CN100497517C - Method for preparing core-shell quantum point of semiconductor in II VI families capable of adjusting and controlling wavelength of fluorescence - Google Patents
Method for preparing core-shell quantum point of semiconductor in II VI families capable of adjusting and controlling wavelength of fluorescence Download PDFInfo
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- CN100497517C CN100497517C CNB2007100364120A CN200710036412A CN100497517C CN 100497517 C CN100497517 C CN 100497517C CN B2007100364120 A CNB2007100364120 A CN B2007100364120A CN 200710036412 A CN200710036412 A CN 200710036412A CN 100497517 C CN100497517 C CN 100497517C
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Abstract
This invention discloses a method for preparing II-VI family semiconductor core/shell quantum dots with controllable fluorescent wavelength. The method comprises: exposing prepared CdSe core quantum dots to air at a high temperature, controlling the fluorescent property of the quantum dots by changing the exposure time, and coating in water and oxygen-free condition. At a certain temperature, the longer the time of quantum dots exposed to air, the shorter the fluorescent wavelength. The method simplifies the preparation of core quantum dots, and can prepare core/shell quantum dots that can emit red, yellow and green fluorescence from red emitting core quantum dots. With the CdS coating, the defect luminescence of the core quantum dots can be eliminated.
Description
Technical field
The present invention relates to the preparation method of a kind of II-VI family semi-conductor nucleocapsid quantum dot, specifically be meant a kind of preparation method of CdSe/CdS/ZnS core-shell quanta dots, this preparation method is adjustable its luminous fluorescent wavelength.
Background technology
Recent two decades comes, because semiconductor-quantum-point has special physical properties, thereby has obtained many scholars' favor, its preparation method is developed rapidly.Wherein the preparation method of the II of one of focus-CdSe of VI family quantum dot emerges in an endless stream especially, reason is that the CdSe quantum dot has the character of many uniquenesses: only need the size of control CdSe, just can obtain the fluorescence that emission wavelength almost covers whole visible light wave range; The full width at half maximum (FWHM) of fluorescence peak (FWHM) is very narrow, generally about 20nm-30nm; After coating the quantum dot of the same clan such as ZnS or CdS of broad stopband more, fluorescence efficiency can bring up to 60%-80%, and anti-fluorescence decline ability is strengthened greatly; Have bigger surface volume ratio, fluorescence is to chemical environment extreme sensitivity or the like.Thereby the CdSe/ZnS nuclear shell structure quantum point all has very tempting development prospect in a plurality of fields such as photodiode, nano laser, solar cell, nanometer bio probe, life codings.
Utilize alternately ion implantation (SILAR) method to realize the CdSe/ZnS nuclear shell structure quantum point, traditional slowly the dripping of comparing (wise drop) method, its advantage is: controlling packet coating layer ranges in thickness accurately; Can realize that the heterogeneity multiwalled coats, such as CdSe/CdS/Cd
0.5Zn
0.5S/ZnS reduces the influence that lattice mismatch brings to greatest extent.But there are two shortcomings in this method: the one, and the temperature of plate requirement is than higher, and the less quantum dot of size can be grown up before reaching this temperature again, fluorescence generation red shift, thereby the difficult coating that realizes less quantum dot; Another shortcoming is that the core-shell quanta dots of emission different colours fluorescence needs corresponding different IPs quantum dot raw material.
Summary of the invention
Defective based on above-mentioned prior art exists the objective of the invention is to propose a kind of the single quantum dot CdSe that glows of need as nuclear, coats CdS/ZnS outward, can realize launching respectively the preparation method of the core-shell quanta dots of red, yellow, green fluorescence.
For achieving the above object, technical scheme of the present invention is: ion implantation technique coats on the basis of CdSe quantum dot adopting alternately, at high temperature be exposed to the CdSe nuclear quantum dot for preparing in the air, realize the nuclear quantum dot fluorescence is regulated and control according to exposure duration, realize coating then under anhydrous and oxygen-free reaction atmosphere, its preparation process is as follows:
A. the preparation of the precursor solution of cadmium.Cadmium oxide and oleic acid are under logical argon gas condition, 240-260 ℃ are dissolved in the vaccenic acid, the amount that adds Cadmium oxide, oleic acid and vaccenic acid, amount is respectively 0.62-1.56%, 16.4-27.0%, 82.98-71.44% by mass percentage, preserves under 80-90 ℃ of water-baths.
