CN103484122B - Method for rapidly preparing thick-wall CdTe/CdS quantum dot with controllable shell thickness - Google Patents
Method for rapidly preparing thick-wall CdTe/CdS quantum dot with controllable shell thickness Download PDFInfo
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Abstract
The invention provides a method for rapidly preparing a thick-wall CdTe/CdS quantum dot with the controllable shell thickness, belonging to the field of nanometer material synthesis. The method is characterized in that a CdTe quantum dot is used as a raw material, 3-mercaptopropionic acid is used as a stabilizing agent and a sulphur source, water is used as a solvent, cadmium salt and the 3-mercaptopropionic acid are prepared into a solution at according to certain proportions, and the CdTe/CdS core-shell type quantum dot with different CdS shell thicknesses can be obtained by controlling reaction conditions through a microwave heating reaction. The method has advantages that the reaction conditions are mild, the operation is simple and convenient, the reaction time is short, the CdS shell with the controllable thickness can grow, the light-emitting wavelength range of the prepared core-shell quantum dot is continuous and adjustable, and the core-shell quantum dot has strong light stability.
Description
Technical field
The invention belongs to nano material preparation, be specifically related to synthesis and the purifying of CdTe quantum solution, the preparation of cadmium source reacting precursor, and the technology utilizing microwave synthesis device to prepare under differential responses condition to have the heavy wall CdTe/CdS core-shell type quantum dot of different CdS shell thickness.
Background technology
Quantum dot is that a class geometric scale is less than its material bohr exciton radii, and carrier moving is all confined semiconductor nano material in the dimension of three, space, is usually also referred to as semiconductor nano.Because it has the spectrochemical property of numerous excellence, as fluorescence emission wavelengths continuously adjustabe, can excite multi-wavelength emission by Single wavelength, light stability is strong, fluorescence quantum efficiency is high, and has shown huge application potential in fields such as biomedicine, photoelectronics and energy environments.
Nucleocapsid structure quantum dot is current most study, the class quantum dot be most widely used.By at the larger semiconductor material of quantum dot core epitaxy band gap, can by the exciton confinement of quantum dot core within shell, reduce defect to the non-radiative decay of exciton, significantly improve the fluorescence property of quantum dot, shell structure can be used as the physical barriers with external environment simultaneously, effectively reduce external environment to the impact of quantum dot and destruction, thus improve light stability and the chemical stability of quantum dot.Early stage research finds, the thickness of quantum dot shell generally at about 1 layer better, otherwise easily causes the decline of optical property.For CdSe/CdS, after CdS shell thickness is greater than 2 layers, quantum dot fluorescence quantum yield obviously declines, this mainly will make the lattice mismatch stress between core-shell structure copolymer build up because shell increases, and will produce defect (J. Am. Chem. Soc.1997,119 when stress is excessive
,7019-7029; Nano. Lett., 2003,3,799-803).Recent research finds, heavy wall nucleocapsid structure quantum dot (shell thickness > 3 layers) has the optical property of some uniquenesses, as " flicker " phenomenon (J. Am. Chem. Soc., 2008,130, the 5026-5027 that obviously reduce; Nat. Mater., 2008,7,659-664), can can change by belt type, fluorescence lifetime obviously extends, and emmission spectrum variable range is wide, good light stability etc., this will be conducive to the application of quantum dot in fields such as opto-electronic device, biomedical detections, thus causes the attention of researchist.The people such as Nie find to use undersized CdTe quantum dot as core, the heavy wall core-shell structure copolymer quantum dot (CdTe/ZnSe etc.) of growth can bear larger internal stress, decrease the defect that stress causes, thus there is high fluorescence quantum efficiency, obvious flicker suppresses, high light stability (Nat. Nano., 2009,4,56-63).
