CN1995279A - Surface modified cadmium telluride-containing silica dioxide nano particle and its preparation method - Google Patents
Surface modified cadmium telluride-containing silica dioxide nano particle and its preparation method Download PDFInfo
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- CN1995279A CN1995279A CN 200610125565 CN200610125565A CN1995279A CN 1995279 A CN1995279 A CN 1995279A CN 200610125565 CN200610125565 CN 200610125565 CN 200610125565 A CN200610125565 A CN 200610125565A CN 1995279 A CN1995279 A CN 1995279A
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Abstract
The invention discloses a surface decorative silica nanometer particle with cadmium telluride, which comprises the following steps: adopting quantum point of cadmium telluride as base; utilizing ligand exchange and siloxane hydrolyzing method to obtain the silica/cadmium telluride nanometer particle as core-case structure through one-step reaction; bonding aromatic cup hydrocarbons on the surface of particle through gel-sol method with stable nanometer, optical and high fluorescent strength.
Description
Technical field
The present invention relates to field of nanometer material technology, what particularly relate to finishing includes cadmium telluride silica dioxide nano particle and preparation method thereof.
Background technology
Quantum dot is an II-VI family semiconductor nano, have that fluorescence intensity is big, fluorescence emission peak is narrow and symmetrical, the composition of fluorescence color and size be that controlled, excitation spectrum is continuous bands of a spectrum, is easy to realize that the unit excites good optical properties such as polynary emission to have huge application potential at biomedical sector.In order to improve the stability of quantum dot, require to superscribe one deck inert material on its surface, silicon-dioxide is that a kind of ideal is selected.The method that preparation includes the silica dioxide nano particle (silicon-dioxide/quantum dot) of quantum dot mainly contains two kinds: St ber method (Chem.Mater., 2000,12,2676-2685) and reverse microemulsion process (J.Am.Chem.Soc., 1994,116,6739-6744).St ber method is based on that ligand exchange finishes, but the fluorescence intensity of the silicon-dioxide of gained/cadmium telluride nanoparticle reduced by 20 times (Chem.Mater., 2000,12,2676-2685); The fluorescence intensity of the silicon-dioxide of reverse microemulsion process gained/cadmium telluride nanoparticle also has obvious decline, and quantum yield is not high yet, only is 7% (Adv.Mater., 2005,17,2354).
Calixarene is a kind of oligopolymer of the gained under alkaline condition by p-tert-butylphenol and formaldehyde, the cavity with adjustable size, and upper limb and lower edge are easy to carry out chemically modified.The more important thing is, compared with quantum dot with the Thiovanic acid parcel, water-soluble CdSe/ZnS quantum dot after Calixarene Derivatives is modified have stronger fluorescence intensity and higher quantum yield (0.1-0.34) (J.Am.Chem.Soc.2006,128,9288-9289).Therefore, can be modified at calixarene the surface of the silica dioxide nano particle that contains the cadmium telluride fluorescence quantum, guarantee under the prerequisite of silicon-dioxide/cadmium telluride fluorescence nano grain stability and then improving the fluorescence intensity and the quantum yield of quantum dot.
Summary of the invention
Technical problem to be solved by this invention is: what provide that a kind of calixarene modifies contains silica dioxide nano particle of cadmium telluride quantum dot and preparation method thereof.Simple to operate, the good reproducibility of this method, calixarene on silicon-dioxide/cadmium telluride fluorescence nano grain surface bond improves its fluorescence intensity and quantum yield, can be used for detecting ion and neutral molecule and is expected to realize mark to biomolecules.
The present invention solves its technical problem and adopts following technical scheme:
Finishing provided by the invention include the cadmium telluride silica dioxide nano particle, be to be nuclear with the cadmium telluride quantum dot, coated silica, calixarene successively form the silica dioxide nano particle that includes cadmium telluride quantum dot (calixarene/silicon-dioxide/cadmium telluride nanoparticle) that a kind of calixarene is modified again.
