CN102086397A - Method for fast preparing soluble near infrared CdTe quantum dots covered with mercaptan in aqueous phase - Google Patents

Method for fast preparing soluble near infrared CdTe quantum dots covered with mercaptan in aqueous phase Download PDF

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CN102086397A
CN102086397A CN 201010583291 CN201010583291A CN102086397A CN 102086397 A CN102086397 A CN 102086397A CN 201010583291 CN201010583291 CN 201010583291 CN 201010583291 A CN201010583291 A CN 201010583291A CN 102086397 A CN102086397 A CN 102086397A
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cadmium
near infrared
quantum dot
cdte quantum
aqueous solution
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严秀平
吴伯岳
王荷芳
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Nankai University
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Nankai University
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Abstract

A method for fast preparing soluble near infrared CdTe quantum dots covered with mercaptan in aqueous phase relates to the preparation field of quantum dot. The method comprises the following steps: (a) adding NaBH4 or KBH4 and Te powder, adding deionized water to react at the room temperature under magnetic stirring and prepare NaHTe or KHTe solution; (b) preparing cadmium salt or cadmium oxide, cadmium hydroxide and cadmium sulfhydryl compound solution; (c) adding the solution obtained in the step (b) in a three-necked bottle, protecting with argon, stirring; (d) adding fresh and oxygen-free NaHTe or KHTe solution prepared in the step (a) in the three-necked bottle of the step (c); and (e) heating and refluxing to react and obtain the near infrared CdTe quantum dots. The method of the invention has simple operations, mild conditions and low cost and toxicity. The synthetized mercaptan modified CdTe quantum dots have good water-solubility and stability; and the fluorescence quantum yield is high and the emission spectrum can be adjusted in the near infrared region.