Although the research of heavy wall core-shell structure copolymer quantum dot has made great progress, but the preparation of such quantum dot is still very difficult, mainly there is following problem: preparation is main uses organic phase method, there is reacting precursor toxicity larger, temperature of reaction is high, the defects such as severe reaction conditions, especially in shell material process of growth in order to avoid independent nucleation phenomenon, and have employed the method (SILAR) of surface ion layer absorption reaction, growth one deck shell needs two steps, first metal precursor is added, then add nonmetallic precursor and keep the longer reaction times respectively, then above process is repeated.This makes the growth of heavy wall shell very loaded down with trivial details (quantum dot that shell is thicker needs the time of about one day) consuming time, and operational condition require very high, controllability and repeatability poor, be difficult to extensive preparation (Nat. Nano., 2009,4,56-63; J. Am. Chem. Soc., 2012,134,9634-9643).In addition, the product prepared does not possess water dispersible, need to carry out ligand exchange, and this process can reduce the fluorescence quantum efficiency of quantum dot in the application of biomedical sector.In a word, no matter organic synthesis heavy wall type core-shell structure copolymer quantum dot is from the viewpoint of preparation process or practical application, all there is many problems.
The condition that aqueous phase prepares quantum dot is comparatively gentle, and reactant toxicity is lower, and price is more cheap.Although the quantum dot that traditional aqueous phase technology of preparing obtains is second-rate, fluorescence property is lower, by using microwave heating greatly can improve temperature of reaction, improving quantum point mass, Reaction time shorten, being conducive to extensive preparation.Although the Patents of the microwave aqueous phase technology of preparing of existing CdTe/CdS core-shell structure copolymer quantum dot at present, as " microwave preparation of a kind of water-soluble CdTe/CdS core/shell type quantum dot " by name, the patent No. is 200510025505.4, authorized announcement date is on March 27th, 2007, Authorization Notice No. is CN1306003C, but its CdS provided is precursor activated high, a large amount of CdS independent nucleation is easily caused to grow, be only applicable to thin-walled CdTe/CdS core-shell structure copolymer quantum dot, cannot the quantum dot of controlled synthesis heavy wall (CdS shell is more than 3 layers).So current being still necessary develops a kind of technology of preparing of efficient heavy wall CdTe/CdS core-shell structure copolymer quantum dot fast.
Summary of the invention
The present invention is directed to the problems referred to above, propose a kind of simple and efficient to handle, technology that reaction conditions is gentle, controllability is strong microwave aqueous phase prepares heavy wall type CdTe/CdS core-shell structure copolymer quantum dot.
CdTe/CdS quantum dot preparation method provided by the invention, concrete steps are as follows:
Step 1, prepare CdTe quantum solution as raw material:
A () prepares cadmium source: in ultrapure water, add cadmium salt, cadmium oxide compound or cadmium oxyhydroxide, add 3-thiohydracrylic acid, and obtain the cadmium source that cadmium concentration is 0.0005 ~ 0.1 mol/L, the pH value of regulator solution, between 8 ~ 10, passes into nitrogen; The concentration sources in cadmium source is in the empirical value of document and experiment, and meanwhile, preparing quantum dot must carry out in the basic conditions, finds in experiment, and the preparation of stronger alkalescence on CdTe quantum has impact, so the scope of place's selection 8 ~ 10;
B () preparation is as the sodium hydrogen telluride (NaHTe) in tellurium source or hydrogen telluride potassium (KHTe) solution: be that the sodium borohydride of 1:1.5 ~ 1:5 or POTASSIUM BOROHYDRIDE and tellurium powder are placed in sample bottle by mol ratio; after vacuumizing; inject ultrapure water under nitrogen protection; at 30 ~ 50 DEG C, ultrasonic reaction 40 ~ 90 min.The mol ratio of reaction is experiment experience gained, uses the environment of Ultrasonic Heating can fast reaction speed, and the time needed for complete reaction is between 40 ~ 90 min;