The preparation method who includes the cadmium telluride silica dioxide nano particle of finishing provided by the invention is: based on cadmium telluride quantum dot, utilize ligand exchange and siloxanes method for hydrolysis, single step reaction obtains the silica dioxide nano particle that contains cadmium telluride quantum dot (silicon-dioxide/cadmium telluride nanoparticle) of nucleocapsid structure; By sol-gel process, calixarene on its surface bond can form a kind of calixarene/silicon-dioxide/cadmium telluride nanoparticle again.
Calixarene/silicon-dioxide provided by the invention/cadmium telluride nanoparticle has the following advantages:
(1) stable, good optical property: this nanoparticle characterizes through fluorescence spectrophotometer, ultraviolet-visual spectrometer and transmission electron microscope(TEM) etc.The ultraviolet-visible absorption spectroscopy peak position and the shape of being modified the nanoparticle of front and back by Fig. 2, Fig. 7 and Figure 10 as can be known have no significant change, and illustrate that this nanoparticle has kept the good optical characteristic.By Fig. 1, Fig. 6 and Fig. 9 as can be seen, this nanoparticle has stronger fluorescence intensity, is approximately 2 times of silicon-dioxide/cadmium telluride nanoparticle; Simultaneously, quantum yield reaches about 15%.By Fig. 4 transmission electron microscope(TEM) photo as can be seen, this nanoparticle monodispersity is good, uniform particles.This nanoparticle has satisfactory stability, deposits after two months, and its performance does not change.
(2) this nanoparticle is compared with silicon-dioxide/cadmium telluride nanoparticle, has introduced a large amount of recognition sites, can work in coordination with quantum dot and realize identification and detection to polarity and apolar substance, and may realize its application aspect biological.
The preparation method who includes the cadmium telluride silica dioxide nano particle of finishing provided by the invention has the following advantages:
(1) simple and feasible, the stable process conditions of modifying method, good reproducibility, agents useful for same safety are easy to get, and have just realized the finishing of silicon-dioxide/cadmium telluride nanoparticle by simple sol-gel process.Infrared spectrogram by Fig. 3, Fig. 8 and Figure 11 shows that the calixarene/silicon-dioxide/cadmium telluride nanoparticle that makes by this method still contains the characteristic peak of calixarene: 1485cm
-1(carbon carbon skeleton vibration peak), 870cm
-1Peaks such as (four substituted benzene ring characteristic peaks) illustrates that thus calixarene has been bonded to the surface of silicon-dioxide/cadmium telluride nanoparticle.
(2) present method be by chemical covalent coupling at silicon-dioxide/cadmium telluride nanoparticle surface bond calixarene, quantum dot is further modified, thereby is had better stability.
In sum, this nanoparticle has than better photoluminescent property of its precursor and stability.This nanoparticle surface modification method operability is good simultaneously, and technology is easy, and general chemistry or the Biochemical Lab complete operation of all having ready conditions is for the widespread use of quantum dot provides a very feasible road.
Description of drawings
Fig. 1 is the embodiment of the invention 2 gained cup [4] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain fluorescence spectrum comparison diagram;
Fig. 2 is the embodiment of the invention 2 gained cup [4] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain uv-visible absorption spectra comparison diagram;
Fig. 3 is the embodiment of the invention 2 gained cup [4] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grain infrared spectrogram;
Fig. 4 is the embodiment of the invention 2 gained cup [4] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grain transmission electron microscope(TEM) photo;
Fig. 5 is the embodiment of the invention 2 gained cup [4] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grain transmission electron microscope(TEM) photo;
Fig. 6 is the embodiment of the invention 4 gained cup [6] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain fluorescence spectrum comparison diagram;
Fig. 7 is the embodiment of the invention 4 gained cup [6] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain uv-visible absorption spectra comparison diagram;
Fig. 8 is the embodiment of the invention 4 gained cup [6] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grain infrared spectrogram;
Fig. 9 is the embodiment of the invention 6 gained cup [7] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain fluorescence spectrum comparison diagram;
Figure 10 is the embodiment of the invention 6 gained cup [7] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grains and silicon-dioxide/cadmium telluride fluorescence nano grain uv-visible absorption spectra comparison diagram;
Figure 11 is the embodiment of the invention 6 gained cup [7] aromatic hydrocarbons/silicon-dioxide/cadmium telluride fluorescence nano grain infrared spectrogram;
Figure 12 is preparation technology's schema of calixarene/silicon-dioxide of the present invention/cadmium telluride fluorescence nano grain.
