claimed in claim 1, its feature may further comprise the steps:
1) silicon oxide nanoparticle of the luminous stable embedded quantum dots of preparation:
Glow or green light quantum point stoste, ultrapure water, ammoniacal liquor and 3-mercaptopropyl trimethoxysilane are mixed in the container synthetic, stir after 4-24 hour, add positive tetraethyl orthosilicate, then stir after 4-24 hour and add the 3-aminopropyl triethoxysilane again, continue to mix liquid, the silicon oxide nanoparticle centrifuge washing of the embedded quantum dots that obtains is scattered in the ultrapure water for several times more again, and is standby;
2) structure of the silicon oxide nanoparticle surface-sensitive quantum dot layer of embedded quantum dots:
The silicon oxide nanoparticle of getting embedded quantum dots is in the 10mL ultrapure water, the quantum dot solution that adds green light or ruddiness, under the effect of condensation agent 1-(3-dimethyl aminopropyl)-3-ethyl carbon diamines/N-maloyl imines, stirred 0.5～5 hour, success makes up the responsive quantum dot layer on embedded quantum dots silicon oxide nanoparticle surface, mixed liquor is centrifugal, abandoning supernatant, the two color development quantum dot superstructure silicon oxide nanoparticles that obtain are scattered in the ultrapure water again, and are standby;
3) the visual sensing of fixing two color development quantum dot superstructure silicon oxide nanoparticles:
The two color development quantum dot superstructure silicon oxide nanoparticles that obtain are scattered in the ultrapure water, get filter paper and immerse in the mixed liquor.After the ultrasonic dispersion, take out filter paper, drying obtains the visual sensor of test paper base; Two color development quantum dot superstructure silicon oxide nanoparticles that perhaps will obtain are scattered in the high molecular polymer aqueous solution, and drying and forming-film obtains the visual sensor of film base in the substrates such as dropping in microslide of taking a sample.
4. method according to claim 3, it is characterized in that in the step 3) that described high molecular polymer is selected from the polymkeric substance of one or more mixing in polyvinyl alcohol (PVA), polyglycol, polyvinylpyrrolidone, polyacrylic acid, polymethylacrylic acid or the gum arabic.
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