CN102516995A - Method for preparing water-phase CdS quantum dots in oil phase - Google Patents
Method for preparing water-phase CdS quantum dots in oil phase Download PDFInfo
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- CN102516995A CN102516995A CN2011103737514A CN201110373751A CN102516995A CN 102516995 A CN102516995 A CN 102516995A CN 2011103737514 A CN2011103737514 A CN 2011103737514A CN 201110373751 A CN201110373751 A CN 201110373751A CN 102516995 A CN102516995 A CN 102516995A
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Abstract
The invention discloses a method for preparing water-phase CdS quantum dots in an oil phase. In an oil phase system environment, a sulfur (S) precursor provided by mercapto (-SH) in 3-mercaptopropyltrimethoxysilane (MPS) molecules and a cadmium (Cd) precursor are used for generating CdS quantum dots at high temperature, and a silicon layer is coated on the surfaces of the CdS quantum dots through the hydrolysis of the silicon-oxygen chemical bonds (Si-O) in MPS molecules to obtain the quantum dots coated with a CdS@SiO2 silicon layer. Owning to the hydrophilicity of the silicon layer, the quantum dots directly have water-solubility and can be directly applied to the fields such as biological imaging labels and the like. By adopting the method for preparing the water-phase quantum dots in the oil phase, the two operating steps namely oil-phase CdS quantum dot synthesis and surface silicon layer coating which are required by the preparation of the CdS@SiO2 quantum dots, are broken, thus the quantum dots prepared in the oil phase can be directly used in bioapplication and the distance between the synthesis of quantum dots and the application can be greatly shortened.
Description
Technical field
The present invention relates to the technology of preparing of quantum dot, specifically be meant the method for preparing water CdS quantum dot in a kind of oil phase.
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Background technology
(quantum dots QDs) typically refers to the semiconductor nanocrystal of radius less than perhaps approximate exciton bohr particle diameter to quantum dot, and they have unique physics and chemistry and optical property; The continuous distribution such as exciting spectrum width, emission wavelength can be regulated through size and moity, and fluorescence quantum yield is high; Life-span is long; Thereby in the fluorescent mark imaging, luminescent device, fields such as photovaltaic material have a wide range of applications.The general method for preparing aqueous phase quantum point comprises direct method and indirect method, and direct method is promptly directly synthetic in the aqueous solution, because its temperature of reaction is lower, the general fluorescence quantum yield of the quantum dot of acquisition is on the low side, and homogeneity is also relatively poor; Indirect method is promptly earlier through synthetic oil phase quantum dot, then through the surface hydrophilicity ligand exchange or coat method such as water-soluble silicon layer, with the oil phase quantum dot water of transduceing.Wherein coat nontoxic silica shell on the quantum dot surface; Not only can strengthen the biocompatibility of quantum dot; Can also improve the stability under coenocorrelation of quantum dot; The numerous chemical group of while silicon ball surface is that the targeting modification of quantum dot provides the site, thereby becomes the method that a kind of very popular oil phase quantum dot changes water.
But coating the method for silicon layer, common quantum dot not only need the oil phase quantum dot synthetic rapid with two operations of silicon layer coating; And the operation steps that silicon layer coats also relatively wastes time and energy; Usually the time of needs about one week of cost, and strict reaction conditions and the purification process process of follow-up complicacy have also seriously hindered its application.A. P. Alivisatos (Science, 1998,281,2013-2016; J. Phys. Chem. B, 2001,105; 8861-8871) with Jackie Y. Ying (Adv. Mater.; 2005,17,1620-1625) wait the oil phase quantum dot to be transduceed into and done a large amount of work aspect the aqueous phase quantum point at the silicon layer coated quantum dots; But without exception, these silicon layers coat synthetic and two steps of silicon layer coating of oil phase that the method for preparing aqueous phase quantum point has all experienced quantum dot without exception.
