CN1553476A - Method for preparing semiconductor quantum-point material by low-temperature solvent method - Google Patents
Method for preparing semiconductor quantum-point material by low-temperature solvent method Download PDFInfo
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Abstract
In the invention, inorganic salt is as raw material including cadmium acetate, cadmium chloride or cadmium oxide. Solvent in high boiling point and strong polarity is selected as reaction medium. Surface-active agents: oleic acid, phospholipid, lecithin and polyvinyl alcohol pyridine are selected to modify surface of quantum point. Dispersed single material of semiconductor quantum point in adjustable size can be obtained through reaction in glass flask under lower reaction temperature 1l0 deg.C - 170 deg.C. Features of the invention are: easy to obtain all raw materials, low cost and toxicity, even dispersed single material of semiconductor quantum point in adjustable size.
Description
Technical field
What the present invention relates to is a kind of semiconductor-quantum-point preparation methods, and particularly a kind of low-temperature solvent legal system is equipped with the method for semiconductor-quantum-point material.Belong to field of material preparation.
Background technology
Quantum dot refer in particular to radius less than or near the semiconductor nanoparticle of exciton Bohr radius, quantum size effect that it is unique and skin effect make it to become the desirable iridescent group of wavelength-brightness multichannel transmission system.With respect to traditional organic fluorescent dye, semiconductor-quantum-point emission spectrum of uniform size is narrow and have size " tuning " characteristic, can excite different quantum dots with single wavelength, the fluorescence quantum yield height, good stability has advantages such as good biocompatibility.And the abundant optical characteristics of quantum dot and progressively be expected in recent years in research huge aspect the biology sign and using value.By strict control growing condition, or by certain physical or chemical means screening, just can obtain narrow size distribution is the quantum dot that emission wavelength is determined.Utilize the different of the color of quantum dot and light intensity, after combination, can " identify " several ten thousand and even biomolecule up to a million, this is to the data acquisition of aspect researchs such as genomics and proteomics, the improvement and the innovation of processing method, and study biological macromolecular celluar localization, interaction and dynamic change, realize that " coding " to large biological molecule reaches " inquiry " etc. and have meaning.
At present, popular in the world quantum dot preparation method is to be solvent with trioctylphosphine oxide (TOPO) (TOPO) with chelation, under high temperature (300C) condition, and organo-metallic compound (Cd (CH
3)
2) decomposition prepare.Reaction needs to carry out under anaerobic, anhydrous condition.But, in this is synthetic, there is severe reaction conditions, the reaction temperature height, the raw material organo-metallic compound is inflammable, and is explosive, and toxicity is big, and shortcomings such as solvent costliness are promoted the use of thereby limited it.Find by literature search, (JACS) (Vol 123 at " Journal of American Chemical Society " for people such as Peng, 2001) " Formation of High-QualityCdTe; CdSe; and CdS Nanocrystals Using CdO as precursor " (with CdO is that presoma prepares high-quality CdTe, and CdSe and CdS are nanocrystalline) literary composition of delivering on the P183-184, this article improves popular synthetic method, use CdO, CdCO
3The substituted metal organic compound, under the inert gas shielding condition, (300 ℃) inject reaction precursor body (TOPSe and CdO) and have the reaction dissolvent (TOPO) that the huge legendary turtle cooperation is used under higher reaction temperature, and a step has been synthesized the quantum dot of high fluorescent yield.Although used the inorganic salts presoma of low toxicity in this reaction, but still used expensive solvent, reaction temperature is higher, reaction condition and required consersion unit harshness.
Summary of the invention
The objective of the invention is at deficiency of the prior art and defective, provide a kind of low-temperature solvent legal system to be equipped with the method for semiconductor-quantum-point material, reaction temperature is lower, make reaction raw materials with inorganic salts, and adopt new surfactant that the quantum dot surface is modified, this method cost is low, materials safety is easy to get, reaction condition gentleness, technology controlling and process convenient, just can obtain the adjustable list of a series of performances easily by conditioned reaction temperature, reaction medium and reaction time and disperse the semiconductor-quantum-point material, be convenient to large-scale industrial production and environmental friendliness.