B. the preparation of the precursor solution of zinc.Zinc oxide and oleic acid are under logical argon gas condition, 300-310 ℃ are dissolved in the vaccenic acid, the amount that adds zinc oxide, oleic acid and vaccenic acid, amount is respectively 0.4-1.0%, 16.5-27.1%, 83.1-71.9% by mass percentage, preserves under 80-90 ℃ of water-baths.
C. the preparation of sulphur precursor solution.Under logical argon gas condition, the sulphur powder is dissolved in the vaccenic acid under 160-180 ℃, adds the amount of sulphur powder and vaccenic acid, and amount is respectively 0.2-0.4%, 99.6-99.8% by mass percentage, at room temperature preserves.
D. examine the preparation of CdSe.Cadmium oxide, oleic acid and vaccenic acid are packed in the reaction vessel, in there-necked flask.The mass percent of Cadmium oxide, oleic acid and the vaccenic acid that adds is respectively 1.13-1.3%, 10.5-12.7%, 88.37-86%.Room temperature is reduced in being stirred and heated to 240-260 ℃ and all dissolving until Cadmium oxide under the logical argon gas condition then, as the storing solution of cadmium stand-by.
In the container bottle of sealing, selenium powder is dissolved in the mixed solution of three normal-butyl phosphorus and vaccenic acid.The mass percent of selenium powder, three normal-butyl phosphorus and the vaccenic acid that adds is respectively 4.1-8.2%, 28.3-32.7%, 67.3-59.1%, and is stand-by as the storing solution of selenium.
In the storing solution of above-mentioned cadmium, add octadecylamine and oxidation tri-n-octyl phosphine again, the octadecylamine mass percent of adding is 33.3-41.6%, and oxidation tri-n-octyl phosphine mass percent is 8.3%-16.6%.Under the argon gas condition, reacting by heating container to 280-300 ℃, then the storing solution with selenium injects wherein, after keeping 3-10min under 240-270 ℃ the temperature, remove after heating unit makes this product be cooled to 80 ℃, inject heavyization of acetone 2-3 times, centrifugal collecting precipitate.
The throw out of above-mentioned centrifugal collection is put into encloses container, add vaccenic acid and octadecylamine.The amount that adds vaccenic acid and octadecylamine, amount is respectively 50-66.6%, 33.3-50% by mass percentage, because the throw out add-on is about the thousandth of vaccenic acid and octadecylamine total mass, thereby ignores.Under logical argon gas condition, be heated to 180-220 ℃ then.Treat to open reaction vessel behind the temperature-stable, sample is contacted with atmosphere, in 2-30min, take out sample in batches, put into different reaction vessels, and recover logical argon gas.
E. the nuclear CdSe sample that contacts different time with atmosphere is coated CdS/ZnS outward.The precursor solution volume that needs are used for coating that how much calculates according to nuclear CdSe amount.At first coat the first layer CdS: inject the cadmium precursor liquid, after 5-10 minutes, inject the sulphur precursor liquid, annealed 230-240 ℃ of annealing temperatures 10-30 minutes; Coat second layer ZnS then, the coating condition is identical with the first layer, and so forth, finally obtains the CdSe/CdS/ZnS nuclear shell structure quantum point of the required coating number of plies.
The present invention regulates and control nuclear quantum dot fluorescence basket by regulation and control nuclear CdSe sample and atmosphere to move duration of contact: under the temperature certain condition, nuclear CdSe sample and atmosphere are long more duration of contact, and it is short more to examine the quantum dot fluorescence wavelength, and follows the luminous appearance of defect state.Then can regulate and control the red shift of core-shell quanta dots fluorescence according to the CdS that coats or the number of plies of ZnS.
