CN1579994A - Method for preparing monodisperse cadium sulfide-silicon dioxide nucleo capsid structure - Google Patents

Method for preparing monodisperse cadium sulfide-silicon dioxide nucleo capsid structure Download PDF

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CN1579994A
CN1579994A CNA2004100185894A CN200410018589A CN1579994A CN 1579994 A CN1579994 A CN 1579994A CN A2004100185894 A CNA2004100185894 A CN A2004100185894A CN 200410018589 A CN200410018589 A CN 200410018589A CN 1579994 A CN1579994 A CN 1579994A
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nucleocapsid structure
monodisperse
silicon dioxide
construction
deionized water
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CN1258823C (en
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杨德仁
谢荣国
李东升
蒋民华
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses an approach to produce monodisperse cadmium sulphide-silicon dioxide nucleocapsid construction. Adopting chemistry water bath sedimentation, it includes nether steps: 1): Use sonic oscillation to make even monodisperse silicon dioxide sphere disperse into solution of deionized water; add sodium citrate as complexing agent, alkylol amine as surface active agent; use ammonia to adjust PH value to 8-13; magnetic stirring in constant temperature of 50-90deg.C; add cadmium chloride and sulfur to react for 1-3 hours; and then get nucleocapsid construction suspending liquid of cadmium sulphide enwrapping silicon dioxide sphere. 2): Use deionized water and absolute ethyl alcohol to clean circularly; remove reaction remnants and drying. The invention has a low cost and simple process. The produced nucleocapsid construction has a averaging diameter without cadmium sulphide grains and heterocoagulation. It can be used as construction primitive to produce three-dimensional photon crystal with unique band gap performance.

Description

The method for preparing monodisperse CdS-silicon dixoide nucleocapsid structure
Technical field
The present invention relates to prepare the method for Cadmium Sulfide-silicon dixoide nucleocapsid structure.
Background technology
Nucleocapsid structure is because its particular structure, optics and surface properties are coating, electronics recently, and fields such as photonics, medicine transmission, catalysis have obtained using widely.Photonic crystal is the artificial microstructure that can be compared with optical wavelength by its cycle that the material with differing dielectric constant (specific refractory power) is arranged according to certain spacial ordering.As " optical semiconductor ", photonic crystal has the function of unique adjusting light spread state, and, fields such as photon integrated, optical communication integrated at photoelectricity have boundless application prospect.The three-D photon crystal that is obtained by the nucleocapsid structure self-assembly has also obtained investigator's extensive interest in recent years.Because nuclear is different with the specific refractory power of shell material, can regulate the position of photon band gap by the size that changes nuclear and shell.Theoretical Calculation show by nucleocapsid structure form the photon band gap characteristic of photonic crystal be different from the photonic crystal that obtains by the self-assembly of homogeneous ball.
Cadmium Sulfide (CdS) is that a kind of very important II-VI family has direct wide bandgap semiconductor materials, is widely used in electronics, optoelectronic areas.Because this material has high relatively specific refractory power, absorb superior optical properties such as less at visible region, also be widely used in the photonic material field in recent years.The nucleocapsid structure relevant with Cadmium Sulfide, existing investigator prepares as nucleocapsid structures such as Cadmium Sulfide-polystyrene spheres, Cadmium Sulfide-Cadmium telluride fine powders.Have the people to prepare the composite structure that Cadmium Sulfide is coated on the silica spheres surface by the unit molecule presoma recently, but the composite structure that this method obtains is not single dispersion, occurs the impurity cohesion easily, and the surface coating is inhomogeneous, the thickness of shell wall is uncontrollable.
Summary of the invention
The objective of the invention is in order to obtain Cadmium Sulfide by high refractive index is that the silica spheres of shell and low-refraction is single distributed nuclei shell structure that nuclear is formed, provide a kind of cheap efficient, simple preparation coats evenly, the method for the monodisperse CdS-silicon dixoide nucleocapsid structure of controllable thickness.
The method for preparing monodisperse CdS-silicon dixoide nucleocapsid structure of the present invention, employing be chemical bath deposition, may further comprise the steps:
1) the uniform monodisperse silica sphere particle of particle diameter is dispersed in the deionized water solution with sonic oscillation, adding concentration is that the Trisodium Citrate of 0.01~0.5 mol is done network and agent, hydramine is a tensio-active agent, and regulate pH value to 8~13 with ammoniacal liquor, 50 ℃~90 ℃ constant temperature magnetic agitation, add Cadmium chloride fine powder and sulphur urine then, the concentration that makes Cadmium chloride fine powder in the solution is 0.001 mol~0.01 mol, the concentration of sulphur urine is 0.002 mol~0.02 mol, reacted 1~3 hour, and obtained the nucleocapsid structure suspension of Cadmium Sulfide parcel silica spheres;
2) add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol centrifugal deposition, remove reaction residue, oven dry obtains the monodisperse CdS hollow ball.
Monodisperse silica sphere particle can be commercially available or by " Si Tuobu (St ber) method " preparation, particle diameter is that 10nm is to 1000nm among the present invention.Said particle diameter is meant that evenly relative standard deviation is less than 10%.Said hydramine can be the trolamine or the diethanolamine of commercially available acquisition.
The inventive method can be regulated the radius of the nuclear of nucleocapsid structure by changing the particle diameter of silica spheres; Change the amount of Trisodium Citrate and hydramine adding and the speed that concentration is regulated Cadmium Sulfide coated silica core; Change the concentration of Cadmium chloride fine powder and sulphur urine, can regulate the thickness of shell.
Method of the present invention is nuclear with the monodisperse silica sphere particle, and silica spheres is compared with other materials and can high temperature heat-resistant be handled, and has more stability.By adding hydramine, down auxiliary at hydramine, chemical bath deposition in the alkaline aqueous solution obtains wrapping up the nucleocapsid structure of even no unnecessary Cadmium Sulfide particle and impurity cohesion, and method is with low cost, the process simple controllable.Monodisperse CdS-silicon dixoide nucleocapsid structure that the present invention makes can be used as structural motif, self-assembly prepares three-D photon crystal, absorb advantages such as few owing to the high refractive index of Cadmium Sulfide with at visible region, can strengthen the photon band gap characteristic of this structure, the radius of nuclear that can also be by changing nucleocapsid structure and the thickness of shell are regulated the residing position of photon band gap.
Description of drawings
Fig. 1 is the transmission electron microscope photo of monodisperse CdS-silicon dixoide nucleocapsid structure;
Fig. 2 is the field emission scanning electron microscope photo of monodisperse CdS-silicon dixoide nucleocapsid structure;
Fig. 3 is the XRD figure spectrum of monodisperse CdS-silicon dixoide nucleocapsid structure.
Embodiment
Embodiment:
1) monodisperse silica sphere particle that is 200nm with 300 milligrams of particle diameters is dispersed in the 250 ml deionized water solution with sonic oscillation, the Trisodium Citrate that adds 10 milliliter of 0.1 mol is done network and agent, add 15 microlitre trolamines and make tensio-active agent, and regulate pH value to 11 with ammoniacal liquor.60 ℃ of constant temperature magnetic agitation, drip the Cadmium chloride fine powder of 10 milliliter of 0.1 mol and the sulphur urine of 50 milliliter of 0.04 mol then, reacted 2 hours, obtain the suspension of the nucleocapsid structure of Cadmium Sulfide parcel silica spheres, adopt centrifugal deposition to add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol, remove reaction residue, 60 ℃ of oven dry, obtain monodisperse CdS-silicon dixoide nucleocapsid structure (as Fig. 1), as can be seen from the figure, Cadmium Sulfide evenly is wrapped in silica sphere, does not have the cohesion of unnecessary Cadmium Sulfide particle and impurity, and the thickness of Cadmium Sulfide shell approximately is 10nm.
Fig. 2 is use emission scan electron microscopic observation Cadmium Sulfide-silicon dixoide nucleocapsid structure, as can be seen from the figure the evengranular silica spheres surface that is coated on of Nano cadmium sulphide.
Products therefrom is XRD tests its crystalline structure, as shown in Figure 3, because silica spheres is an amorphous, the spectrogram peak is corresponding with the spectrogram of the Cadmium Sulfide with hexaplanar structure.

