CN108251116A - A kind of preparation method of chirality CdSe quantum dot - Google Patents

A kind of preparation method of chirality CdSe quantum dot Download PDF

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CN108251116A
CN108251116A CN201711383313.XA CN201711383313A CN108251116A CN 108251116 A CN108251116 A CN 108251116A CN 201711383313 A CN201711383313 A CN 201711383313A CN 108251116 A CN108251116 A CN 108251116A
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quantum dot
cysteine
cdse quantum
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赵丹
马诗瑶
郝健
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South Central Minzu University
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Abstract

The invention discloses a kind of preparation methods of chiral CdSe quantum dot, include the following steps:(1) sodium hydrogen selenide aqueous solution is prepared, and in less than 4 DEG C preservations;(2) caddy and ligand are dissolved in the water, it is 7 12 to adjust pH value, precursor solution is obtained, under the protection of inert gas, by precursor solution ice bath stirring;Wherein described ligand is combinations two or more in penicillamine, cysteine, N acetylcysteines, glutathione or N isobutyryl cysteines;(3) the sodium hydrogen selenide solution prepared in step (1) is injected into the precursor solution in step (2), 70 220 DEG C of 10 120min of heating are cooled to room temperature to get chiral CdSe quantum dot solution.The quantum dot can be widely applied to enantiomer identification with detaching, the fields such as nano-equipment, chiral sensor and asymmetry catalysis.

Description

A kind of preparation method of chirality CdSe quantum dot
Technical field
The invention belongs to the preparation method technical fields of nano material, specifically disclose a kind of synthesis multiple ligands package The straightforward procedure of chiral CdSe quantum dot shows strong circular dichroism in the range of 200-475nm.It is different by mixing Structure or different stereochemical chiral ligand, can effectively quantum point optical isomerism.
Background technology
On chemistry, biology and medical science, chirality has been already engaged in many practices and basic research, and researchers have found It is an important factor for influencing structure-activity relationship.Schaaff seminars are found that inorganic nanocrystal has chirality for the first time, And then, researchers are found that gold, silver nano-cluster and the quantum dot of chiral molecules package also have chirality, these achievements successively Have great importance for the development of nano science and nanometer technology.Chiral nanomaterial has potential application prospect, It will be identified for enantiomer with detaching, the open new visual field in fields such as nano-equipment, chiral sensor and asymmetry catalysis.
Chiral quantum dot, by its good photostability, small size and surface are easy to the advantages such as functionalization and have attracted The sight of numerous researchers.The quantum dot of general ligand package does not have optical activity, and only chiral ligand wraps up Quantum dot has optical activity, however the type of chiral ligand is limited, so that the type of chiral quantum dot is more single, limitation Its subsequent application.
Invention content
The invention solves technical barrier be current chiral quantum dot type it is less, be unfavorable for chiral theoretical research And it is detected in biochemistry, the application in the fields such as asymmetric syntheses and medical diagnosis.
In order to solve the above technical problem, the present invention provides a kind of preparation methods of chiral CdSe quantum dot:Pass through two kinds The combination of more than ligand can obtain novel chiral quantum dot, greatly extend the diversity of chiral quantum dot.And By changing the molar ratio of multiple ligands, the delicately chirality of quantum point.The present invention will be ground for the theory of chiral quantum dot Study carefully and provide solid foundation with practical application.
The preparation method of chirality CdSe quantum dot provided by the invention, includes the following steps:
(1) sodium hydrogen selenide aqueous solution is prepared, and in less than 4 DEG C preservations;
(2) caddy and ligand are dissolved in the water, adjusting pH value is 7-12, precursor solution is obtained, in the guarantor of inert gas Under shield, by precursor solution ice bath stirring;The wherein described ligand is penicillamine, cysteine, N- acetyl-cysteine, paddy Guang Two or more combination in sweet peptide or N- isobutyryls-cysteine;
(3) the sodium hydrogen selenide solution prepared in step (1) is injected into the precursor solution in step (2), 70-220 DEG C 10-120min is heated, is cooled to room temperature to get chiral CdSe quantum dot solution.