The present invention is achieved by the following technical solutions, the present invention with inorganic salts as raw material, raw material is cadmium acetate, caddy or the cadmium oxide that contains cadmium ion, the solvent of selecting higher boiling point, strong polarity for use is as reaction medium, select for use surfactant oleic acid, phosphatide, lecithin, polyvinylpyridine that the surface of quantum dot is modified, in the glass flask reaction vessel, lower reaction temperature is reacted 3min～60min down for 110～170 ℃, can obtain the humorous and monodispersed semiconductor-quantum-point material of size adjustable.
Below the inventive method is done further to limit, method step is as follows:
(1) with inorganic cadmium salt and surfactant by weight 1: 1, under 110～170 ℃ of heating conditions that relax, be dissolved in the organic solvent diphenyl ether, N, in dinethylformamide or the N-methyl pyrrolidone, cooling obtains precursor A.
(2) under ultrasound condition, with metal selenium powder (Cd
2+/ Se
2-=1: 2) be dissolved in the tri octyl phosphine, obtain precursor B.
(3) at room temperature, fully mix precursor A and precursor B and obtain reacting storing solution C.
(4) will be heated to 110 ℃～170 ℃ of reaction temperatures as the organic solvent of reaction medium, quick dropwise reaction storing solution C under intense agitation, according to the size of needed particle diameter, reaction time 3min～60min.
(5) under stirring condition, the stopped reaction of lowering the temperature rapidly.The reactant liquor that obtains adds double methyl alcohol precipitating, through the centrifugal solid product that obtains.
(6) solid product is dispersed in organic solvent-normal hexane, stores in chloroform or the toluene, according to the size of quantum dot, obtains yellow solution to dark brown red, can obtain the semiconductor-quantum-point material.
Selected surfactant is oleic acid, phosphatide, lecithin or polyvinylpyridine, can choose according to the performance of material requested.
Reaction raw materials of the present invention is an inorganic cadmium salt but not inflammable, explosive, the metallo-organic compound that toxicity is big.Reaction condition is relatively gentleer, and reaction needn't be anhydrous, and anaerobic is carried out under the condition of inert gas shielding; Reaction temperature is lower, at 110～170 ℃, can regulate according to the particle size difference of material requested.The present invention can be between 3min～60min adjusting reaction time, obtain the semiconductor-quantum-point particle diameter between 1.8nm～3.9nm, optical property is tunable (a series of semiconductor-quantum-point materials of emission wavelength 500nm～599nm).Choosing different solvents is the fluorescence property of the quantum dot that obtains of scalable as reaction medium.The solvent of choosing comprises the boiling point height, the diphenyl ether that polarity is strong, N, dinethylformamide, N-methyl pyrrolidone.
Compared with prior art, all raw material that the present invention uses all obtains easily, and raw material are not only cheap but also toxicity is low.In the process of using these raw materials, do not need special consersion unit and protective condition, greatly reduce the cost of reaction.By simple change reaction temperature, reaction medium, surfactant just can obtain the semiconductor-quantum-point material of the humorous even size distribution of adjustable grain at an easy rate.For the large-scale production and the practical application of quanta point material provides feasible and preparation method environmental protection.Can prepare other II-VI family, the single semiconductor-quantum-point material that disperses of size adjustable by the inventive method.
Embodiment
Provide following examples in conjunction with content of the present invention:
Embodiment 1
With the 0.267g cadmium acetate, 1ml oleic acid, the 4ml diphenyl ether adds in the 150ml three-neck flask, is heated to 170 ℃, and stirring and dissolving also kept 30 minutes under 170 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add the 10ml diphenyl ether in three-neck flask, nitrogen protection is heated to 170 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 3 minutes to 45 minutes, performance test is carried out in sampling.
Reacted 3 minutes, and obtained particle size 1.8nm, its ultraviolet absorption peak is positioned at 472nm, and the fluorescence emission peak wavelength is positioned at 500nm; Reacted 11 minutes, and obtained particle size 2.1nm, its ultraviolet absorption peak is positioned at 499nm, and the fluorescence emission peak wavelength is positioned at 526nm; Reacted 45 minutes, and obtained particle size 3.1nm, its ultraviolet absorption peak is positioned at 540nm, and the fluorescence emission peak wavelength is positioned at 562nm.Narrow half-peak breadth (30nm) illustrates that the CdSe quanta point material that obtains is monodispersed.The position of diffraction maximum is consistent with the standard spectrogram of cube type CdSe in the X-ray diffractogram of resultant CdSe quanta point material, and the broadening of diffraction maximum has illustrated that particle size is less.Can see resulting CdSe quanta point material distribution of sizes homogeneous intuitively from transmission electron microscope photo, in medium, be uniformly dispersed do not have agglomeration.