Description

Water prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast
[technical field]:
The present invention relates to the method for the preparation field of quantum dot, particularly water-soluble CdTe quantum dots.
[background technology]:
Quantum dot is a kind of semiconductor nanocrystal or crystallite, is made up of II-VI, III-V or IV-VI period element, and diameter is at the spherical material of 1-12 nanometer.What research was more at present is II-VI type quantum dots such as CdS, CdSe, CdTe, ZnS.These nanoparticles show the character different with macroscopic material, comprise high quantum emission productive rate, the size adjustable of emmission spectrum, narrow spectrum band etc.In addition, the controlling dimension size can be regulated the position of emmission spectrum.The character of quantum dot uniqueness is based on it self quantum effect, when particle size reaches nanometer scale, because the size confinement causes dimensional effect, quantum confined effect, macro quanta tunnel effect and surface effects, thereby derive nanometer system and have the normal sight system low-dimensional rerum natura different with microsystem, show many electronics and optical characteristics that are different from macroscopic material, it is had broad application prospects at aspects such as luminescent material, photosensors.
Adopt the synthetic quantum dot of chemical process to mainly contain Organometallic Chemistry method and aqueous phase synthesis method at present.
The Organometallic Chemistry method is a kind of chemical process of synthetic quantum dot commonly used.This method is normally under the anhydrous and oxygen-free condition, with TOP, TOPO etc. is part, organic coordination compound with component is a precursor, it is synthetic to reflux under 200～300 ℃ condition, the shortcoming that this method prepares quantum dot is the preparation condition harshness, the reactions steps complexity, the reagent cost height, toxicity is bigger; For further application, the quantum dot that the organic synthesis method need be made is transferred to water, and its complex steps, the quantum yield of the quantum dot aqueous solution that obtains after the processing and stability all reduce greatly.
In recent years, the direct quantum dot that synthesizes excellent property in the aqueous solution became the research focus.The ultimate principle of aqueous phase synthesis method is to add stablizer (as mercaptan compound etc.) in water, obtains nanoparticle by the water ion exchange reaction.Its reaction conditions gentleness, simple to operate, toxicity is little, cost is low.Because quantum dot is at the aqueous phase synthetic, has directly solved the water-soluble problem of nanoparticle.But water synthetic quantum dot has shortcomings such as emmission spectrum is wide, distribution of sizes is inhomogeneous, fluorescence quantum yield is low.
In II-VI type quanta point material, the fluorescence spectrum with it of CdTe quantum dot is narrow, and the variable range of fluorescent emission is wide, and quantum yield is higher, is subjected to extensive concern.The factor that influences CdTe quantum dot fluorescence transmitting site and intensity has a lot, for example the concentration of pH, heat-up time, reacting precursor and ratio etc. but simultaneously.On the other hand, because during water is synthetic, be subjected to the influence of the boiling point of aqueous solvent, reaction system is difficult to obtain enough energy makes the CdTe quantum dot can be with six narrower side's zinc sulphide crystal formations (wurtzite structure) to change from a cube zinc sulphide crystal formation (zinc blende structure); Thereby, by the synthetic near infrared CdTe quantum dot of ordinary method water, often need to expend the long period or to other heavy metal ion of wherein mixing.
Present method is utilized in the mercaptan compound structure, other functional groups except sulfydryl (for example amino and carboxyl) are as homing device, induce the non-directional growth of CdTe quantum dot in forming process by the ratio of mercaptan compound and cadmium ion in the regulation and control reacting precursor, thereby quickening above-mentioned crystal formation changes to such an extent that take place, shorten the reaction times, reach the simple purpose of synthesizing water-solubility near infrared CdTe quantum dot fast.
[summary of the invention]:
The purpose of this invention is to provide a kind of regulation and control mercaptan consumption that passes through, water prepares near infrared CdTe quantum dot method fast.
A kind of water prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, and this method comprises the steps:
(a) in closed reaction vessel, add NaBH 4Or KBH 4With the Te powder, add deionized water, normal-temperature reaction under the magnetic agitation makes colourless transparent liquid, i.e. the NaHTe of fresh anaerobic or the KHTe aqueous solution;
(b) preparation of the oxide compound of cadmium salt or cadmium, oxyhydroxide and the sulfhydryl compound aqueous solution: in beaker, add deionized water and the oxide compound of cadmium salt or cadmium, the aqueous solution of oxyhydroxide, regulate pH to 10.0～12.0 with the NaOH aqueous solution to sulfhydryl compound;
(c) add (b) step gained solution in the there-necked flask, argon shield is stirred;
(d) get the NaHTe or the KHTe aqueous solution of the fresh anaerobic of preparation in (a) step, join in (c) step;
(e) (d) step in the mixing solutions reflux, the reaction, can obtain near infrared CdTe quantum dot;
(f) get an amount of (e) step solution as observation fluorescence and characterization sample; Obtain water miscible near infrared CdTe quantum dot, the fluorescence maximum emission wavelength is in 650～800 nanometers.
In the described step (a), NaBH 4(KBH 4) with the mol ratio of Te powder be 2: 1～3: 1, the amount that adds deionized water is 1～5mL, the normal-temperature reaction time is 10～60 minutes under the magnetic agitation.
In the described step (b), the mol ratio of cadmium and sulfydryl be 1: 0.81～: 1.2.
In the described step (c), churning time is 20～30 minutes.
In the described step (d), get the NaHTe or the KHTe aqueous solution of the fresh anaerobic of preparation in (a) step, join in (c) step, make Cd: Te: the mol ratio of sulfydryl is 4: 0.5～1: 4～4.8.
In the described step (e), reflux, the reaction times is 60～90 minutes.
The oxide compound of cadmium salt or cadmium, oxyhydroxide are Cadmium oxide, Cadmium chloride fine powder, cadmium bromide, cadmium iodide, cadmium nitrate, cadmium chlorate, cadmium acetate, cadmium perchlorate, cadmium chlorate, Cadmium Sulphate, cadmium carbonate or cadmium hydroxide.
