CN101864296A - Preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots - Google Patents

Preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots Download PDF

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CN101864296A
CN101864296A CN201010199804A CN201010199804A CN101864296A CN 101864296 A CN101864296 A CN 101864296A CN 201010199804 A CN201010199804 A CN 201010199804A CN 201010199804 A CN201010199804 A CN 201010199804A CN 101864296 A CN101864296 A CN 101864296A
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water
thiocarbamide
coo
dehydrated alcohol
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赵肃清
赵斌
张焜
刘端
苏娟
黎文聪
叶建斌
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Guangdong University of Technology
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Guangdong University of Technology
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Abstract

The invention relates to a preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots, which comprises the following steps: firstly, using Zn(CH3COO)2.2H2O as zinc sources, Cd(CH3COO)2.2H2O as cadmium sources and absolute ethyl alcohol as solvents for carrying back flowing for 3h in water bath under the condition of 80 DEG C; adding the PVP K-30 as stabilizing agents for preparing precursor solution; then, adding absolute ethyl alcohol solution of thiourea, LiOH.H2O and Eu(NO3)3 for carrying out water bath reaction for 1h at 50 DEG C to obtain the thiourea modified Cd doping ZnO water-soluble quantum dots. The method of the invention has the advantages of simplicity, easy implementation, mild reaction condition and simple equipment. The prepared quantum dots have high stability, good dispersivity, uniform grain diameter distribution and high fluorescence quantum dot efficiency.