Preferably, step (4) is further included after step (3):The chiral CdSe quantum dot solution that step (3) is obtained carries out Purifying mixes quantum dot solution and organic reagent, centrifugation, and lower part precipitation is CdSe quantum dot after purification.
Preferably, the organic reagent is one of methanol, ethyl alcohol, acetonitrile, isopropanol or acetone or combination, The volume ratio of more preferably isopropanol or methanol, quantum dot solution and organic reagent is 1:1-10.
Preferably, the Cd:Se:The molar ratio of ligand total amount is 1:0.1-1:0.5-5, wherein, mole of caddy A concentration of 1-10mmol/L.
Preferably, the ligand is penicillamine, cysteine, N- acetyl-cysteine, glutathione or N- isobutyls Two kinds of combination in acyl-cysteine, the molar ratio of two kinds of ligands is 1:0.1-10.
Preferably, combination or glutathione and N- isobutyryl-half Guang ammonia of the ligand for penicillamine and cysteine The combination of acid.
Preferably, the ligand is penicillamine, cysteine, N- acetyl-cysteine, glutathione or N- isobutyls Three kinds of combination in acyl-cysteine, the molar ratio of three kinds of ligands is 1:0.1-10:0.1-10.
Preferably, the ligand is the combination of penicillamine, N- acetyl-cysteine and N- isobutyryls-cysteine.
Preferably, the preparation method of the sodium hydrogen selenide aqueous solution is:Sodium borohydride and selenium powder, which are dissolved in ultra-pure water, to be made Standby sodium hydrogen selenide solution, and saved backup in less than 4 DEG C, wherein the input amount of the selenium powder is 30mg, the throwing of sodium borohydride Enter amount for 10-100mg.
Preferably, mode of heating has 3 kinds, and immersion method, bath oiling, hydro-thermal method, the reaction temperature of immersion method is 70-90 DEG C, Bath oiling, hydro-thermal method reaction temperature be 80-220 DEG C.
The wherein described reaction vessel is hydrothermal reaction kettle, round-bottomed flask.
Preferably, reaction vessel is hydrothermal reaction kettle.
The wherein described heating container is water-bath, oil bath pan, electric heating constant-temperature blowing drying box.
Preferably, reaction vessel is electric heating constant-temperature blowing drying box.
Compared with prior art, it is the advantages of the method for the present invention with advantageous effect:
1. the multiple ligands that the present invention the uses successful chirality induction of CdSe quantum dot.Ligand with opposite configuration Mirror symmetry relationship is presented in the circular dichroism spectrogram of the CdSe quantum dot of preparation.
2. the quantum dot of general ligand package does not have optical activity, the quantum dot of only chiral ligand package has light Activity is learned, but the quantity of chiral ligand is limited so that the type of chiral quantum dot is more single.However the present invention is based on The compatible use of multiple ligands, extension and diversification for chiral quantum vertex type provide possibility, are more advantageous to quantum dot and exist The application in the fields such as the identification of enantiomer is with detaching, nano-equipment, chiral sensor and asymmetry catalysis.
3. the present invention is by changing the rate of charges of multiple ligands, can delicately quantum point Chiral properties, be hand Property quantum dot detected in biochemistry, the potential application of asymmetric syntheses and area of medical diagnostics provides wide prospect.
Description of the drawings
Figure 1A:The circular dichroism spectrogram of the CdSe quantum dot of comparative example 1.
Figure 1B:The circular dichroism spectrogram of the CdSe quantum dot of comparative example 2.
Fig. 1 C:The circular dichroism spectrogram of synthesized CdSe quantum dot in embodiment 1.