Summary of the invention
The invention solves the deficiency of prior art; The method for preparing aqueous phase quantum point in this oil phase, the quantum dot surface coats two operation stepss that silicon layer need experience before having broken, and makes that the quantum dot for preparing in the oil phase can be directly towards biologic applications; Shortened the distance between the synthetic of quantum dot and the application greatly; In oil phase system environment, (the S precursor that SH) provides at high temperature generates the quantum dot of CdS (Cadmium Sulfide) with the Cd precursor through the sulfydryl in the MPS molecule; Hydrolysis through the silica chemical bond (Si-O) in the MPS molecule simultaneously coats silicon layer, the CdSSiO of acquisition on the CdS surface
2The quantum dot that silicon layer coats directly possesses water-soluble.
Prepare the method for water CdS quantum dot in a kind of oil phase of the present invention, it comprises the steps:
1), trimethoxy mercaptopropylsilane (MPS) is added in the mixing solutions of P contained compound, amine-containing compound and octadecylene (ODE); Under the condition of anhydrous and oxygen-free; Use electric mantle to be heated to 260～320 ℃; The MPS precursor solution that makes, wherein MPS content is 0.0135～0.135 mol/L.
2), with mol ratio be Cadmium oxide (CdO) and the fatty acid cpds mixing back adding ODE solution of 1:2; In electric mantle, be heated to 230 ℃ jointly; After treating that CdO dissolves fully, be cooled to room temperature, the Cd content of preparation is the cadmium precursor compound of 0.01～0.1 mol/L.
3), the cadmium precursor fast injection is gone in the described MPS precursor solution of step 1, question response cooled to 100 ℃ after 3～100 minutes; Be injected into the basic soln of 0.02～1 mL; Reacted 1～35 minute, and be cooled to room temperature, the deposition of acquisition is the CdS with water miscible coated with silica
(CdSSiO 2 )Quantum dot.
And, in the said MPS precursor solution in the MPS precursor solution P contained compound be among TOPO, the TOP one or both.When being several kinds of mixing, can the arbitrary proportion configuration.
And amine-containing compound is 1 ~ 3 kind among HAD, ODA, the OLA in the described MPS precursor solution, when being several kinds of mixing, and can the arbitrary proportion configuration
And the mass ratio of P contained compound and amine-containing compound is 1:0.1 ~ 1:99 in the described MPS precursor solution.
And the mass content of ODE is 0～99% in the described MPS precursor solution.
And described fatty acid cpds is oleic acid (OA) or Triple Pressed Stearic Acid (SA).
And the described basic soln that is injected into is the methanol solution of TMAOH, and its concentration is 0.1～1 g/mL, or massfraction is the ammoniacal liquor of 25 %.
And the process of preparation is in the single oil phase system all the time, and is middle without successive what aqueous environment.
And the MPS that uses in the process of preparation both as the S precursor of synthetic CdS quantum dot, also carried out silicon layer as the Si precursor to the CdS quantum dot and coated.
Among the present invention, under regulation and control high temperature, the temperature and the reaction times of cadmium precursor and MPS precursors reaction, can regulate and control the size and the fluorescence quantum yield of CdS quantum dot; The volume of the alkaline solution through regulating injection and concentration with and subsequent the reaction times, can regulate and control the thickness of the silicon layer of coating, thereby obtain the big or small CdSSiO of different-grain diameter
2Material satisfies different application requiring.
The method of synthetic aqueous phase quantum point in the relevant oil phase among the present invention; The method that coats silicon layer with traditional quantum dot surface is completely different; This at first shows the MPS that uses in the preparation process both as the S precursor of synthetic CdS quantum dot; Also as the Si precursor that coats the CdS quantum dot, than the synthetic CdSSiO of routine
2Both need use the S precursor substance, need use other Si precursor substance again, save reaction raw materials, make that reacting precursor was able to use to greatest extent, meet the demand for development of conservation-minded society; The second, be in single oil phase environment all the time in the process for preparing, middle environment without successive what water, reaction conditions is simple; And employing one kettle way; Only need a reactions step,, practiced thrift a large amount of reaction times and manpower such as the two steps operation of the synthetic back coating of traditional quantum dot silicon ball transduction water; The quantum dot that obtains directly possesses water-soluble, can directly apply to fields such as biomarker.Therefore quantum dot preparation method shown in the present is different from the method that the synthetic back of traditional quantum dot silicon layer coats fully, is a kind of brand-new preparation method, also is a kind of direct application oriented preparation method, can be referred to as saving type Green Chemistry preparation method.