Sulfhydryl compound is one or more in halfcystine, Gelucystine, homocysteine, Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, mercaptoethanol, mercaptoethylamine, Methyl Thioglycolate, ethyl thioglycolate, mercapto-propionate, gsh or the sulfydryl oxysuccinic acid.
By to the kind of the sulfhydryl compound that added with and and the regulation and control of the ratio of cadmium, the spectrum that can be implemented near infrared region is adjustable.
Advantage of the present invention and effect: method provided by the invention does not need harsh equipment, condition; simple and safe operation; toxicity is little, cost is low; used plant and instrument is common equipment; as: induction stirring well heater, nitrogen protection device, there-necked flask, reflux condensing tube, thermometer and syringe, its production cost is low, and reaction conditions is simple; reflux gets final product, and does not have the exacting terms requirement.
Under alkaline condition,, realized that the fluorescence maximum emission wavelength is at the adjustable quantum dot of 650～800 nanometers at the stable near infrared CdTe quantum dot of aqueous phase controlledly synthesis by regulation and control mercaptan consumption.Other functional groups in the mercaptan compound except sulfydryl (for example amino and carboxyl) can induce the non-directional growth of CdTe quantum dot in forming process, thereby promote the crystal formation conversion of CdTe quantum dot, reduce the energy difference between quantum dot conduction band and the valence band, make the fluorescence emission spectrum of quantum dot that obvious red shift take place, reach the simple purpose of synthesizing water-solubility near infrared CdTe quantum dot fast.
[embodiment]:
Embodiment 1
(a) airtight, have in the reaction vessel of syringe needle, add 49mg (0.9mmol) KBH 4, the deionized water of 38mg (0.3mmol) Te powder and 3mL, normal-temperature reaction is 20 minutes under the magnetic agitation, makes colourless transparent liquid, i.e. the KHTe aqueous solution of fresh anaerobic;
(b) CdCl 2Preparation with the L-halfcystine aqueous solution: in beaker, add 34ml deionized water and 1mL (0.4mol L to 49mg (0.4mmol) stablizer L-halfcystine -1) CdCl 2The aqueous solution is used 1mol L -1The NaOH aqueous solution regulate pH to 10.0;
(c) add (b) in the there-necked flask of 50mL and go on foot the CdCl that contains for preparing 2With the aqueous solution of L-halfcystine, argon shield, stirred 30 minutes;
(d) the KHTe aqueous solution 0.5mL that gets the fresh anaerobic of preparation in (a) step joined in (c) step;
(e) (d) step in mixing solutions be heated to 100 ℃, back flow reaction 60～90 minutes;
(f) get CdTe solution that 5mL (e) step prepares as observation fluorescence.
Embodiment 2
(a) airtight, have in the reaction vessel of syringe needle, add 16mg (0.3mmol) KBH 4, the deionized water of 12.7mg (0.1mmol) Te powder and 1mL, normal-temperature reaction is 10 minutes under the magnetic agitation, makes colourless transparent liquid, i.e. the KHTe aqueous solution of fresh anaerobic;
(b) CdCl 2And the preparation of gsh (GSH) aqueous solution: in beaker, add 34mL deionized water and 1mL (0.4mol L to 122.6mg (0.4mmol) stablizer gsh -1) CdCl 2The aqueous solution is used 1mol L -1The NaOH aqueous solution regulate pH to 10.0;
(c) add (b) in the there-necked flask of 100mL and go on foot the CdCl that contains for preparing 2With the aqueous solution of gsh, argon shield, stirred 20 minutes;
(d) the KHTe aqueous solution 1mL with the fresh anaerobic of preparation in (a) step all joined in (c) step;
(e) (d) step in mixing solutions be heated to 100 ℃, back flow reaction 30 minutes;
(f) get CdTe solution that 5mL (e) step prepares as the observation fluorescent samples.
Embodiment 3
(a) airtight, have in the reaction vessel of syringe needle, add 49mg (0.9mmol) KBH 4, the deionized water of 38mg (0.3mmol) Te powder and 3mL, normal-temperature reaction is 20 minutes under the magnetic agitation, makes colourless transparent liquid, i.e. the KHTe aqueous solution of fresh anaerobic;
(b) CdCl 2Preparation with the thiohydracrylic acid aqueous solution: in beaker, add 34ml deionized water and 1mL (0.4mol L to 35 μ L (0.4mmol) stablizer thiohydracrylic acids -1) CdCl 2The aqueous solution is used 1mol L -1The NaOH aqueous solution regulate pH to 10.0;
(c) add (b) in the there-necked flask of 50mL and go on foot the CdCl that contains for preparing 2With the aqueous solution of thiohydracrylic acid, argon shield, stirred 30 minutes;
(d) the KHTe aqueous solution 0.5mL that gets the fresh anaerobic of preparation in (a) step joined in (c) step;
(e) (d) step in mixing solutions be heated to 100 ℃, back flow reaction 60～90 minutes;
(f) get CdTe solution that 5mL (e) step prepares as observation fluorescence.
Embodiment 4
(a) airtight, have in the reaction vessel of syringe needle, add 49mg (0.9mmol) KBH 4, the deionized water of 38mg (0.3mmol) Te powder and 3mL, normal-temperature reaction is 20 minutes under the magnetic agitation, makes colourless transparent liquid, i.e. the KHTe aqueous solution of fresh anaerobic;
(b) CdCl 2Preparation with the Thiovanic acid aqueous solution: in beaker, add 34ml deionized water and 1mL (0.4mol L to 28 μ L (0.4mmol) stablizer Thiovanic acids -1) CdCl 2The aqueous solution is used 1mol L -1The NaOH aqueous solution regulate pH to 10.0;
(c) add (b) in the there-necked flask of 50mL and go on foot the CdCl that contains for preparing 2With the aqueous solution of Thiovanic acid, argon shield, stirred 30 minutes;
(d) the KHTe aqueous solution 0.5mL that gets the fresh anaerobic of preparation in (a) step joined in (c) step;
(e) (d) step in mixing solutions be heated to 100 ℃, back flow reaction 60～90 minutes;
(f) get CdTe solution that 5mL (e) step prepares as observation fluorescence.
Embodiment 5
(a) airtight, have in the reaction vessel of syringe needle, add 49mg (0.9mmol) KBH 4, the deionized water of 38mg (0.3mmol) Te powder and 3mL, normal-temperature reaction is 20 minutes under the magnetic agitation, makes colourless transparent liquid, i.e. the KHTe aqueous solution of fresh anaerobic;
(b) CdCl 2Preparation with the N-acetyl-L-cysteine aqueous solution: in beaker, add 34ml deionized water and 1mL (0.4mol L to 65.3mg (0.4mmol) stablizer N-acetyl-L-cysteine -1) CdCl 2The aqueous solution is used 1mol L -1The NaOH aqueous solution regulate pH to 10.0;
(c) add (b) in the there-necked flask of 50mL and go on foot the CdCl that contains for preparing 2With the aqueous solution of N-acetyl-L-cysteine, argon shield, stirred 30 minutes;
(d) the KHTe aqueous solution 0.5mL that gets the fresh anaerobic of preparation in (a) step joined in (c) step;
(e) (d) step in mixing solutions be heated to 100 ℃, back flow reaction 60～90 minutes;
(f) get CdTe solution that 5mL (e) step prepares as observation fluorescence.