Embodiment
Innovative point of the present invention is at silicon-dioxide/cadmium telluride nanoparticle surface bond calixarene to be arranged.
Calixarene/silicon-dioxide provided by the invention/cadmium telluride nanoparticle, its kernel is a cadmium telluride quantum dot, is coated with silicon oxide successively, calixarene again.Its fluorescent emission center peak position is at 510～650nm, and particle diameter is 30～120nm.
Calixarene/silicon-dioxide provided by the invention/cadmium telluride nanoparticle, its preparation method is: based on cadmium telluride quantum dot, utilize ligand exchange and siloxanes method for hydrolysis, single step reaction obtains silicon-dioxide/cadmium telluride nanoparticle, i.e. the silica dioxide nano particle that contains cadmium telluride quantum dot of nucleocapsid structure; By sol-gel process, calixarene on its surface bond can form a kind of calixarene/silicon-dioxide/cadmium telluride nanoparticle again.Its preparation process comprises the preparation of silicon-dioxide/cadmium telluride nanoparticle, the preparation of calixarene sol-gel and the preparation of calixarene/silicon-dioxide/cadmium telluride nanoparticle.
Preparation method to calixarene/silicon-dioxide/cadmium telluride nanoparticle is described further below in conjunction with specific embodiment, but does not limit the present invention.
(1) getting 2～5mL concentration is 2 * 10
-3～10
-5The mol/L cadmium telluride quantum dot adds 1～2mL methyl alcohol while stirring, adds 1～3 μ L mercaptopropyl trimethoxysilane after 5～30 minutes, continues under the room temperature to stir 15～40 minutes, promptly makes silicon-dioxide/cadmium telluride nanoparticle, and the dilution back is stand-by.
(2) get cup [4] aromatic hydrocarbons of 1～10mg, the methylene dichloride dissolving that adds 100～250 μ L, γ-[(2, the 3)-epoxy third oxygen] propyl trimethoxy silicane that adds 50 μ L adds the trifluoroacetic acid of 50 μ L, ultrasonic 1～3 minute, the tetraethoxysilane that adds 100～150 μ L again, ultrasonic 3～10 minutes, under 8000～12000r/min centrifugal 5～10 minutes then, promptly make cup [4] aromatic hydrocarbons colloidal sol, it is stand-by to take out supernatant liquid.
(3) get 2～5mL silicon-dioxide/cadmium telluride nanoparticle solution, add 2～25 μ L cup [4] aromatic hydrocarbons colloidal sols while stirring, continue to stir 20～30 minutes, and made cup [4] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.
Embodiment 2
(1) getting 5ml concentration is 10
-3The quantum dot of mol/L adds 2mL methyl alcohol while stirring, adds 1 μ L mercaptopropyl trimethoxysilane after 20 minutes, continues to stir 20 minutes, makes silicon-dioxide/cadmium telluride nanoparticle, and redilution is to 25mL.
(2) get 2mg cup [4] aromatic hydrocarbons, the methylene dichloride dissolving that adds 200 μ l, γ-[(2, the 3)-epoxy third oxygen] propyl trimethoxy silicane that adds 50 μ l adds the trifluoroacetic acid of 38 μ l, ultrasonic 1 minute, the tetraethoxysilane that adds 100 μ l again, ultrasonic 3 minutes, under 10000r/min centrifugal 8 minutes then, promptly make cup [4] aromatic hydrocarbons colloidal sol, stand-by.
(3) get silicon-dioxide in the step (1)/cadmium telluride nanoparticle solution 2.5ml, add 15 μ l cup [4] aromatic hydrocarbons colloidal sols while stirring, continue to stir 30 minutes, and made cup [4] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.See Fig. 1, its fluorescent emission center peak position is at 517nm.