Description

A kind of preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots
Technical field
The present invention relates to field of nanometer technology, be specifically related to a kind of preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots.
Background technology
Quantum dot is called semiconductor nanocrystal again, is a kind of by the elementary composition nano particle of II-VI or III-V family, the about 1～100nm of diameter.Under the inducing of exciting light, quantum dot can produce fluorescence.That research is maximum at present mainly is CdX (X=S, Se, Te), also has the nano particle of some composite structures and multilayered structure.From the end of the seventies in last century, because quantum dot has the attention that unique optics and electrical properties have just caused physicist, chemist, electronic engineering scholar.In recent years, comparatively outstanding with ZnO especially, ZnO had excellent optics, electrical properties, it is a kind of semiconductor material with wide forbidden band of direct band gap, energy gap is 3.2eV under its room temperature, and exciton bind energy is a kind of material that is suitable for carrying out under the room temperature condition exciton emission up to 60meV.The ZnO quantum dot can produce tangible quantum confined effect because of its small size, causes and the distinct light of body material ZnO, electricity, magnetic effect, becomes one of focus of people's research.
In organic solvent system, prepared at present the nano particle quantum dot of many kinds of II-VI or III-V group composition, and the quantum dot nano-particle of core-shell type, Yao Jianxi etc. are at " Journal of Inorganic Materials ", make surperficial modifier with thiocarbamide in 2 phases, 445～450 pages of the preparations of 2003 18 volumes with polyvinylpyrrolidone thiourea modified Cd S nanoparticle, and it is even to be with PVP K-30 that stablizer has synthesized size distribution in aqueous ethanolic solution, the CdS nano particle of stable performance.And as the preparation of CdTe and CdTe/CdS quantum dot nano-particle, but the quantum dot experimental implementation complexity of this method preparation, agents useful for same is inflammable and explosive, cost is high and repeated shortcoming such as bad.Therefore, to be subjected to a certain degree restriction being used for the biomedical research field.
Also have in the prior art a kind of as crops etc. at " high chemical journal ", the preparation of the water-soluble ZnO quantum dot of being delivered on 2007 28 volume 2246～2251 pages of 12 phases and the research of optical property thereof is characterized in that with the 3-mercaptopropyltriethoxysilane ZnO being carried out depositing SiO after the finishing 2, prepare water-soluble SiO 2The quantum dot of clading ZnO, thus make the intensity of exciton fluorescence emission peak at 362nm place improve 4 times nearly.Because mercapto functional group has been introduced on the surface, the water-soluble obvious raising of quantum dot, stability strengthens, even also can not reunite under higher salt concn.By the change condition, prepared the blue luminescence quantum dot of emission wavelength at 420nm.In addition, the existing patent No. is 200810060102.7 " methods of phosphorus doping growing ZnO quanta dots ", its goal of the invention mainly is the electric property of wishing can regulate by the introducing of phosphorus ZnO film, and a kind of method that adopts Metalorganic Chemical Vapor Deposition to prepare phosphorus doping ZnO quantum dot is provided simultaneously.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots is provided, make it under the reaction conditions of gentleness, acquisition has the adulterated ZnO quantum dot of water-soluble Cd of good dispersiveness, even particle size distribution and high fluorescence efficiency, lays a good foundation for being applied in the biomarker aspect later on.
The present invention realizes by following technological method, at first uses Zn (CH 3COO) 22H 2O is the zinc source, Cd (CH 3COO) 22H 2O is the cadmium source, and dehydrated alcohol is a solvent, and behind backflow 3h under 80 ℃ of conditions of water-bath, adding PVP K-30 is stablizer, makes precursor solution, and then adds thiocarbamide, LiOHH 2O and Eu (NO 3) 350 ℃ of water-bath 1h of ethanol solution, obtain thiourea modified Cd doping ZnO water-soluble quantum dots.
The inventive method concrete steps are as follows:
(1) with 5mmolZn (CH 3COO) 22H 2O and 5mmolCd (CH 3COO) 22H 2O is blended in the ethanol solution of 20ml, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid;
(2) get phegma 5ml in (1), add PVP K-30, make that the mass concentration of PVP K-30 is 4mg/ml;
(3) take by weighing thiocarbamide and be dissolved in the 10ml dehydrated alcohol, the thiocarbamide ethanol solution is joined in (2), stirring makes that thiocarbamide ethanol solution mass concentration is 8mg/ml～100mg/ml;
(4) take by weighing 0.1180gLiOHH 2O adds in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Add in the 5ml dehydrated alcohol, stir accelerate dissolution, above-mentioned LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise in the vigorous stirring (3), and 50 ℃ of reactions of water-bath 1h makes quantum dot fluorescence body colloidal solution;
(5) add isopyknic normal hexane purifying in (4), stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly.
The invention has the beneficial effects as follows:
The prepared product of this patent is to adopt thiourea modified ZnO quantum dot in non-water dilute solution, while doping metals Cd, thereby improved the luminous efficiency of ZnO quantum dot greatly, and nano particle diameter is evenly distributed after thiourea modified, the grain diameter size also obviously diminishes, and grain size is about 20nm.Therefore the water miscible quantum dot of this patent preparation has significantly different with the quantum dot of prior art for preparing.
From present development trend, the research and the range of application of quantum dot nano-particle are more and more wider, particularly demonstrate good prospects for application at biomedicine field.Therefore develop good reproducibility, can scale operation, that optical property is stable, preparation condition is simple, spectroscopic properties is excellent, the quantum dot of high fluorescence efficiency seems is very urgent.
Description of drawings
Fig. 1 is ZnO:Li emmission spectrum figure.
Wherein: excitation wavelength lambda=365nm.
Fig. 2 is that ZnO:Li mixes Cd emmission spectrum figure.
Wherein: excitation wavelength lambda=365nm.
Fig. 3 is the emmission spectrum figure of the content of thiocarbamide to the quantum dot light emitting Effect on Performance.
Wherein: excitation wavelength lambda=365nm,
1. the concentration of thiocarbamide is 8mg/ml,
2. the concentration of thiocarbamide is 16mg/ml,
3. the concentration of thiocarbamide is 32mg/ml,
4. the concentration of thiocarbamide is 64mg/ml,
5. the concentration of thiocarbamide is 100mg/ml.