Claims (8)

1. a water prepares the method for the solubility near infrared CdTe quantum dot that mercaptan coats fast, it is characterized in that this method comprises the steps:
(a) in closed reaction vessel, add NaBH 4Or KBH 4With the Te powder, add deionized water, normal-temperature reaction under the magnetic agitation makes colourless transparent liquid, i.e. the NaHTe of fresh anaerobic or the KHTe aqueous solution;
(b) preparation of the oxide compound of cadmium salt or cadmium, oxyhydroxide and the sulfhydryl compound aqueous solution: in beaker, add deionized water and the oxide compound of cadmium salt or cadmium, the aqueous solution of oxyhydroxide, regulate pH to 10.0～12.0 with the NaOH aqueous solution to sulfhydryl compound;
(c) add (b) step gained solution in the there-necked flask, argon shield is stirred;
(d) get the NaHTe or the KHTe aqueous solution of the fresh anaerobic for preparing in (a) step, join in (c) step;
(e) (d) the mixing solutions reflux in the step, reaction can obtain near infrared CdTe quantum dot;
(f) get (e) step solution as observation fluorescence and characterization sample; Obtain water miscible near infrared CdTe quantum dot, the fluorescence maximum emission wavelength is in 650～800 nanometers.
2. water according to claim 1 prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, it is characterized in that, and in the described step (a), NaBH 4(KBH 4) with the mol ratio of Te powder be 2: 1～3: 1, the amount that adds deionized water is 1～5mL, the normal-temperature reaction time is 10～60 minutes under the magnetic agitation.
3. water according to claim 1 prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, it is characterized in that in the described step (b), the mol ratio of cadmium and sulfydryl is 1: 0.8～1: 1.2.
4. water according to claim 1 prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, it is characterized in that in the described step (c), churning time is 20～30 minutes.
5. water according to claim 1 prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, it is characterized in that, in the described step (d), get the NaHTe or the KHTe aqueous solution of the fresh anaerobic of preparation in (a) step, join in (c) step, make Cd: Te: the mol ratio of sulfydryl is 4: 0.5～1: 4～4.8.
6. water according to claim 1 prepares the method for the solubility near infrared CdTe quantum dot of mercaptan coating fast, it is characterized in that, and in the described step (e), reflux, the reaction times is 60～90 minutes.
7. synthetic method according to claim 1, it is characterized in that the oxide compound of cadmium salt or cadmium, oxyhydroxide are Cadmium oxide, Cadmium chloride fine powder, cadmium bromide, cadmium iodide, cadmium nitrate, cadmium chlorate, cadmium acetate, cadmium perchlorate, cadmium chlorate, Cadmium Sulphate, cadmium carbonate or cadmium hydroxide.
8. synthetic method according to claim 1, it is characterized in that sulfhydryl compound is one or more in halfcystine, Gelucystine, homocysteine, Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, mercaptoethanol, mercaptoethylamine, Methyl Thioglycolate, ethyl thioglycolate, mercapto-propionate, gsh or the sulfydryl oxysuccinic acid.
CN 201010583291 2010-12-10 2010-12-10 Method for fast preparing soluble near infrared CdTe quantum dots covered with mercaptan in aqueous phase Pending CN102086397A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304361A (en) * 2011-07-04 2012-01-04 江苏大学 Aqueous synthesis method of cadmium telluride quantum dot with hydrophobic surface
CN102719254A (en) * 2012-06-11 2012-10-10 广西师范学院 Preparation method of water-soluble N-acetyl-L-cysteic acid-modified CdTe/CdS core/shell quantum dot
CN102796525A (en) * 2012-08-17 2012-11-28 徐州医学院 Water-phase preparation method of acidity-sensitive CdTe quantum dot modified by double stabilizers
CN103897700A (en) * 2014-03-28 2014-07-02 东华大学 Preparation method of L-cysteine/thiohydracrylic acid modified CdTe quantum dot
CN110684534A (en) * 2019-09-19 2020-01-14 杭州电子科技大学 Method for preparing near-infrared cadmium telluride quantum dots in hydrothermal mode