Embodiment 2
With the 0.267g cadmium acetate, 1ml oleic acid, the 4ml diphenyl ether adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add the 10ml diphenyl ether in three-neck flask, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 8 minutes, and obtained particle size 2.3nm.UV absorption is positioned at 510nm, fluorescence emission peak wavelength 532nm.Tangible ultraviolet absorption peak and high fluorescence intensity and the narrow half-peak breadth of the fluorescent emission CdSe quanta point material that obtained having hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 3
With the 0.228g caddy, 1ml oleic acid, the 4ml diphenyl ether adds in the 150ml three-neck flask, is heated to 110 ℃, and stirring and dissolving also kept 30 minutes under 110 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add the 10ml diphenyl ether in three-neck flask, nitrogen protection is heated to 110 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 45 minutes, and obtained particle size 1.8nm.Ultraviolet absorption peak is positioned at 476nm, fluorescence emission peak wavelength 500nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 4
With the 0.267g cadmium acetate, 1ml oleic acid, 4ml N, dinethylformamide adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
In three-neck flask, add 10ml N, dinethylformamide, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 12 minutes, and obtained particle size 3.0nm.Fluorescence emission peak wavelength 563nm; Reacted 60 minutes, and obtained particle size 3.8nm.Fluorescence emission peak wavelength 582nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 5
With the 0.128g cadmium oxide, 1ml oleic acid, 4ml N-methyl pyrrolidone adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add 10ml N-methyl pyrrolidone in three-neck flask, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 5 minutes.Obtain particle size 2.7nm.Fluorescence emission peak wavelength 534nm.Reacted 40 minutes.Obtain particle size 3.7nm.Fluorescence emission peak wavelength 580nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 6
With the 0.267g cadmium acetate, the 0.2560g PVP, 4ml N, dinethylformamide adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
In three-neck flask, add 10ml N, dinethylformamide, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.
Reacted 30 minutes.Obtain particle size 3.9nm.Fluorescence emission peak wavelength 599nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 7
With the 0.267g cadmium acetate, 0.2600g phosphatide, the 4ml diphenyl ether adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add the 10ml diphenyl ether in three-neck flask, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C reacted 10 minutes under intense agitation.Obtain particle size 2.3nm.Fluorescence emission peak wavelength 526nm.Reacted 60 minutes.Obtain particle size 3.1nm.Fluorescence emission peak wavelength 565nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Embodiment 8
With the 0.267g cadmium acetate, 0.2605g lecithin, the 4ml diphenyl ether adds in the 150ml three-neck flask, is heated to 140 ℃, and stirring and dissolving also kept 30 minutes under 140 ℃, cooled to room temperature and obtained precursor A.
0.158g metal selenium powder is dissolved in the 2ml tri octyl phosphine under ultrasound condition, obtains precursor B.
Mix precursor A and precursor B and obtain reacting storing solution C.
Add the 10ml diphenyl ether in three-neck flask, nitrogen protection is heated to 140 ℃, and quick dropwise reaction storing solution C begins reaction under intense agitation.Reacted 40 minutes.Obtain particle size 2.9nm.Fluorescence emission peak wavelength 550nm.The CdSe quanta point material that obtains has hyperfluorescence effect and distribution of sizes homogeneous.
Claims (6)
1, a kind of low-temperature solvent legal system is equipped with the method for semiconductor-quantum-point material, it is characterized in that, with inorganic salts as raw material, raw material is cadmium acetate, caddy or the cadmium oxide that contains cadmium ion, the solvent of selecting higher boiling point, strong polarity for use is as reaction medium, select for use surfactant oleic acid, phosphatide, lecithin, polyvinylpyridine that the surface of quantum dot is modified, in the glass flask reaction vessel, lower reaction temperature is reacted 3min～60min down for 110～170 ℃, can obtain the humorous and monodispersed semiconductor-quantum-point material of size adjustable.