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Description of drawings
Fig. 1 is the method synoptic diagram for preparing water CdS quantum dot in the oil phase of the present invention.
Fig. 2 prepares product fluorescence contrast under uv lamp in the aqueous phase quantum point process for the embodiment of the invention 1 oil phase, and wherein A is that oil phase CdS quantum dot, B are CdSSiO in the oil phase
2Quantum dot deposition, C are water CdSSiO
2The fluorescence of quantum dot.
Fig. 3 is the water CdSSiO of the embodiment of the invention 1 preparation
2The fluorescent emission collection of illustrative plates of quantum dot.
Fig. 4 is the water CdSSiO of the embodiment of the invention 1 preparation
2The ultraviolet absorpting spectrum of quantum dot.
Fig. 5 is the water CdSSiO of the embodiment of the invention 1 preparation
2The high-resolution-ration transmission electric-lens photo of quantum dot.
Fig. 6 is the water CdSSiO of the embodiment of the invention 1 preparation
2Quantum dot and nucleus dyestuff HOECHS cell be localized confocal fluorescent microphotograph altogether, and wherein D is water CdSSiO
2Quantum dot detects the luminous situation of wave band, and E is that nucleus dyestuff HOECHS detects the luminous situation of wave band, and F is the overlapping luminous situation of D and E.
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Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
Flow process can be referring to Fig. 1.
1), get 0.13 g TOPO, 0.37 g HAD, 200 μ L MPS and 9.5 mL ODE mix the back and under Ar gas, in electric mantle, being heated to 280 ℃, obtain the colourless MPS precursor solution of clarification.
2), get 0.0128 g CdO, 0.063 mL OA, 1 mL ODE, mix the back in electric mantle, be heated under the Ar gas 230 ℃ dissolve fully to CdO after, be cooled to room temperature, obtain the colourless Cd (OA) of clarification
2Precursor solution.
3), with Cd (OA)
2The precursor solution fast injection is gone in the MPS solution under the high temperature, and temperature of reaction is set in 285 ℃, reacts 15 minutes, in air, is cooled to 100 ℃.
4), fast injection is gone into 500 μ L in above-mentioned solution, the methanol solution of 0.4 g/mL TMAOH reacted 35 minutes, removed thermal source, was cooled to room temperature.
5), with reaction soln 500 r/min low-speed centrifugal 2 minutes, being deposited in the normal hexane after the washing of acquisition is dispersed in the water again, promptly obtains to be dissolved in the CdS quantum dot of aqueous phase.
The check of the water CdS quantum dot for preparing in the oil phase:
A. with product as under the uv lamp, can see tangible fluorescent emission, as shown in Figure 2.
B. product is dispersed in the water, on luminoscope, detects its fluorescent emission, can observe tangible fluorescence emission peak, as shown in Figure 3.
C. product is dispersed in the water, on ultraviolet-visible pectrophotometer, detects its uv-absorbing, can observe tangible uv-absorbing, as shown in Figure 4.
D. product is dispersed in the water, drips 2 in copper mesh, imaging can be observed the structure that the silicon bag covers quantum dot under high-resolution-ration transmission electric-lens, and is as shown in Figure 5.
E, product is dispersed in the water, through with the 293T co-culture of cells after, through dying altogether, detect at confocal fluorescent microscopically different-waveband with nucleus dyestuff HOECHST, can observe tangible cell marking imaging, as shown in Figure 6.
Embodiment 2
Flow process can be referring to Fig. 1.
1), get 0.13 g TOPO, 1 mL TOP, 0.5mL OLA, 200 μ L MPS and 3.5 mL ODE mix the back and under Ar gas, in electric mantle, being heated to 260 ℃, obtain the colourless MPS precursor solution of clarification.