In the preparation of product of the present invention, all adopt reagent commonly used, such as Zn (CH3COO) 2·2H 2O (zinc acetate), Cd (CH3COO) 2·2H 2O (cadmium acetate), Eu (NO3) 3With PVP K-30 (PVP K-30), H2NCSNH 2Deng no inflammable and explosive danger, and with low cost; Preparation temperature is generally at 50～80 ℃, and one kettle way can be finished, and is simple to operation, easily-controlled experimental conditions. The quantum dot optics stable in properties that what is more important prepares with this type of reagent, fluorescence efficiency is efficient. Therefore, the invention provides the effective ways of a kind of on a large scale repeatability preparation. In the time of can finding not mix Cd from detection analysis result Fig. 1, Fig. 2 of this experiment preparation, ZnO quantum dot emission main peak is positioned near the 433nm, and luminous intensity is not strong, may be because of low the causing of absorption efficiency to exciting light sources; But the red shift of emission main peak is near 548nm behind the doping Cd, and luminous intensity increases obviously, may be because the radius of Cd and Zn ion is close, enters into easily the lattice of ZnO, strengthens the energy transfer efficiency of ZnO quantum dot, and luminous intensity is strengthened.
The present invention can pass through luminescent properties such as Fig. 3 of the content influence ZnO quantum dot of change thiocarbamide, under excitation source wavelength 365nm, and the introducing of thiocarbamide, emission spectrum generation blue shift, luminous intensity also obviously strengthens; And along with the gradually increase of thiocarbamide content, the emission spectrum blue-shifted phenomenon is more and more obvious, and luminous intensity is also more and more stronger; But when the content of thiocarbamide was higher than 64mg/ml, luminous intensity descended gradually. The quantum dot that makes by this experiment has high fluorescence efficiency, and the nano particle diameter advantage such as be evenly distributed is for further laying a good foundation in the application aspect the biomarker.
Embodiment
Embodiment 1
1. get 1.0975gZn (CH 3COO) 22H 2O and 1.3326gCd (CH 3COO) 22H 2O places the 20ml dehydrated alcohol, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid.
2. get 5mlZn (CH 3COO) 22H 2O and Cd (CH 3COO) 22H 2The O phegma adds PVP K-30, makes that the mass concentration of PVPK-30 is 4mg/ml, stirring and dissolving.
3. take by weighing the 0.12g thiocarbamide and place the dehydrated alcohol of 10ml to dissolve, join the ethanol solution of thiocarbamide 2. again, stir, make that thiocarbamide ethanol solution mass concentration is 8mg/ml.
4. take by weighing 0.1180gLiOHH in addition 2O joins in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Join in the 5ml dehydrated alcohol, stir accelerate dissolution.With LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise to 50 ℃ of reactions of 3. middle water-bath 1h of vigorous stirring, makes quantum dot fluorescence body colloidal solution.
5. get isopyknic normal hexane and join in the quantum dot fluorescence liquid solution, stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly, preserves stand-by.
Embodiment 2
1. get 1.0975gZn (CH 3COO) 22H 2O and 1.3326gCd (CH 3COO) 22H 2O places the 20ml dehydrated alcohol, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid.
2. get 5mlZn (CH 3COO) 22H 2O and Cd (CH 3COO) 22H 2The O phegma adds PVP K-30, makes that the mass concentration of PVPK-30 is 4mg/ml, stirring and dissolving.
3. take by weighing the 0.24g thiocarbamide and place the dehydrated alcohol of 10ml to dissolve, join the ethanol solution of thiocarbamide 2. again, stir, make that thiocarbamide ethanol solution mass concentration is 16mg/ml.
4. take by weighing 0.1180gLiOHH in addition 2O joins in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Join in the 5ml dehydrated alcohol, stir accelerate dissolution.With LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise to 50 ℃ of reactions of 3. middle water-bath 1h of vigorous stirring, makes quantum dot fluorescence body colloidal solution.
5. get isopyknic normal hexane and join in the quantum dot fluorescence liquid solution, stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly, preserves stand-by.
Embodiment 3
1. get 1.0975gZn (CH 3COO) 22H 2O and 1.3326gCd (CH 3COO) 22H 2O places the 20ml dehydrated alcohol, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid.
2. get 5mlZn (CH 3COO) 22H 2O and Cd (CH 3COO) 22H 2The O phegma adds PVP K-30, makes that the mass concentration of PVPK-30 is 4mg/ml, stirring and dissolving.
3. take by weighing the 0.48g thiocarbamide and place the dehydrated alcohol of 10ml to dissolve, join the ethanol solution of thiocarbamide 2. again, stir, make that thiocarbamide ethanol solution mass concentration is 32mg/ml.
4. take by weighing 0.1180gLiOHH in addition 2O joins in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Join in the 5ml dehydrated alcohol, stir accelerate dissolution.With LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise to 50 ℃ of reactions of 3. middle water-bath 1h of vigorous stirring, makes quantum dot fluorescence body colloidal solution.
5. get isopyknic normal hexane and join in the quantum dot fluorescence liquid solution, stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly, preserves stand-by.
Embodiment 4
1. get 1.0975gZn (CH 3COO) 22H 2O and 1.3326gCd (CH 3COO) 22H 2O places the 20ml dehydrated alcohol, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid.
2. get 5mlZn (CH 3COO) 22H 2O and Cd (CH 3COO) 22H 2The O phegma adds PVP K-30, makes that the mass concentration of PVPK-30 is 4mg/ml, stirring and dissolving.
3. take by weighing the 0.96g thiocarbamide and place the dehydrated alcohol of 10ml to dissolve, join the ethanol solution of thiocarbamide 2. again, stir, make that thiocarbamide ethanol solution mass concentration is 64mg/ml.
4. take by weighing 0.1180gLiOHH in addition 2O joins in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Join in the 5ml dehydrated alcohol, stir accelerate dissolution.With LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise to 50 ℃ of reactions of 3. middle water-bath 1h of vigorous stirring, makes quantum dot fluorescence body colloidal solution.
5. get isopyknic normal hexane and join in the quantum dot fluorescence liquid solution, stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly, preserves stand-by.
Embodiment 5
1. get 1.0975gZn (CH 3COO) 22H 2O and 1.3326gCd (CH 3COO) 22H 2O places the 20ml dehydrated alcohol, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid.
2. get 5mlZn (CH 3COO) 22H 2O and Cd (CH 3COO) 22H 2The O phegma adds PVP K-30, makes that the mass concentration of PVPK-30 is 4mg/ml, stirring and dissolving.
3. take by weighing the 1.50g thiocarbamide and place the dehydrated alcohol of 10ml to dissolve, join the ethanol solution of thiocarbamide 2. again, stir, make that thiocarbamide ethanol solution mass concentration is 100mg/ml.
4. take by weighing 0.1180gLiOHH in addition 2O joins in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Join in the 5ml dehydrated alcohol, stir accelerate dissolution.With LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise to 50 ℃ of reactions of 3. middle water-bath 1h of vigorous stirring, makes quantum dot fluorescence body colloidal solution.
5. get isopyknic normal hexane and join in the quantum dot fluorescence liquid solution, stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly, preserves stand-by.

