CN101585517A - A kind of synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light - Google Patents
A kind of synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light Download PDFInfo
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- CN101585517A CN101585517A CNA2009100538812A CN200910053881A CN101585517A CN 101585517 A CN101585517 A CN 101585517A CN A2009100538812 A CNA2009100538812 A CN A2009100538812A CN 200910053881 A CN200910053881 A CN 200910053881A CN 101585517 A CN101585517 A CN 101585517A
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Abstract
The present invention relates to a kind of synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light, belong to nm inorganic compound semiconductor material manufacturing process technology field.With Cadmium diacetate dihydrate and Sodium Selenite is raw material, and disodium ethylene diamine tetraacetate is a sequestrant, in the weakly alkaline aqueous solution, utilizes the mode of electron beam irradiation to synthesize CdSe quantum dots, and product has obtained powder of cadmium selenide quanta dots capable through separating.The prepared cadmium selenide powder of the present invention has fabulous water-soluble, and monodispersity is good, big or small homogeneous, and median size is 3nm, and the emission blue light, has good fluorescent characteristic, can be used for making biological fluorescent labeling.
Description
Technical field
The present invention relates to a kind of synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light, synthetic product is water-soluble emission blue light powder of cadmium selenide quanta dots capable, belongs to nm inorganic compound semiconductor material manufacturing process technology field.
Background technology
Quantum dot is mainly elementary composition by II-VI or III-V family, and it has electricity and the optical property that size relies on.It is widely used in a lot of fields, such as photodiode (LED), nonlinear optical device, solar cell, fields such as life science.The CdSe quantum dot becomes the maximum a kind of quantum dot of present research because its emission wavelength covers whole visible region.The more than ten years in past, scientists is developed the method for multiple synthetic CdSe quantum dot.
The method for preparing the CdSe quantum dot commonly used has the ultrasound wave irradiation, reverse micelle micro emulsion method of two-phase hydro-thermal surface reaction, polymkeric substance householder method, particular solution etc.But exist complex process, preparation time is long, needs High Temperature High Pressure, raw materials used shortcoming such as poisonous.Prepare the method that nano material is a kind of novelty with electronic beam irradiation technology, its preparation process is simple, quick, and the desired raw material low toxicity is easy to get, and product property is good, is a kind of synthetic method of green high-efficient.
Summary of the invention
The electronic-beam radiation synthesizing method that the purpose of this invention is to provide a kind of water-soluble emission blue light powder of cadmium selenide quanta dots capable.
The present invention adopts following technical scheme to realize.
A kind of synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light is characterized in that having following technological process and step:
A. at first, take by weighing a certain amount of Cadmium diacetate dihydrate and disodium ethylene diamine tetraacetate (EDTA) with electronic balance, it is dissolved in the distilled water, makes that concentration of cadmium ions and disodium ethylene diamine tetraacetate (EDTA) molar concentration rate are 1: 3～1: 5 in the solution, mix; Add Sodium Selenite then, making the molar concentration rate of itself and cadmium ion is 1: 1～1: 2, mix and make water white colloidal sol, regulating the pH value with the NaOH solution of 1mol/L then is 8～9, add Virahol again as oxidative free radical OH scavenging agent, its add-on is 6～10ml/100ml, again with the abundant stirring and evenly mixing of solution;
The sealed vessel that b. will fill the above-mentioned mixing solutions for preparing is positioned under the electron beam irradiation that the rumbatron of 2.5MeV, 6～7mA produces and carries out radiation treatment, and its irradiation dose is 14～42Mrad, and the irradiation reaction time is 7～21 minutes;
C. then the product behind the irradiation is revolved inspissation and contract, the supercentrifuge centrifugation is used in dialysis again, the solid after the separation more repeatedly with washing with alcohol, to remove wherein unreacted ion and excessive disodium ethylene diamine tetraacetate;
D. above-mentioned solid is placed on drying in the vacuum drying oven, temperature is 60～80 ℃, and drying time is 7～12 hours, finally obtains the nanometer selenizing cadmium dust of white, is powder of cadmium selenide quanta dots capable.