Fig. 1 D:The CdSe amounts that the CdSe quantum dot and the two of individual L-cysteine or L- penicillamines package are wrapped up jointly The ultraviolet absorpting spectrum of son point.
Fig. 2A:The molar ratio of cysteine and penicillamine is 1:The circular dichroism spectrogram of the CdSe quantum dot prepared when 1.
Fig. 2 B:The molar ratio of cysteine and penicillamine is 1:The circular dichroism spectrogram of the CdSe quantum dot prepared when 2.
Fig. 2 C:Molar ratio for cysteine and penicillamine is 1:The circular dichroism spectrogram of the CdSe quantum dot prepared when 3.
Fig. 3:N- acetyl-cysteine and the circle of the CdSe quantum dot of N- isobutyryls-cysteine functionalization in embodiment 3 Two chromatograms.
Fig. 4:The circular dichroism spectra of the CdSe quantum dot of 4 GSH-PX activity of embodiment and N- isobutyryls-cysteine functionalization Figure.
Fig. 5:The CdSe quantum of penicillamine, N- acetyl-cysteine and N- isobutyryls-cysteine package in embodiment 5 The circular dichroism spectrogram of point.
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments, so that those skilled in the art can be with It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
The preparation method of the chiral CdSe quantum dot of the present embodiment, is as follows:
(1) 30mg selenium powders and 60mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, it will Freshly prepared sodium hydrogen selenide solution saves backup at 4 DEG C;
(2) caddy, cysteine and penicillamine are dissolved in ultra-pure water and are vigorously stirred 5min, obtain precursor solution. Then the pH value that precursor solution is adjusted with 1mol/L sodium hydroxides is 10.Under the protection of nitrogen, precursor solution is placed in ice water In be vigorously stirred 5min;
(3) in the precursor solution that the sodium hydrogen selenide solution prepared in (1) is injected into (2) and it is vigorously stirred 5min.Most Afterwards, mixed solution is transferred in hydrothermal reaction kettle, it is cold is placed in 150 DEG C of heating 60min, bath in electric heating constant-temperature blowing drying box But to room temperature to get chiral CdSe quantum dot solution, Cd:Se:Cysteine:The molar ratio of penicillamine is 1:0.5:0.9:0.9, The molar concentration of caddy is 5mmol/L;
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, is by volume by quantum dot solution and methanol 1:1 mixing, 3000rpm centrifugation 30min, lower part precipitation are CdSe quantum dot after purification.
Comparative example 1 is the CdSe quantum dot of independent cysteine package, and circular dichroism collection of illustrative plates is shown in Figure 1A, and comparative example 2 is single The CdSe quantum dot of only penicillamine package, circular dichroism collection of illustrative plates are shown in Figure 1B, and embodiment 1 is wrapped up jointly for cysteine and penicillamine CdSe quantum dot, circular dichroism collection of illustrative plates is shown in Fig. 1 C.By Figure 1A~C it is found that ligand (either single ligand with opposite configuration Or double ligands) mirror symmetry relationship is presented in the circular dichroism collection of illustrative plates of CdSe quantum dot for preparing.
Fig. 1 D are the CdSe that the CdSe quantum dot of individual L-cysteine or L- penicillamines package and the two are wrapped up jointly Ultraviolet absorpting spectrum corresponding to quantum dot, by Fig. 1 D it is found that the CdSe quantum dot table of L-cysteine or L- penicillamines package Reveal weaker ultraviolet absorption peak, and the CdSe quantum dot that L-cysteine and L- penicillamines wrap up jointly shows apparent purple Outer absorption peak shows the CdSe quantum dot of double ligand packages, compared to the CdSe quantum dot of single ligand package, has more uniform Grain size and more excellent monodispersity.The phenomenon that similary, also occurs in the CdSe amounts of D-Cys and Beracilline package In son point.