Embodiment 3
(1) getting 2～5mL concentration is 2 * 10
-3～10
-5The quantum dot of mol/L adds 1～2mL methyl alcohol while stirring, adds 1～3 μ L mercaptopropyl trimethoxysilane after 5～30 minutes, continues under the room temperature to stir 15～40 minutes, and the dilution back is stand-by.
(2) get cup [6] aromatic hydrocarbons of 1～10mg, the methylene dichloride dissolving that adds 100～250 μ L, γ-[(2, the 3)-epoxy third oxygen] propyl trimethoxy silicane that adds 50 μ L adds the trifluoroacetic acid of 50 μ L, ultrasonic 1～3 minute, the tetraethoxysilane that adds 100～150 μ L again, ultrasonic 3～10 minutes, under 8000～12000r/min centrifugal 5～10 minutes then, promptly make cup [6] aromatic hydrocarbons colloidal sol, stand-by.
(3) get 2～5mL silicon-dioxide/cadmium telluride nanoparticle, add 2～20 μ L cup [6] aromatic hydrocarbons colloidal sols while stirring, continue to stir 30 minutes, and made cup [6] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.
Embodiment 4
(1) getting 5ml concentration is 10
-3The quantum dot of mol/L adds 2mL methyl alcohol while stirring, adds 1 μ L mercaptopropyl trimethoxysilane after 20 minutes, continues to stir 20 minutes, makes silicon-dioxide/cadmium telluride nanoparticle, and redilution is to 25mL.
(2) get 2mg cup [6] aromatic hydrocarbons, the methylene dichloride dissolving that adds 200 μ l, the γ-[(2 that adds 50 μ l, 3)-and epoxy third oxygen] propyl trimethoxy silicane, the trifluoroacetic acid that adds 38 μ l ultrasonic 1 minute, adds the tetraethoxysilane of 100 μ l again, ultrasonic 3 minutes, under 10000r/min centrifugal 8 minutes then.Promptly make cup [6] colloidal sol, stand-by.
(3) get silicon-dioxide in the step (1)/cadmium telluride nanoparticle solution 2.5ml, add 8 μ l cup [6] aromatic hydrocarbons colloidal sols while stirring, continue to stir 30 minutes, and made cup [6] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.See Fig. 6, its fluorescent emission center peak position is at 560nm.
Embodiment 5
(1) getting 2～5mL concentration is 2 * 10
-3～10
-5The quantum dot of mol/L adds 1～2mL methyl alcohol while stirring, adds 1～3 μ L mercaptopropyl trimethoxysilane after 5～30 minutes, continues under the room temperature to stir 15～40 minutes, and the dilution back is stand-by.
(2) get cup [7] aromatic hydrocarbons of 1～10mg, the methylene dichloride dissolving that adds 100～250 μ L, γ-[(2, the 3)-epoxy third oxygen] propyl trimethoxy silicane that adds 50 μ L adds the trifluoroacetic acid of 50 μ L, ultrasonic 1～3 minute, the tetraethoxysilane that adds 100～150 μ L again, ultrasonic 3～10 minutes, under 8000～12000r/min centrifugal 5～10 minutes then, promptly make cup [7] aromatic hydrocarbons colloidal sol, stand-by.
(3) get 2～5mL silicon-dioxide/cadmium telluride nanoparticle, add 2～20 μ L cup [7] aromatic hydrocarbons colloidal sols while stirring, continue to stir 30 minutes, and made cup [7] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.
Embodiment 6
(1) getting 5ml concentration is 10
-3The quantum dot of mol/L adds 2mL methyl alcohol while stirring, adds 1 μ L mercaptopropyl trimethoxysilane after 20 minutes, continues to stir 20 minutes, makes silicon-dioxide/cadmium telluride nanoparticle, and redilution is to 25mL.
(2) get 2mg cup [7] aromatic hydrocarbons, the methylene dichloride dissolving that adds 200 μ l, the γ-[(2 that adds 50 μ l, 3)-and epoxy third oxygen] propyl trimethoxy silicane, the trifluoroacetic acid that adds 38 μ l ultrasonic 1 minute, adds the tetraethoxysilane of 100 μ l again, ultrasonic 3 minutes, under 10000r/min centrifugal 8 minutes then.Promptly make cup [7] colloidal sol, stand-by.