C () prepares CdTe quantum: in the solution of cadmium source, add tellurium source, under 100 DEG C of conditions, oil bath heating reflux reaction 0.5 ~ 48 h, namely CdTe quantum solution is obtained, along with the increase in reaction times, the size of the CdTe quantum prepared increases, and reaction 0.5 ~ 48 h, can obtain the CdTe quantum that diameter is 2 ~ 4 nm;
D the purifying of () CdTe quantum: by reaction mixture concentrated by rotary evaporation, adds appropriate aqueous isopropanol, high speed centrifugation, until supernatant liquid clear, colorless, precipitation adds appropriate ultrapure water and dissolves;
Step 2, preparation CdTe/CdS core-shell type quantum dot:
A (), by CdTe solution dilution, tests the ultra-violet absorption spectrum of CdTe quantum solution, the scale of construction before adding according to formulae discovery developing m layer CdS needs;
B () preparation contains the precursor solution in part and sulphur source, namely as the Cd-MPA solution in cadmium source and sulphur source: add cadmium salt, cadmium oxide compound or cadmium oxyhydroxide and 3-thiohydracrylic acid MPA in ultrapure water, obtain cadmium and 3-thiohydracrylic acid ratio is the precursor solution of 1:1 ~ 1:4, adjust ph is between 8 ~ 10.Experimentally experience, when both ratios are greater than 1:1, precursor solution cannot configure, and too small ratio is then unfavorable for the controlled synthesis realizing CdTe/CdS quantum dot, the carrying out that pH value is tested below being conducive between 8 ~ 10;
C () prepares CdTe/CdS core-shell type quantum dot: the precursor solution adding m layer amount in raw material CdTe quantum solution, i.e. Cd-MPA solution, and adjust ph is between 10 ~ 13, after passing into nitrogen, at power 100 ~ 150 W, at temperature 100 ~ 170 DEG C, microwave reaction 5 ~ 20 min.Experimentally experience, the pH value of augmenting response, the power of microwave heating and temperature, can improve the speed of reaction, and above numerical range all have passed through experiment;
In the present invention, the mol ratio of described cadmium salt and 3-thiohydracrylic acid is, cadmium salt: 3-thiohydracrylic acid=1:(1 ~ 3.7), this scope is experiment experience gained.
In the present invention, the mol ratio of described cadmium salt and sodium hydrogen telluride or hydrogen telluride potassium is, cadmium salt: HTe
-=1:(0.05 ~ 1), different reaction ratio, can have an impact to the optical property of CdTe quantum, and in experimentation, inquire into above scope, result is ideal.
In the present invention, described cadmium salt, cadmium oxide compound or cadmium oxyhydroxide comprise: Cadmium oxide, cadmium hydroxide, Cadmium chloride fine powder, cadmium bromide, cadmium iodide, Cadmium Sulphate, cadmium nitrate, cadmium carbonate, cadmium acetate, cadmium perchlorate, cadmium chlorate, cadmium bromate, cadmium iodate, and their hydrate.
In the present invention, use the oxygen in high pure nitrogen expeling solution, other rare gas elementes also can be used to replace high pure nitrogen.
In the present invention, described calculating developing m layer CdS needs the precursor volume used, and calculation formula is document Nature Nanotechnology, method described in 2009,4,56-63: the volume of CdS shell, wherein r
cbe the radius of quantum dot core, m is the number of plies of shell growth, d
mLbe the thickness of every one deck shell, be generally 0.337 nm; The molecule number of reacting precursor
, D
corethe density of core, MW
corethe relative molecular mass of nuclear matter, N
ait is Avogadro constant; n
qDit is the molecule number of quantum dot.
Step 2(c of the present invention) in, described preparation CdTe/CdS core-shell type quantum dot, divides solution and is filled in microwave tube, under different pH value (10 ~ 13), temperature (100 ~ 170 DEG C) and microwave power (100 ~ 150 W), and reacting by heating 5 ~ 20 min.