Embodiment 2
The preparation method of the chiral CdSe quantum dot of the present embodiment, is as follows:
(1) 30mg selenium powders and 60mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, it will Freshly prepared sodium hydrogen selenide solution saves backup at 4 DEG C;
(2) caddy, cysteine and penicillamine are dissolved in ultra-pure water and are vigorously stirred 5min, then with 1mol/L hydrogen The pH that sodium oxide molybdena adjusts precursor solution is 10.Under the protection of argon gas, precursor solution is placed in ice water and is vigorously stirred 5min, Cd:Se:The molar ratio of total ligand is 1:0.5:1.8, the molar ratio of cysteine and penicillamine is 1:1~3, mole of caddy A concentration of 5mmol/L.
(3) in the precursor solution that the sodium hydrogen selenide solution prepared in (1) is injected into (2) and it is vigorously stirred 5min.Most Afterwards, mixed solution is transferred in hydrothermal reaction kettle, it is cold is placed in 150 DEG C of heating 60min, bath in electric heating constant-temperature blowing drying box But to room temperature to get chiral CdSe quantum dot solution.
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, by quantum dot solution and methanol by volume 1: 1 mixing, 3000rpm centrifugation 30min, lower part precipitation are CdSe quantum dot after purification.Fig. 2A is cysteine and penicillamine Molar ratio be 1:The circular dichroism spectrogram of the CdSe quantum dot prepared when 1, Fig. 2 B are that the molar ratio of cysteine and penicillamine is 1:The circular dichroism spectrogram of the CdSe quantum dot prepared when 2, Fig. 2 C are that the molar ratio of cysteine and penicillamine is 1:It is prepared when 3 The circular dichroism spectrogram of CdSe quantum dot.By Fig. 2A~C it is found that with the increase of penicillamine input amount, the circle two of CdSe quantum dot The slight blue shift of absorption peak of chromatogram illustrates the molar ratio by adjusting double ligands, can delicately adjust CdSe quantum dot It is chiral.
Embodiment 3
The preparation method of the chiral CdSe quantum dot of the present embodiment, is as follows:
(1) 30mg selenium powders and 10mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, it will Freshly prepared sodium hydrogen selenide solution saves backup at 4 DEG C;
(2) caddy, N- acetyl-cysteine and N- isobutyryls-cysteine are dissolved in ultra-pure water and be vigorously stirred 120min, the pH value that precursor solution is then adjusted with 1mol/L ammonium hydroxide are 12.Under the protection of nitrogen, precursor solution is placed in ice 120min, Cd are vigorously stirred in water:Se:N- acetyl-cysteine:The molar ratio of N- isobutyryls-cysteine is 1:0.3: 0.25:0.25, the molar concentration of caddy is 1mmol/L.
(3) it is vigorously stirred in the precursor solution that the sodium hydrogen selenide solution prepared in a certain amount of (1) is injected into (2) 120min.Finally, mixed solution is transferred in round-bottomed flask, is placed in 120 DEG C of heating 80min, bath in oil bath pan and is cooled to Room temperature is to get chiral CdSe quantum dot solution.
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, by quantum dot solution and ethyl alcohol by volume 1: 10 mixing, 15000rpm centrifugation 5min, lower part precipitation is CdSe quantum dot after purification, and N- acetyl-cysteine and N- are different The circular dichroism spectrogram of the CdSe quantum dot of the common functionalization of butyryl-cysteine is shown in Fig. 3.From the figure 3, it may be seen that with opposite configuration Mirror symmetry is presented in the circular dichroism collection of illustrative plates for the CdSe quantum dot that N- acetyl-cysteine is prepared with N- isobutyryls-cysteine Relationship.