The present invention prepares cadmium selenide quantum dot nano by the electron beam that uses rumbatron to produce as source of radiation, and is pollution-free in the radiation synthesis process, the one-step synthesis good water solubility, can launch the CdSe quantum dot of blue light.The inventive method technology is simple, does not have any intermediate product, and is easy to operate, can realize suitability for industrialized production.The nano-tube/CdS e quantum dot that utilizes the inventive method to prepare can be used for biological fluorescent labelling and photocatalysis field.
In the preparation process of the present invention, as sequestrant, can make CdSe quantum dot surface coat one deck EDTA disodium ethylene diamine tetraacetate, form Cd
2+-EDTA complexing layer not only stops between the nanoparticle mutually and assembles, and it is luminous and obtain the luminous of more exciton states to have reduced defect state that its surface imperfection causes, thereby makes electronics and the hole can be effectively directly luminous.The regulator solution pH value is 8～9, makes solution be weakly alkaline, helps EDTA and Cd
2+Complexing.The effect that adds Virahol is to remove the OH oxidative free radical.
The advantage of the inventive method is: can not use any catalyzer just can operate at normal temperatures and pressures, and preparation process only need tens minutes time, and simple very fast; In addition, since electron beam by rumbatron produce, rumbatron cuts out, electron beam disappears immediately, so security is good, pollution-free, helps environmental protection.
Description of drawings
Fig. 1 is the XRD figure spectrum of the CdSe quantum dot powder of electron beam irradiation method preparation, among the figure X-coordinate be angular unit (°), illustrate that synthetic product is a zink sulphide type CdSe powder.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
The concrete preparation process of present embodiment is as follows:
A. at first, take by weighing a certain amount of Cadmium diacetate dihydrate and disodium ethylene diamine tetraacetate (EDTA), it is dissolved in the distilled water, make wherein that concentration of cadmium ions and EDTA molar concentration rate are 1: 3, mix with electronic balance; Add Sodium Selenite then, making the molar concentration rate of itself and cadmium ion is 1: 1, mix and make water white colloidal sol, using NaOH (1mol/L) solution to regulate the pH value then is 9, add Virahol again as oxidative free radical OH scavenging agent, its add-on is 6ml/100ml, again with the abundant stirring and evenly mixing of solution;
B. the above-mentioned sealed vessel that fills the mixing solutions for preparing is positioned under the electron beam irradiation that the rumbatron of 2.5MeV, 7mA produces and carries out radiation treatment, its irradiation dose is 14,28,42Mrad, the irradiation reaction time was respectively 10,20,30 minutes, and the poor performance of the final gained powder of these several conditions is few;
C. then the product behind the irradiation is revolved inspissation and contract, the supercentrifuge centrifugation is used in dialysis again, the solid after the separation more repeatedly with washing with alcohol, to remove wherein unreacted ion and excessive disodium ethylene diamine tetraacetate;
D. resultant of reaction is placed on drying in the vacuum drying oven, temperature is 70 ℃, and drying time is 12 hours, finally obtains the nanometer selenizing cadmium dust of white, is powder of cadmium selenide quanta dots capable.
Prepared sample in the foregoing description carries out every characteristic test with instrument, and its test case and result thereof are as follows:
1, with X-ray diffraction analysis (XRD), can determine that from diffraction peak prepared white powder is the nanometer cadmium selenide.
2, utilize atomic force microscope (AFM), transmission electron microscope (TEM), high power transmission electron microscope (HRTEM) is observed particulate pattern and size, can see prepared nanometer cadmium selenide is particulate state, monodispersity is good, no agglomeration, and its median size is 2.5nm.
3, by the optical property of ultraviolet-visible pectrophotometer test material, calculate to such an extent that the nanocrystalline energy gap of CdSe is 2.78eV,, shown the quantum size effect of nano material obviously greater than the energy gap (1.70eV) of block CdSe.
4, pass through the optical property of spectrophotofluorometer analyser specimen, CdSe launches blue light under the excitation wavelength of 350nm, fluorescence quantum yield is up to 21.63%, because product has fabulous water-solublely, utilizes this fluorescent characteristic can be used to make biological fluorescent labeling again.