2), get 0.0128 g CdO, 0.0569 g SA, 10 mL ODE, mix the back in electric mantle, be heated under the Ar gas 230 ℃ dissolve fully to CdO after, be cooled to room temperature, obtain the colourless Cd (SA) of clarification
2Precursor solution.
3), with Cd (SA)
2The precursor solution fast injection is gone in the MPS solution under the high temperature, and temperature of reaction is set in 260 ℃, reacts 100 minutes, in air, is cooled to 100 ℃.
4), fast injection is gone into 1 mL in above-mentioned solution then, the ammoniacal liquor of 25 % reacted 3 minutes, removed thermal source, was cooled to room temperature.
5), with reaction soln 500 r/min low-speed centrifugal 2 minutes, being deposited in the normal hexane after the washing of acquisition is dispersed in the water again, promptly obtains to be dissolved in the CdS quantum dot of aqueous phase.
Embodiment 3
Flow process can be referring to Fig. 1.
1), get 0.13 g TOPO, 0.37 g HAD, 0.5 mL ODA, 200 μ L MPS and 9 mL ODE mix the back and under Ar gas, in electric mantle, being heated to 320 ℃, obtain the colourless MPS precursor solution of clarification.
2), get 0.0128 g CdO, 0.063 mL OA, 5 mL ODE, mix the back in electric mantle, be heated under the Ar gas 230 ℃ dissolve fully to CdO after, be cooled to room temperature, obtain the colourless Cd (OA) of clarification
2Precursor solution.
3), with Cd (OA)
2The precursor solution fast injection is gone in the MPS solution under the high temperature, and temperature of reaction is set in 320 ℃, reacts 3 minutes, in air, is cooled to 100 ℃.
4), fast injection is gone into 2 mL in above-mentioned solution then, the methanol solution of 0.1 g/mL TMAOH reacted 10 minutes, removed thermal source, was cooled to room temperature.
5), with reaction soln 500 r/min low-speed centrifugal 2 minutes, being deposited in the normal hexane after the washing of acquisition is dispersed in the water again, promptly obtains to be dissolved in the CdS quantum dot of aqueous phase.
Embodiment 4
Flow process is referring to Fig. 1.
1), get 1 mL TOP, 0.37 g HAD, 0.5 mL ODA, 0.5 mL OLA, 200 μ L MPS and 7.5 mL ODE mix the back and under Ar gas, in electric mantle, being heated to 300 ℃, obtain the colourless MPS precursor solution of clarification.
2), get 0.0128 g CdO, 0.063 mL OA, 2 mL ODE, mix the back in electric mantle, be heated under the Ar gas 230 ℃ dissolve fully to CdO after, be cooled to room temperature, obtain the colourless Cd (OA) of clarification
2Precursor solution.
3), with Cd (OA)
2The precursor solution fast injection is gone in the MPS solution under the high temperature, and temperature of reaction is set in 300 ℃, reacts 5 minutes, in air, is cooled to 100 ℃.
4), fast injection is gone into 200 μ L in above-mentioned solution then, the methanol solution of 1 g/mL TMAOH reacted 1 minute, removed thermal source, was cooled to room temperature.
5), with reaction soln 500 r/min low-speed centrifugal 2 minutes, being deposited in the normal hexane after the washing of acquisition is dispersed in the water again, promptly obtains to be dissolved in the CdS quantum dot of aqueous phase.