Claims (2)

1. the preparation method of a thiourea modified Cd doping ZnO water-soluble quantum dots is characterized in that: at first use Zn (CH 3COO) 22H 2O is the zinc source, Cd (CH 3COO) 22H 2O is the cadmium source, and dehydrated alcohol is a solvent, and behind backflow 3h under 80 ℃ of conditions of water-bath, adding PVP K-30 is stablizer, makes precursor solution, and then adds thiocarbamide, LiOHH 2O and Eu (NO 3) 350 ℃ of water-bath 1h of ethanol solution, obtain thiourea modified Cd doping ZnO water-soluble quantum dots.
2. preparation method according to claim 1 is characterized in that: its concrete steps are as follows:
(1) with 5mmolZn (CH 3COO) 22H 2O and 5mmolCd (CH 3COO) 22H 2O is blended in the ethanol solution of 20ml, and at 80 ℃ of following backflow 3h, the solution after the backflow is colourless transparent liquid;
(2) get phegma 5ml in (1), add PVP K-30, make that the mass concentration of PVP K-30 is 4mg/ml;
(3) take by weighing thiocarbamide and be dissolved in the 10ml dehydrated alcohol, the thiocarbamide ethanol solution is joined in (2), stirring makes that thiocarbamide ethanol solution mass concentration is 8mg/ml～100mg/ml;
(4) take by weighing 0.1180gLiOHH 2O adds in the 10ml dehydrated alcohol, 0.2300g Eu (NO 3) 3Add in the 5ml dehydrated alcohol, stir accelerate dissolution, above-mentioned LiOHH 2O, Eu (NO 3) 3Solution successively is added drop-wise in the vigorous stirring (3), and 50 ℃ of reactions of water-bath 1h makes quantum dot fluorescence body colloidal solution;
(5) add isopyknic normal hexane purifying in (4), stirring is left standstill, and the centrifugal 10min of 6000r/min removes supernatant liquor, uses anhydrous alcohol solution again, will precipitate lyophilize after twice repeatedly.
CN201010199804A 2010-06-11 2010-06-11 Preparation method of thiourea modified Cd doping ZnO water-soluble quantum dots Pending CN101864296A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105478148A (en) * 2014-09-15 2016-04-13 中国科学院理化技术研究所 Doped quantum dot catalyst, preparation method thereof, hydrogen production system containing doped quantum dot catalyst and hydrogen production method
CN106566535A (en) * 2016-11-04 2017-04-19 广东南海启明光大科技有限公司 Preparation method of water soluble Cd-doped ZnO/ZnS core-shell quantum dot
CN109292812A (en) * 2018-12-04 2019-02-01 淮阴工学院 The preparation method of the monodispersity ZnO quantum dot hydrosol
CN112939062A (en) * 2021-04-19 2021-06-11 陕西科技大学 Rodlike Zn0.7Cd0.3Preparation method of S material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
黄凤华: "硫脲表面修饰的ZnS:Cd纳米晶的合成及表征", 《分子科学学报》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105478148A (en) * 2014-09-15 2016-04-13 中国科学院理化技术研究所 Doped quantum dot catalyst, preparation method thereof, hydrogen production system containing doped quantum dot catalyst and hydrogen production method
CN106566535A (en) * 2016-11-04 2017-04-19 广东南海启明光大科技有限公司 Preparation method of water soluble Cd-doped ZnO/ZnS core-shell quantum dot
CN109292812A (en) * 2018-12-04 2019-02-01 淮阴工学院 The preparation method of the monodispersity ZnO quantum dot hydrosol
CN112939062A (en) * 2021-04-19 2021-06-11 陕西科技大学 Rodlike Zn0.7Cd0.3Preparation method of S material
CN112939062B (en) * 2021-04-19 2022-08-05 陕西科技大学 Rodlike Zn 0.7 Cd 0.3 Preparation method of S material

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Application publication date: 20101020