Claims (2)

1. the method for preparing monodisperse CdS-silicon dixoide nucleocapsid structure is characterized in that may further comprise the steps:
1) the uniform monodisperse silica sphere particle of particle diameter is dispersed in the deionized water solution with sonic oscillation, network made by the adding Trisodium Citrate and agent, hydramine are made tensio-active agent, and regulate pH value to 8~13 with ammoniacal liquor, 50 ℃~90 ℃ constant temperature magnetic agitation, add Cadmium chloride fine powder and sulphur urine then, the concentration that makes Cadmium chloride fine powder in the solution is 0.001~0.01 mol, and the concentration of sulphur urine is 0.002~0.02 mol, reacted 1~3 hour, and obtained the nucleocapsid structure suspension of Cadmium Sulfide parcel silica spheres;
2) add the ultra-sonic dispersion wash cycles with deionized water and dehydrated alcohol centrifugal deposition, remove reaction residue, oven dry obtains monodisperse CdS-silicon dixoide nucleocapsid structure.
2. the method for preparing monodisperse CdS-silicon dixoide nucleocapsid structure according to claim 1 is characterized in that said hydramine is trolamine or diethanolamine.
CNB2004100185894A 2004-05-19 2004-05-19 Method for preparing monodisperse cadium sulfide-silicon dioxide nucleo capsid structure Expired - Fee Related CN1258823C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100582196C (en) * 2006-05-19 2010-01-20 中国科学院理化技术研究所 Rare earth nano fluorescent particle with core-shell structure and preparation method and application thereof
EP1918264A3 (en) * 2006-11-06 2010-08-11 Howmedica Osteonics Corp. Method of synthesising a nano metric composite and for use thereof in a method for producing a ceramic component
CN104355290A (en) * 2014-11-27 2015-02-18 中国科学院重庆绿色智能技术研究院 Three-dimensional inner communicating multi-hole micro-nano structure and additive manufacturing method thereof
CN105964277A (en) * 2016-05-13 2016-09-28 南京理工大学 CdS/BiVO4 composite photocatalyst and preparation method thereof
CN108219238A (en) * 2017-05-24 2018-06-29 许晓山 A kind of new material for being used to prepare PE pipes

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100582196C (en) * 2006-05-19 2010-01-20 中国科学院理化技术研究所 Rare earth nano fluorescent particle with core-shell structure and preparation method and application thereof
EP1918264A3 (en) * 2006-11-06 2010-08-11 Howmedica Osteonics Corp. Method of synthesising a nano metric composite and for use thereof in a method for producing a ceramic component
CN104355290A (en) * 2014-11-27 2015-02-18 中国科学院重庆绿色智能技术研究院 Three-dimensional inner communicating multi-hole micro-nano structure and additive manufacturing method thereof
CN105964277A (en) * 2016-05-13 2016-09-28 南京理工大学 CdS/BiVO4 composite photocatalyst and preparation method thereof
CN108219238A (en) * 2017-05-24 2018-06-29 许晓山 A kind of new material for being used to prepare PE pipes

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