(3) get silicon-dioxide in the step (1)/cadmium telluride nanoparticle solution 2.5ml, add 5 μ l cup [7] aromatic hydrocarbons colloidal sols while stirring, continue to stir 30 minutes, and made cup [7] aromatic hydrocarbons colloidal sol be bonded in the silicon-dioxide laminar surface, and wherein methylene dichloride is volatilized fully get final product by chemical covalent coupling.See Fig. 9, its fluorescent emission center peak position is at 570nm.
According to method provided by the invention, other calixarene or derivatives thereof can be modified at the surface of silicon-dioxide/cadmium telluride nanoparticle, and also can obtain similar fluorescence nano grain.
Claims (5)
1. a finishing includes the cadmium telluride silica dioxide nano particle, it is characterized in that being is nuclear with the cadmium telluride quantum dot, coated silica, calixarene successively again, form a kind of calixarene/silicon-dioxide/cadmium telluride nanoparticle, i.e. the silica dioxide nano particle that includes cadmium telluride quantum dot of calixarene modification.
Finishing according to claim 1 include the cadmium telluride silica dioxide nano particle, it is characterized in that described calixarene/silicon-dioxide/cadmium telluride nanoparticle, its fluorescent emission center peak position is at 510～650nm, particle diameter is 30～120nm.
3. the preparation method who includes the cadmium telluride silica dioxide nano particle of a finishing, it is characterized in that: based on cadmium telluride quantum dot, utilize ligand exchange and siloxanes method for hydrolysis, single step reaction obtains silicon-dioxide/cadmium telluride nanoparticle, i.e. the silica dioxide nano particle that contains cadmium telluride quantum dot of nucleocapsid structure; By sol-gel process, calixarene on its surface bond can form a kind of calixarene/silicon-dioxide/cadmium telluride nanoparticle again.
4. the preparation method who includes the cadmium telluride silica dioxide nano particle of finishing according to claim 3 is characterized in that described calixarene/silicon-dioxide/cadmium telluride nanoparticle, and its preparation method may further comprise the steps:
(1) preparation of silicon-dioxide/cadmium telluride nanoparticle:
Getting 5mL concentration is 2 * 10
-3～10
-5The cadmium telluride quantum dot of mol/L adds 1～2mL methyl alcohol while stirring, adds mercaptopropyl trimethoxysilane after 5～30 minutes, continues under the room temperature to stir 15～40 minutes, and the dilution back is stand-by,
(2) preparation of calixarene sol-gel:
Get 1～10mg calixarene, add the dissolving of 100～250 μ L methylene dichloride, add γ-[(2 again, 3)-and epoxy third oxygen] propyl trimethoxy silicane and trifluoroacetic acid, add tetraethoxysilane after ultrasonic 1～3 minute, ultrasonic again 3～10 minutes, under 8000～12000r/min centrifugal 5～10 minutes then, promptly make calixarene colloidal sol, it is stand-by to take out supernatant liquid
(3) preparation of calixarene/silicon-dioxide/cadmium telluride nanoparticle:
Get silicon-dioxide/cadmium telluride nanoparticle solution that step (1) makes, add 2～25 μ L calixarene colloidal sols while stirring, continue to stir 20～30 minutes, make calixarene colloidal sol be bonded in the silicon-dioxide laminar surface, and methylene dichloride is wherein volatilized fully, promptly make calixarene/silicon-dioxide/cadmium telluride nanoparticle.
5. the preparation method who includes the cadmium telluride silica dioxide nano particle of finishing according to claim 3, it is characterized in that calixarene is: 5,11,17,23-four-tertiary butyl-25,27-oxyethyl group-26,28-dihydroxyl cup [4] aromatic hydrocarbons, or to tertiary butyl cup [6] aromatic hydrocarbons, or to tertiary butyl cup [7] aromatic hydrocarbons, or to tertiary butyl cup [n] aromatic hydrocarbons parent aromatic hydrocarbons and derivative thereof, n=4,6,7 or 8.
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