Claims (1)
1. synthetic method of launching the powder of cadmium selenide quanta dots capable of blue light is characterized in that having following technological process and step:
A. at first, take by weighing a certain amount of Cadmium diacetate dihydrate and disodium ethylene diamine tetraacetate, it is dissolved in the distilled water, make that the molar concentration rate of concentration of cadmium ions and disodium ethylene diamine tetraacetate is 1: 3～1: 5 in the solution, mix with electronic balance; Add Sodium Selenite then, making the molar concentration rate of itself and cadmium ion is 1: 1～1: 2, mix and make water white colloidal sol, regulating the pH value with the NaOH solution of 1mol/L then is 8～9, add Virahol again as oxidative free radical OH scavenging agent, its add-on is 6～10ml/100ml, again with the abundant stirring and evenly mixing of solution;
The sealed vessel that b. will fill the above-mentioned mixing solutions for preparing is positioned under the electron beam irradiation that the rumbatron of 2.5MeV, 6～7mA produces and carries out radiation treatment, and its irradiation dose is 14～42Mrad, and the irradiation reaction time is 7～21 minutes;
C. then the product behind the irradiation is revolved inspissation and contract, the supercentrifuge centrifugation is used in dialysis again, the solid after the separation more repeatedly with washing with alcohol, to remove wherein unreacted ion and excessive disodium ethylene diamine tetraacetate;
D. above-mentioned solid is placed on drying in the vacuum drying oven, temperature is 60～80 ℃, and drying time is 7～12 hours, finally obtains the nanometer selenizing cadmium dust of white, is powder of cadmium selenide quanta dots capable.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528804A (en) * | 2014-11-04 | 2015-04-22 | 华文蔚 | Irradiation synthetic method for silicon carbide nano-crystal whisker composite material coated with zinc sulfide (ZnS) |
| CN105148973A (en) * | 2015-09-17 | 2015-12-16 | 上海大学 | Preparation method for electron beam irradiation modified graphite-like-phase carbon nitride for visible-light-driven photocatalyst |
| CN107993923A (en) * | 2017-12-08 | 2018-05-04 | 青岛大学 | A kind of controllable quantum dots array preparation method based on photo-thermal effect |
| CN109536159A (en) * | 2018-12-14 | 2019-03-29 | 南京航空航天大学 | A method of quantum dot fluorescence performance is improved using radiation |
| CN112349870A (en) * | 2019-08-08 | 2021-02-09 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN112631019A (en) * | 2020-12-25 | 2021-04-09 | 舟山扑浪实业有限公司 | Preparation method of quantum dot display panel and quantum dot display panel |
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2009
- 2009-06-26 CN CNA2009100538812A patent/CN101585517A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528804A (en) * | 2014-11-04 | 2015-04-22 | 华文蔚 | Irradiation synthetic method for silicon carbide nano-crystal whisker composite material coated with zinc sulfide (ZnS) |
| CN104528804B (en) * | 2014-11-04 | 2016-05-18 | 华文蔚 | A kind of irradiation synthesis method of zinc sulphide (ZnS) carbon coated SiClx nano whisker composite material |
| CN105148973A (en) * | 2015-09-17 | 2015-12-16 | 上海大学 | Preparation method for electron beam irradiation modified graphite-like-phase carbon nitride for visible-light-driven photocatalyst |
| CN107993923A (en) * | 2017-12-08 | 2018-05-04 | 青岛大学 | A kind of controllable quantum dots array preparation method based on photo-thermal effect |
| CN107993923B (en) * | 2017-12-08 | 2020-02-21 | 青岛大学 | Preparation method of controllable quantum dot array based on photothermal effect |
| CN109536159A (en) * | 2018-12-14 | 2019-03-29 | 南京航空航天大学 | A method of quantum dot fluorescence performance is improved using radiation |
| CN109536159B (en) * | 2018-12-14 | 2019-10-22 | 南京航空航天大学 | A method of quantum dot fluorescence performance is improved using radiation |
| CN112349870A (en) * | 2019-08-08 | 2021-02-09 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN112631019A (en) * | 2020-12-25 | 2021-04-09 | 舟山扑浪实业有限公司 | Preparation method of quantum dot display panel and quantum dot display panel |
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