Advantage of the present invention is:
1: simplified the preparation of nuclear quantum dot, only needed the single quantum dot nuclear that glows, just can coat out and launch core-shell quanta dots red, yellow, green fluorescence respectively, and the quantum dot nuclear preparation repeatability that size glows more greatly has been all well and good as raw material,
2: though it is luminous defect state to occur behind the nuclear quantum dot fluorescence blue shift, after coating CdS, but the luminous basically eliminate of defect state, and full width at half maximum (FWHM) and fluorescence efficiency still can be accepted.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of embodiment 1.Label 1-9 is respectively that nuclear CdSe sample contacts the fluorescence spectrum figure after 0 minute, 2 minutes, 5 minutes, 8 minutes, 11 minutes, 16 minutes, 20 minutes, 25 minutes, 30 minutes with atmosphere.
No. 9 spectrograms among Fig. 2 are exactly No. 9 spectrograms among Fig. 1, and No. 10 fluorescence spectrum figure are the spectrograms that coat one deck CdS sample outside No. 9 samples, and No. 11 is the spectrogram that continues to coat one deck ZnS sample on No. 10 samples.
Fig. 3 is that nuclear CdSe quantum dot respectively coats one deck outward
The trend map that CdSe/CdS/ZnS nuclear shell structure quantum point fluorescence peak wavelength changed along with the nuclear CdSe quantum dot contact atmosphere time.
Embodiment
Embodiment 1
A. the preparation of the precursor solution of cadmium.Cadmium oxide and oleic acid are under logical argon gas condition, and 250 ℃ are dissolved in the vaccenic acid, add the amount of Cadmium oxide, oleic acid and vaccenic acid, and amount is respectively 1.3%, 21.7%, 77.0% by mass percentage, preserves under 80 ℃ of water-baths;
B. the preparation of the precursor solution of zinc.Zinc oxide and oleic acid are under logical argon gas condition, and 300 ℃ are dissolved in the vaccenic acid, add the amount of zinc oxide, oleic acid and vaccenic acid, and amount is respectively 0.8%, 21.82%, 77.38% by mass percentage, preserves under 80 ℃ of water-baths;
C. the preparation of sulphur precursor solution.Under the same logical argon gas condition, the sulphur powder is dissolved in the vaccenic acid under 170 ℃, adds the amount of sulphur powder and vaccenic acid, and amount is respectively 0.32%, 99.68% by mass percentage, at room temperature preserves;
D. examine the preparation of CdSe.Detailed process is as follows: takes by weighing the 0.3mmol Cadmium oxide, packs into 0.5ml oleic acid, 3.8ml vaccenic acid and lead in the there-necked flask of argon gas, be stirred and heated to 260 ℃ and all dissolve, stop heating after finishing until Cadmium oxide, and stand-by as the storing solution of cadmium.
The 1.8mmol selenium powder is dissolved in the mixed solution of 0.7ml three normal-butyl phosphorus and 1.3ml vaccenic acid in the anhydrous and oxygen-free glove box, it is stand-by that the stock solution that obtains selenium is put into the pyriform bottle of sealing.
After the storing solution of cadmium is reduced to room temperature, add 2.5g 18 carbon amine and 0.5g oxidation tri-n-octyl phosphine, be heated to the stock solution that injects selenium after 280 ℃ immediately, after keeping 5min under 255 ℃ the temperature, remove after heating unit makes it be cooled to 80 ℃, inject heavyization of acetone 2 times, centrifugal collecting precipitate.
The throw out of above-mentioned centrifugal collection is put into encloses container, add vaccenic acid and octadecylamine.The amount that adds vaccenic acid and octadecylamine, amount is respectively 60% and 40% by mass percentage, under logical argon gas condition, is heated to 200 ℃ then.Treat to open reaction vessel behind the temperature-stable, sample is contacted with atmosphere, take out sample at 0 minute, 2 minutes, 5 minutes, 8 minutes, 11 minutes, 16 minutes, 20 minutes, 25 minutes, 30 minutes nine batches of branches, put into different reaction vessels, and recover logical argon gas.