Embodiment 4
The preparation method of the chiral CdSe quantum dot of the present embodiment, is as follows:
(1) sodium borohydride and selenium powder are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, by fresh preparation Sodium hydrogen selenide solution saved backup at 4 DEG C, the input amount of selenium powder is 30mg, and the input amount of sodium borohydride is 80mg;
(2) caddy, glutathione and N- isobutyryls-cysteine are dissolved in ultra-pure water and are vigorously stirred 30min, so The pH for adjusting precursor solution with 1mol/L ammonium hydroxide afterwards is 7.Under the protection of argon gas, precursor solution is placed in ice water and is acutely stirred Mix 30min, Cd:Se:Glutathione:The molar ratio of N- isobutyryls-cysteine is 1:1:2.5:2.5, caddy it is mole dense It spends for 3mmol/L.
(3) it is vigorously stirred in the precursor solution that the sodium hydrogen selenide solution prepared in a certain amount of (1) is injected into (2) 30min.Finally, mixed solution is transferred in hydrothermal reaction kettle, is placed in 220 DEG C of heating in electric heating constant-temperature blowing drying box 10min, bath are cooled to room temperature to get chiral CdSe quantum dot solution.
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, is by volume by quantum dot solution and acetonitrile 1:10 mixing, 10000rpm centrifugation 10min, the CdSe quantum dot of lower part precipitation as after purification, glutathione and N- isobutyryls- The circular dichroism spectrogram of the CdSe quantum dot of cysteine functionalization is shown in Fig. 4.
As shown in Figure 4, the CdSe quantum dot that prepared by the glutathione with opposite configuration and N- isobutyryls-cysteine Mirror symmetry relationship is presented in circular dichroism collection of illustrative plates.
Embodiment 5
The preparation method of the chiral CdSe quantum dot of the present embodiment, is as follows:
(1) 30mg selenium powders and 100mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, Freshly prepared sodium hydrogen selenide solution is saved backup at 4 DEG C;
(2) caddy, penicillamine, N- acetyl-cysteine and N- isobutyryls-cysteine are dissolved in ultra-pure water acute Strong stirring 20min, the pH that precursor solution is then adjusted with 1mol/L sodium hydroxides are 9.Under the protection of nitrogen, by precursor solution It is placed in ice water and is vigorously stirred 20min, Cd:Se:Penicillamine:N- acetyl-cysteine:Mole of N- isobutyryls-cysteine Than being 1:0.1:1.5:1.5:1.5, the molar concentration of caddy is 10mmol/L.
(3) it is vigorously stirred in the precursor solution that the sodium hydrogen selenide solution prepared in a certain amount of (1) is injected into (2) 20min.Finally, mixed solution is transferred in round-bottomed flask, is placed in 70 DEG C of heating 120min, bath in water-bath and is cooled to room Temperature is to get chiral CdSe quantum dot solution.
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, by quantum dot solution and isopropanol by volume It is 1:3 mixing, 8000rpm centrifugation 10min, the CdSe quantum dot of lower part precipitation as after purification, penicillamine ,-half Guang of N- acetyl The circular dichroism collection of illustrative plates of the CdSe quantum dot of propylhomoserin and N- isobutyryls-cysteine package is shown in Fig. 5.
As shown in Figure 5, prepared by penicillamine, N- acetyl-cysteine and N- isobutyryls with opposite configuration-cysteine The circular dichroism collection of illustrative plates of CdSe quantum dot mirror symmetry relationship is presented.
Comparative example 1
1. a kind of preparation method of chirality CdSe quantum dot, is as follows:
(1) 30mg selenium powders and 60mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, it will Freshly prepared sodium hydrogen selenide solution saves backup at 4 DEG C;
(2) caddy and cysteine are dissolved in ultra-pure water and are vigorously stirred 5min, obtain precursor solution.Then it uses The pH value that 1mol/L sodium hydroxides adjust precursor solution is 10.Under the protection of nitrogen, precursor solution is placed in ice water acutely Stir 5min;
(3) in the precursor solution that the sodium hydrogen selenide solution prepared in (1) is injected into (2) and it is vigorously stirred 5min.Most Afterwards, mixed solution is transferred in hydrothermal reaction kettle, it is cold is placed in 150 DEG C of heating 60min, bath in electric heating constant-temperature blowing drying box But to room temperature to get chiral CdSe quantum dot solution, Cd:Se:The molar ratio of cysteine is 1:0.5:1.8, caddy rubs You are a concentration of 5mmol/L;
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, is by volume by quantum dot solution and methanol 1:1 mixing, 3000rpm centrifugation 30min, the CdSe quantum dot of lower part precipitation as after purification, the CdSe amounts of cysteine package The circular dichroism spectrogram of son point is shown in Figure 1A.