Claims (9)
1. prepare the method for water CdS quantum dot in the oil phase, it is characterized in that it comprises the steps:
1), 3-sulfydryl propyl trimethoxy silicane (MPS) is added in the mixing solutions of P contained compound, amine-containing compound and octadecylene (ODE); Under the condition of anhydrous and oxygen-free; Be heated to 260～320 ℃; The MPS precursor solution that makes, wherein MPS content is 0.0135～0.135 mol/L;
2) be that the Cadmium oxide of 1:2 (CdO) and fatty acid cpds mix back adding ODE solution, with the molar weight ratio; Be heated to 230 ℃ jointly; After treating that CdO dissolves fully, be cooled to room temperature, the Cd compounds content of preparation is the cadmium precursor compound of 0.01～0.1 mol/L;
3), the cadmium precursor fast injection is gone in the described MPS precursor solution of step 1; Behind the question response 3～100 minutes; Cool to 100 ℃, be injected into the basic soln of 0.02～1 mL, reacted 1～35 minute; Be cooled to room temperature, the deposition of acquisition is the CdS (CdSSiO with water miscible coated with silica
2) quantum dot.
2. the method for preparing water CdS quantum dot in the oil phase according to claim 1; It is characterized in that; P contained compound is one or both in trioctylphosphine oxide (TOPO), the trioctylphosphine phosphorus (TOP) in the MPS precursor solution, when being two kinds of mixing, and can the arbitrary proportion configuration.
3. the method for preparing water CdS quantum dot in the oil phase according to claim 1; It is characterized in that; Amine-containing compound is 1 ~ 3 kind in cetylamine (HAD), stearylamine (ODA), the oleyl amine (OLA) in the MPS precursor solution, when being several kinds of mixing, and can the arbitrary proportion configuration.
4. oil phase according to claim 1 prepares the method for water CdS quantum dot, it is characterized in that, the mass ratio of P contained compound and amine-containing compound is 1:0.1 ~ 1:99 in the MPS precursor solution.
5. prepare the method for water CdS quantum dot in the oil phase according to claim 1, it is characterized in that, the massfraction of ODE is 0～99% in the MPS precursor solution.
6. prepare the method for water CdS quantum dot in the oil phase according to claim 1, it is characterized in that, fatty acid cpds is oleic acid (OA) or Triple Pressed Stearic Acid (SA).
7. the method for preparing water CdS quantum dot in the oil phase according to claim 1; It is characterized in that; The basic soln that is injected into is the methanol solution of tetramethyl-aqua ammonia (TMAOH), and its concentration is 0.1～1 g/mL, or massfraction is the ammoniacal liquor of 25 %.
8. prepare the method for water CdS quantum dot in the oil phase according to claim 1, it is characterized in that, the process of preparation is in the single oil phase system all the time, and is middle without successive what aqueous environment.
9. prepare the method for water CdS quantum dot in the oil phase according to claim 1, it is characterized in that, the MPS that uses in the process of preparation both as the S precursor of synthetic CdS quantum dot, also carried out silicon layer as the Si precursor to the CdS quantum dot and coated.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103149185A (en) * | 2013-02-05 | 2013-06-12 | 苏州大学 | Novel high-efficiency protease activity detecting method |
| CN104045105A (en) * | 2014-05-11 | 2014-09-17 | 桂林理工大学 | Process for preparing cadmium sulfide quantum dots by low temperature two-phase synthesis method |
| CN105655136A (en) * | 2015-12-28 | 2016-06-08 | 华侨大学 | Preparation method of quantum dot sensitized solar cell counter electrode |
| JP2017523472A (en) * | 2014-07-28 | 2017-08-17 | コーニンクレッカ フィリップス エヌ ヴェＫｏｎｉｎｋｌｉｊｋｅ Ｐｈｉｌｉｐｓ Ｎ．Ｖ． | Silica-coated quantum dots with improved quantum efficiency |
| CN108807608A (en) * | 2017-05-02 | 2018-11-13 | Tcl集团股份有限公司 | A kind of preparation method of oxide coated quantum dots LED |
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| CN103149185A (en) * | 2013-02-05 | 2013-06-12 | 苏州大学 | Novel high-efficiency protease activity detecting method |
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| CN108807608A (en) * | 2017-05-02 | 2018-11-13 | Tcl集团股份有限公司 | A kind of preparation method of oxide coated quantum dots LED |
| CN108807608B (en) * | 2017-05-02 | 2020-06-12 | Tcl科技集团股份有限公司 | Preparation method of oxide-coated quantum dot LED |
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