The present invention uses the cadmium salts such as Cadmium chloride fine powder or its inorganics such as oxide compound, oxyhydroxide as raw material, using 3-thiohydracrylic acid as stablizer and sulphur source, in aqueous environment, utilize microwave heating, " one kettle way " fast controlled synthesis goes out to have the CdTe/CdS nucleocapsid structure quantum dot of different CdS shell thickness.Raw material is easy to get, simple to operate, and controllability is strong, prepares gained quantum dot uniform particle diameter, good dispersity, and emmission spectrum covers visible and near-infrared region, can be widely used at photoelectric device and biomedical aspect.
Accompanying drawing explanation
Fig. 1 adopts the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 3 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
Fig. 2 adopts the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 7 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
Fig. 3 adopts the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 11 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
Fig. 4 adopts the present invention, the CdTe/CdS(CdS:11 layer that the CdTe quantum being 2.1 nanometers with diameter prepares) the high resolution TEM photo of quantum dot.
Embodiment
In order to better understand content of the present invention, set forth the present invention further below in conjunction with embodiment and accompanying drawing.The present embodiment is implemented based on technology of the present invention, gives detailed embodiment and operation steps, but protection scope of the present invention is not limited to following embodiment.
A kind of method preparing the controlled heavy wall CdTe/CdS quantum dot of shell thickness fast comprises three parts: the preparation of (a) CdTe core quantum dot solution; The preparation of (b) reacting precursor solution; The growth of (c) CdTe/CdS core-shell type quantum dot.
Embodiment 1
The preparation of (a) CdTe core quantum dot solution
115 mg CdCl are added in 1 L two-mouth bottle
2, dissolve with 500 mL ultrapure waters, then add 199 μ L MPA solution, after stirring, adding NaOH solution regulator solution pH value is 9, in this cadmium source solution, inject high pure nitrogen 30 min, add freshly prepd NaHTe solution 0.25 mL, heating reflux reaction 40 min.Question response solution is cooled to room temperature, and after concentrated by rotary evaporation, add appropriate Virahol, high speed centrifugation carries out purifying.
The preparation of (b) reacting precursor solution
229 mg CdCl are added in 10 mL sample bottles
2, after dissolving with 4 mL ultrapure waters, add 109 μ L MPA solution and 891 μ L NaOH solution (mass concentration is 20%).
The growth of (c) CdTe/CdS core-shell type quantum dot
CdTe quantum solution after purifying is carried out UV spectrum test, calculates the amount of the precursor solution needed for growth 3 layers of CdS.Then in 20 mL CdTe solution, adding Cd-MPA precursor solution, is 12 by NaOH solution adjust ph, passes into high pure nitrogen 30 min, and power setting is 150W, and temperature is set to 140 DEG C, microwave reaction 8 min.
Embodiment 2
The preparation of (a) CdTe core quantum dot solution
115 mg CdCl are added in 1 L two-mouth bottle
2, dissolve with 500 mL ultrapure waters, then add 199 μ L MPA solution, after stirring, adding NaOH solution regulator solution pH value is 9.5, in this cadmium source solution, inject high pure nitrogen 30 min, add freshly prepd NaHTe solution 0.25 mL, heating reflux reaction 60 min.Question response solution is cooled to room temperature, and after concentrated by rotary evaporation, add appropriate Virahol, high speed centrifugation carries out purifying.
The preparation of (b) reacting precursor solution
229 mg CdCl are added in 10 mL sample bottles
2, after dissolving with 3.5 mL ultrapure waters, add 164 μ L MPA solution and 1.34 mL NaOH solution (mass concentration is 20%).
The growth of (c) CdTe/CdS core-shell type quantum dot
CdTe quantum solution after purifying is carried out UV spectrum test, calculates the amount of the precursor solution needed for growth 3 layers of CdS.Then in 5 mL CdTe solution, adding Cd-MPA precursor solution, is 11 by NaOH solution adjust ph, passes into high pure nitrogen 30 min, and power setting is 100W, and temperature is set to 130 DEG C, microwave reaction 15 min.