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CN101148590A (en) * 2007-11-09 2008-03-26 南开大学 Water-phase preparation method for CdTe quantum point modified by cyclodextrin
CN101250403A (en) * 2008-02-28 2008-08-27 上海交通大学 Method for synthesizing water-soluble long-chain mercapto compound coated cadmium telluride quantum dot

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CN101148590A (en) * 2007-11-09 2008-03-26 南开大学 Water-phase preparation method for CdTe quantum point modified by cyclodextrin
CN101250403A (en) * 2008-02-28 2008-08-27 上海交通大学 Method for synthesizing water-soluble long-chain mercapto compound coated cadmium telluride quantum dot

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304361A (en) * 2011-07-04 2012-01-04 江苏大学 Aqueous synthesis method of cadmium telluride quantum dot with hydrophobic surface
CN102304361B (en) * 2011-07-04 2013-10-23 江苏大学 Aqueous synthesis method of cadmium telluride quantum dot with hydrophobic surface
CN102719254A (en) * 2012-06-11 2012-10-10 广西师范学院 Preparation method of water-soluble N-acetyl-L-cysteic acid-modified CdTe/CdS core/shell quantum dot
CN102719254B (en) * 2012-06-11 2014-01-08 广西师范学院 Preparation method of water-soluble N-acetyl-L-cysteic acid-modified CdTe/CdS core/shell quantum dot
CN102796525A (en) * 2012-08-17 2012-11-28 徐州医学院 Water-phase preparation method of acidity-sensitive CdTe quantum dot modified by double stabilizers
CN103897700A (en) * 2014-03-28 2014-07-02 东华大学 Preparation method of L-cysteine/thiohydracrylic acid modified CdTe quantum dot
CN103897700B (en) * 2014-03-28 2015-11-18 东华大学 The preparation method of the CdTe quantum that a kind of Cys/thiohydracrylic acid is modified
CN110684534A (en) * 2019-09-19 2020-01-14 杭州电子科技大学 Method for preparing near-infrared cadmium telluride quantum dots in hydrothermal mode
CN110684534B (en) * 2019-09-19 2022-02-15 杭州电子科技大学 Method for preparing near-infrared cadmium telluride quantum dots in hydrothermal mode

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Application publication date: 20110608