E. the nuclear CdSe sample that contacts different time with atmosphere is coated CdS/ZnS outward respectively.At first coat the first layer CdS: inject the cadmium precursor liquid, after 7 minutes, inject the sulphur precursor liquid, annealed 235 ℃ of annealing temperatures 20 minutes; Coat second layer ZnS then, the coating condition is identical with the first layer, and so forth, Fig. 3 is nuclear CdSe quantum dot and coating
The trend map that CdSe/CdS/ZnS nuclear shell structure quantum point fluorescence peak wavelength changed along with the nuclear CdSe quantum dot contact atmosphere time.
Claims (1)
1. the preparation method of the II of an adjustable wavelength of fluorescence-VI family semi-conductor nucleocapsid quantum dot is characterized in that preparation process is as follows:
A. the preparation Cadmium oxide of the precursor solution of cadmium and oleic acid are under logical argon gas condition, 240-260 ℃ are dissolved in the vaccenic acid, the amount that adds Cadmium oxide, oleic acid and vaccenic acid, amount is respectively 0.62-1.56%, 16.4-27.0%, 82.98-71.44% by mass percentage, preserves under 80-90 ℃ of water-baths;
B. the preparation zinc oxide of the precursor solution of zinc and oleic acid are under logical argon gas condition, 300-310 ℃ are dissolved in the vaccenic acid, the amount that adds zinc oxide, oleic acid and vaccenic acid, amount is respectively 0.4-1.0%, 16.5-27.1%, 83.1-71.9% by mass percentage, preserves under 80-90 ℃ of water-baths;
C. the preparation of sulphur precursor solution is under logical argon gas condition, and the sulphur powder is dissolved in the vaccenic acid under 160-180 ℃, adds the amount of sulphur powder and vaccenic acid, and amount is respectively 0.2-0.4%, 99.6-99.8% by mass percentage, at room temperature preserves;
D. the preparation of examining CdSe is packed Cadmium oxide, oleic acid and vaccenic acid in the reaction vessel, the mass percent of Cadmium oxide, oleic acid and the vaccenic acid that adds is respectively 1.13-1.3%, 10.5-12.7%, 88.37-86%, being stirred and heated to 240-260 ℃ under the logical argon gas condition all dissolves until Cadmium oxide, reduce to room temperature then, stand-by as the storing solution of cadmium;
In the container bottle of sealing, the mass percent that selenium powder is dissolved in the selenium powder, three normal-butyl phosphorus and the vaccenic acid that add in the mixed solution of three normal-butyl phosphorus and vaccenic acid is respectively 4.1-8.2%, 28.3-32.7%, 67.3-59.1%, and is stand-by as the storing solution of selenium;
Again in the storing solution of above-mentioned cadmium, add octadecylamine and oxidation tri-n-octyl phosphine, the octadecylamine mass percent that adds is 33.3-41.6%, and oxidation tri-n-octyl phosphine mass percent is 8.3%-16.6%, under the argon gas condition, reacting by heating container to 280-300 ℃, then the storing solution of selenium is injected wherein, after keeping 3-10min under 240-270 ℃ the temperature, remove after heating unit makes this product be cooled to 80 ℃, inject heavyization of acetone 2-3 times, centrifugal collecting precipitate;
The throw out of above-mentioned centrifugal collection is put into an encloses container, add vaccenic acid and octadecylamine, the amount that adds vaccenic acid and octadecylamine, amount is respectively 50-66.6%, 33.3-50% by mass percentage, then under logical argon gas condition, be heated to 180-220 ℃, treat to open reaction vessel behind the temperature-stable, sample is contacted with atmosphere, in 2-30min, take out sample in batches, put into different reaction vessels, and recover logical argon gas;
E. the nuclear CdSe sample that contacts different time with atmosphere is coated how much calculate the precursor solution volume that needs be used for coat of CdS/ZnS according to nuclear CdSe amount outward, at first coat the first layer CdS: inject the cadmium precursor liquid, after 5-10 minutes, inject the sulphur precursor liquid, annealed 230-240 ℃ of annealing temperatures 10-30 minutes; Coat second layer ZnS then, the coating condition is identical with the first layer, and so forth, finally obtains the CdSe/CdS/ZnS nuclear shell structure quantum point of the required coating number of plies.
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