Embodiment 3
The preparation of (a) CdTe core quantum dot solution
115 mg CdCl are added in 1 L two-mouth bottle
2, dissolve with 500 mL ultrapure waters, then add 109 μ L MPA solution, after stirring, adding NaOH solution regulator solution pH value is 8.5, in this cadmium source solution, inject high pure nitrogen 30 min, add freshly prepd NaHTe solution 0.5 mL, heating reflux reaction 45 min.Question response solution is cooled to room temperature, and after concentrated by rotary evaporation, add appropriate Virahol, high speed centrifugation carries out purifying.
The preparation of (b) reacting precursor solution
229 mg CdCl are added in 10 mL sample bottles
2, after dissolving with 3.5 mL ultrapure waters, add 164 μ L MPA solution and 1.34 mL NaOH solution (mass concentration is 20%).
The growth of (c) CdTe/CdS core-shell type quantum dot
CdTe quantum solution after purifying is carried out UV spectrum test, calculates the amount of the precursor solution needed for growth 7 layers of CdS.Then in 20 mL CdTe solution, adding Cd-MPA precursor solution, is 13 by NaOH solution adjust ph, passes into high pure nitrogen 30 min, and power setting is 150W, and temperature is set to 150 DEG C, microwave reaction 10 min.
Embodiment 4
The preparation of (a) CdTe core quantum dot solution
115 mg CdCl are added in 1 L two-mouth bottle
2, dissolve with 500 mL ultrapure waters, then add 109 μ L MPA solution, after stirring, adding NaOH solution regulator solution pH value is 10, in this cadmium source solution, inject high pure nitrogen 30 min, add freshly prepd NaHTe solution 0.5 mL, heating reflux reaction 30 min.Question response solution is cooled to room temperature, and after concentrated by rotary evaporation, add appropriate Virahol, high speed centrifugation carries out purifying.
The preparation of (b) reacting precursor solution
229 mg CdCl are added in 10 mL sample bottles
2, after dissolving with 4 mL ultrapure waters, add 109 μ L MPA solution and 891 μ L NaOH solution (mass concentration is 20%).
The growth of (c) CdTe/CdS core-shell type quantum dot
CdTe quantum solution after purifying is carried out UV spectrum test, calculates the amount of the precursor solution needed for growth 11 layers of CdS.Then in 7 mL CdTe solution, adding Cd-MPA precursor solution, is 12 by NaOH solution adjust ph, passes into high pure nitrogen 30 min, and power setting is 100W, and temperature is set to 160 DEG C, microwave reaction 10 min.
According to the method for the invention, by changing the pH value of reaction, the temperature and time of heating and microwave power, the CdTe/CdS quantum dot with different CdS shell thickness can be obtained.
Shown in Fig. 1, be adopt the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 3 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
Shown in Fig. 2, be adopt the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 7 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
Shown in Fig. 3, be adopt the present invention, the CdTe quantum being 2.1 nanometers with diameter CdTe/CdS(CdS: 11 layers of preparing) UV, visible light of quantum dot and fluorescence spectrum figure.
From Fig. 1 ~ 3, along with the increase of CdS shell thickness, all there is obvious Red Shift Phenomena in the ultraviolet of CdTe/CdS quantum dot and fluorescence spectrum, Stokes shift increases, fluorescence spectrum can covering visible light to near-infrared region, which demonstrate realizability of the present invention and prepare the potential using value of gained CdTe/CdS quantum dot in fields such as biomedical and photoelectronics.
Shown in Fig. 4, be adopt the present invention, the CdTe/CdS(CdS:11 layer that the CdTe quantum being 2.1 nanometers with diameter prepares) the high resolution TEM photo of quantum dot.As seen from the figure, the product prepared has good dispersiveness, and particle size is comparatively homogeneous.