2, be equipped with the method for semiconductor-quantum-point material according to the described low-temperature solvent legal system of claim 1, it is characterized in that, below the inventive method is done further to limit, method step is as follows:
(1) with inorganic cadmium salt and surfactant by weight 1: 1, under 110～170 ℃ of heating conditions that relax, be dissolved in the organic solvent diphenyl ether, N, in dinethylformamide or the N-methyl pyrrolidone, cooling obtains precursor A;
(2) under ultrasound condition, the metal selenium powder is dissolved in the tri octyl phosphine, wherein Cd
2+/ Se
2-=1: 2, obtain precursor B;
(3) at room temperature, fully mix precursor A and precursor B and obtain reacting storing solution C;
(4) will be heated to 110 ℃～170 ℃ of reaction temperatures as the organic solvent of reaction medium, quick dropwise reaction storing solution C under intense agitation, according to the size of needed particle diameter, reaction time 3min～60min;
(5) under stirring condition, the stopped reaction of lowering the temperature rapidly, the reactant liquor that obtains adds double methyl alcohol precipitating, through the centrifugal solid product that obtains;
(6) solid product is dispersed in organic solvent-normal hexane, stores in chloroform or the toluene, according to the size of quantum dot, obtains yellow solution to dark brown red, can obtain the semiconductor-quantum-point material.
3, be equipped with the method for semiconductor-quantum-point material according to the described low-temperature solvent legal system of claim 1, it is characterized in that, selected surfactant is oleic acid, phosphatide, lecithin or polyvinylpyridine, chooses according to the performance of material requested.
4, be equipped with the method for semiconductor-quantum-point material according to the described low-temperature solvent legal system of claim 1, it is characterized in that reaction temperature is lower,, regulate according to the particle size of material requested at 110～170 ℃.
5, the method that is equipped with the semiconductor-quantum-point material according to claim 1 or 2 described low-temperature solvent legal systems, it is characterized in that, adjusting reaction time between 3min～60min, obtain semiconductor-quantum-point particle diameter adjustable a series of semiconductor-quantum-point materials between 1.8nm～3.9nm, the optical property of the quanta point material that obtains is tunable, emission wavelength 520nm～599nm.
6, the method that is equipped with the semiconductor-quantum-point material according to the described low-temperature solvent legal system of claim 2, it is characterized in that, the solvent of choosing comprises the boiling point height, the diphenyl ether that polarity is strong, N, dinethylformamide, the N-methyl pyrrolidone, choosing solvent is the fluorescence property of the quantum dot that obtains of scalable as reaction medium.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328351C (en) * | 2005-09-23 | 2007-07-25 | 上海大学 | Method for preparing II-VI family fluorescent mark semiconductor quantum point MX |
| CN100391849C (en) * | 2006-07-13 | 2008-06-04 | 中国科学技术大学 | Nanometer cadmium chloride tube and its prepn |
| CN101196461B (en) * | 2007-03-17 | 2010-05-19 | 广西师范大学 | Method for measuring CdTe quantum point grain diameter by resonant vibration scattered spectrum |
| CN104030256A (en) * | 2014-06-17 | 2014-09-10 | 福州大学 | CdSe quantum dot and preparation method thereof |
| CN105689700A (en) * | 2016-01-29 | 2016-06-22 | 云南师范大学 | Method for preparing germanium quantum dots |
| CN110962427A (en) * | 2019-11-25 | 2020-04-07 | Tcl华星光电技术有限公司 | Quantum dot film |
-
2003
- 2003-12-19 CN CN 200310122744 patent/CN1288716C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328351C (en) * | 2005-09-23 | 2007-07-25 | 上海大学 | Method for preparing II-VI family fluorescent mark semiconductor quantum point MX |
| CN100391849C (en) * | 2006-07-13 | 2008-06-04 | 中国科学技术大学 | Nanometer cadmium chloride tube and its prepn |
| CN101196461B (en) * | 2007-03-17 | 2010-05-19 | 广西师范大学 | Method for measuring CdTe quantum point grain diameter by resonant vibration scattered spectrum |
| CN104030256A (en) * | 2014-06-17 | 2014-09-10 | 福州大学 | CdSe quantum dot and preparation method thereof |
| CN104030256B (en) * | 2014-06-17 | 2016-03-09 | 福州大学 | A kind of CdSe quantum dot and preparation method thereof |
| CN105689700A (en) * | 2016-01-29 | 2016-06-22 | 云南师范大学 | Method for preparing germanium quantum dots |
| CN110962427A (en) * | 2019-11-25 | 2020-04-07 | Tcl华星光电技术有限公司 | Quantum dot film |
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