Comparative example 2
1. a kind of preparation method of chirality CdSe quantum dot, is as follows:
(1) 30mg selenium powders and 60mg sodium borohydrides are dissolved in the ultra-pure water of 3mL first and prepare sodium hydrogen selenide solution, it will Freshly prepared sodium hydrogen selenide solution saves backup at 4 DEG C;
(2) caddy and penicillamine are dissolved in ultra-pure water and are vigorously stirred 5min, obtain precursor solution.Then it uses The pH value that 1mol/L sodium hydroxides adjust precursor solution is 10.Under the protection of nitrogen, precursor solution is placed in ice water acutely Stir 5min;
(3) in the precursor solution that the sodium hydrogen selenide solution prepared in (1) is injected into (2) and it is vigorously stirred 5min.Most Afterwards, mixed solution is transferred in hydrothermal reaction kettle, it is cold is placed in 150 DEG C of heating 60min, bath in electric heating constant-temperature blowing drying box But to room temperature to get chiral CdSe quantum dot solution, Cd:Se:The molar ratio of penicillamine is 1:0.5:1.8 mole of caddy A concentration of 5mmol/L;
(4) the chiral CdSe quantum dot solution that (3) obtain is purified, is by volume by quantum dot solution and methanol 1:1 mixing, 3000rpm centrifugation 30min, lower part precipitation are CdSe quantum dot after purification, cysteine and penicillamine package The circular dichroism spectrogram of CdSe quantum dot see Figure 1B.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention It encloses without being limited thereto.The equivalent substitute or transformation that those skilled in the art are made on the basis of the present invention, in the present invention Protection domain within.Protection scope of the present invention is subject to claims.

Claims (10)

1. a kind of preparation method of chirality CdSe quantum dot, which is characterized in that include the following steps:
(1) sodium hydrogen selenide aqueous solution is prepared, and in less than 4 DEG C preservations;
(2) caddy and ligand being dissolved in the water, adjusting pH value is 7-12, obtains precursor solution, under the protection of inert gas, By precursor solution ice bath stirring;The wherein described ligand for penicillamine, cysteine, N- acetyl-cysteine, glutathione or Two or more combination in N- isobutyryls-cysteine;
(3) the sodium hydrogen selenide solution prepared in step (1) is injected into the precursor solution in step (2), 70-220 DEG C of heating 10-120min is cooled to room temperature to get chiral CdSe quantum dot solution.
2. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that also wrapped after step (3) Include step (4):The chiral CdSe quantum dot solution that step (3) obtains is purified, quantum dot solution and organic reagent are mixed It closes, centrifugation, lower part precipitation is CdSe quantum dot after purification.
3. the preparation method of chirality CdSe quantum dot according to claim 2, which is characterized in that the organic reagent is The volume ratio of one of methanol, ethyl alcohol, acetonitrile, isopropanol or acetone or combination, quantum dot solution and organic reagent is 1:1-10。
4. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the Cd:Se:Ligand The molar ratio of total amount is 1:0.1-1:0.5-5, wherein, the molar concentration of caddy is 1-10mmol/L.
5. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the ligand is mould Two kinds of combination, two kinds of ligands in amine, cysteine, N- acetyl-cysteine, glutathione or N- isobutyryls-cysteine Molar ratio be 1:0.1-10.
6. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the ligand is penicillamine Combination or glutathione and the combination of N- isobutyryls-cysteine with cysteine.
7. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the ligand is mould Three kinds of combination, three kinds of ligands in amine, cysteine, N- acetyl-cysteine, glutathione or N- isobutyryls-cysteine Molar ratio be 1:0.1-10:0.1-10.
8. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the ligand is mould The combination of amine, N- acetyl-cysteine and N- isobutyryls-cysteine.
9. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that the sodium hydrogen selenide is water-soluble The preparation method of liquid is:Sodium borohydride and selenium powder, which are dissolved in ultra-pure water, prepares sodium hydrogen selenide solution, and preserves in less than 4 DEG C standby With wherein the input amount of the selenium powder is 30mg, the input amount of sodium borohydride is 10-100mg.
10. the preparation method of chirality CdSe quantum dot according to claim 1, which is characterized in that mode of heating has 3 kinds, Immersion method, bath oiling, hydro-thermal method, the reaction temperature of immersion method are 70-90 DEG C, bath oiling, hydro-thermal method reaction temperature be 80- 220℃。
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* Cited by examiner, † Cited by third party
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101747899A (en) * 2010-01-08 2010-06-23 浙江大学 Method for synthesizing gold-doped fluorescent quantum dots
CN102925160A (en) * 2010-01-08 2013-02-13 浙江大学 Gold-doped fluorescent quantum dot synthetic method
CN103663390A (en) * 2012-09-25 2014-03-26 江南大学 Preparation method of chiral CdTe quantum dot and use thereof for detecting optical isocompound enantiomer
CN104710989A (en) * 2014-07-08 2015-06-17 中南民族大学 Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101747899A (en) * 2010-01-08 2010-06-23 浙江大学 Method for synthesizing gold-doped fluorescent quantum dots
CN102925160A (en) * 2010-01-08 2013-02-13 浙江大学 Gold-doped fluorescent quantum dot synthetic method
CN103663390A (en) * 2012-09-25 2014-03-26 江南大学 Preparation method of chiral CdTe quantum dot and use thereof for detecting optical isocompound enantiomer
CN104710989A (en) * 2014-07-08 2015-06-17 中南民族大学 Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘婧文 等: "手性化合物组合修饰剂对CdSe纳米晶荧光性能的影响及标记大肠杆菌的研究", 《无机化学学报》 *
陈帼敏 等: "手性双修饰剂修饰的CdSe纳米晶的合成及选择性识别Hg(II)的研究", 《分析化学》 *
陈帼敏: "新型CdSe纳米晶的制备及其应用研究", 《万方数据知识服务平台,华南师范大学硕士学位论文》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111517359A (en) * 2020-04-23 2020-08-11 江南大学 Synthesis method of chiral copper sulfide super particle
CN111517359B (en) * 2020-04-23 2021-08-20 江南大学 Synthesis method of chiral copper sulfide super particle
CN113880128A (en) * 2020-07-01 2022-01-04 上海大学 Copper sulfide with chiral optical activity and preparation method thereof
CN111795958A (en) * 2020-07-14 2020-10-20 南宁师范大学 Specific detection of Ag+Preparation of CdSe quantum dot, detection method and application thereof
CN111795958B (en) * 2020-07-14 2022-09-09 南宁师范大学 Specific detection of Ag + Preparation of CdSe quantum dot, detection method and application thereof
CN112852405A (en) * 2021-01-07 2021-05-28 苏州国纳思新材料科技有限公司 Synthetic method of circular polarization luminous chiral quantum dot film
US12006461B2 (en) 2021-12-30 2024-06-11 Industrial Technology Research Institute Light color conversion material and light color conversion ink
CN115417384A (en) * 2022-07-11 2022-12-02 湖北大学 Preparation method of chiral tellurium (Te) nanocrystal material
CN115417384B (en) * 2022-07-11 2023-06-27 湖北大学 Preparation method of chiral tellurium (Te) nanocrystalline material

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