Claims (2)
1. prepare a method for the controlled heavy wall CdTe/CdS quantum dot of shell thickness fast, its feature comprises the following steps:
Step 1, prepare CdTe quantum solution as raw material:
A () prepares cadmium source: in ultrapure water, add cadmium salt, cadmium oxide compound or cadmium oxyhydroxide, add 3-thiohydracrylic acid, and obtain the cadmium source that cadmium concentration is 0.0005 ~ 0.1 mol/L, the pH value of regulator solution, between 8 ~ 10, passes into nitrogen;
B () preparation is as the sodium hydrogen telluride (NaHTe) in tellurium source or hydrogen telluride potassium (KHTe) solution: be that the sodium borohydride of 1:1.5 ~ 1:5 or POTASSIUM BOROHYDRIDE and tellurium powder are placed in sample bottle by mol ratio, after vacuumizing, inject ultrapure water under nitrogen protection, at 30 ~ 50 DEG C, ultrasonic reaction 40 ~ 90 min;
C () prepares CdTe quantum: in the solution of cadmium source, add tellurium source, and under 100 DEG C of conditions, oil bath heating reflux reaction 0.5 ~ 48 h, namely obtains CdTe quantum solution;
D the purifying of () CdTe quantum: by reaction mixture concentrated by rotary evaporation, adds appropriate aqueous isopropanol, high speed centrifugation, until supernatant liquid clear, colorless, precipitation adds appropriate ultrapure water and dissolves;
Step 2, preparation CdTe/CdS core-shell type quantum dot:
A (), by CdTe solution dilution, tests the ultra-violet absorption spectrum of CdTe quantum solution, the scale of construction before adding according to formulae discovery developing m layer CdS needs;
Described calculating developing m layer CdS needs the precursor volume used, and calculation formula is: the volume of CdS shell
, wherein r
cbe the radius of quantum dot core, m is the number of plies of shell growth, d
mLbe the thickness of every one deck shell, be generally 0.337 nm; The molecule number of reacting precursor
, D
corethe density of core, MW
corethe relative molecular mass of nuclear matter, N
ait is Avogadro constant; n
qDthe molecule number of quantum dot ";
Described m layer is: 3 ~ 11 layers.
B the precursor solution of () preparation containing part and sulphur source: add cadmium salt, cadmium oxide compound or cadmium oxyhydroxide and 3-thiohydracrylic acid (MPA) in ultrapure water, obtains cadmium and 3-thiohydracrylic acid ratio is the precursor solution of 1:1 ~ 1:4, and adjust ph is between 8 ~ 10;
C () prepares CdTe/CdS core-shell type quantum dot: the precursor solution adding m layer amount in raw material CdTe quantum solution, adjust ph between 10 ~ 13, after passing into nitrogen, at power 100 ~ 150W, at temperature 100 ~ 170 DEG C, microwave reaction 5 ~ 20 min.
2. a kind of method preparing the controlled heavy wall CdTe/CdS quantum dot of shell thickness fast according to claim 1, is characterized in that step 1(a) in, the mol ratio of cadmium salt and 3-thiohydracrylic acid is, cadmium salt: 3-thiohydracrylic acid=1:(1 ~ 3.7).
3. a kind of method preparing the controlled heavy wall CdTe/CdS quantum dot of shell thickness fast according to claim 1, is characterized in that step 1(c) in, the mol ratio of cadmium salt and sodium hydrogen telluride or hydrogen telluride potassium is, cadmium salt: HTe
-=1:(0.05 ~ 1).
4. a kind of method preparing the controlled heavy wall CdTe/CdS quantum dot of shell thickness fast according to claim 1, it is characterized in that described cadmium salt, cadmium oxide compound or cadmium oxyhydroxide comprise: Cadmium oxide, cadmium hydroxide, Cadmium chloride fine powder, cadmium bromide, cadmium iodide, Cadmium Sulphate, cadmium nitrate, cadmium carbonate, cadmium acetate, cadmium perchlorate, cadmium chlorate, cadmium bromate, cadmium iodate, and their hydrate.
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