CN115651638A - PN junction CdSe/PbS/CdS quantum well material with one-dimensional core-shell heterostructure and preparation method thereof - Google Patents
PN junction CdSe/PbS/CdS quantum well material with one-dimensional core-shell heterostructure and preparation method thereof Download PDFInfo
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- ZTSAVNXIUHXYOY-CVBJKYQLSA-L cadmium(2+);(z)-octadec-9-enoate Chemical compound [Cd+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O ZTSAVNXIUHXYOY-CVBJKYQLSA-L 0.000 claims description 15
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Abstract
The invention discloses a PN junction CdSe/PbS/CdS quantum well material with a one-dimensional core-shell heterostructure and a preparation method thereof. The invention uses the thermal injection method to prepare the CdSe/PbS/CdS quantum well material with the nuclear shell heterostructure, the process is clear, the operation is convenient to control, and the prepared material with the N-P-N heterostructure has more excellent quantum efficiency, good optical property and adjustable excitation wavelength compared with other quantum dots, and has huge application potential in the material fields of illumination, photoelectric detection, display technology and the like of the quantum dots.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a PN junction CdSe/PbS/CdS quantum well material with a core-shell heterostructure and a preparation method thereof.
Background
The quantum dot is a quasi-zero-dimensional material with three-dimensional dimensions within the range of 1 to 100nm, and the size, the shape and the excitation wavelength of the quantum dot can be controlled by regulating and controlling the growth time, the reaction temperature and the ligand of the quantum dot. The lead sulfide quantum dot belongs to a P-type semiconductor nano material, has an adjustable band gap (0.7-2.1 eV), and becomes an excellent choice for a wavelength tunable quantum dot device due to low cost, solution processability and band gap adjustability. The lead sulfide quantum dots are large in size and are regarded as excellent choices in application fields such as near-infrared light emitting LEDs and solar cells, but the research on the lead sulfide quantum dots in the visible light excitation wavelength range still has a development space.
In order to solve lattice mismatch and surface defects of lead sulfide core-shell quantum dot materials, researches on how to passivate defects, reduce lattice mismatch between quantum dot shells and further improve optical properties of the quantum dot shells are continuously sought. Researches show that the lattice mismatch can be greatly reduced by strictly controlling the temperature and the precursor concentration in the synthesis process of the core-shell structure of the quantum dot, and partial researches show that other materials are added into the lead sulfide quantum dot to form a composite material so as to adjust the energy band structure, so that the optical performance of the composite material is improved. (CN 114316947A) provides a large-sized PbS quantum dot, a quantum dot ink, a printed solar cell and a method for preparing the same: hexamethyldisilathiane is used as a sulfur source, and a lead acetate solution with the concentration of 5-10mg/ml is added. (CN 114933898A) provides a preparation method of transition metal element doped lead sulfide quantum dots: the method comprises the steps of synthesizing a transition metal ion-doped micron/submicron lead source by an aqueous solution precipitation method, then reacting the micron/submicron lead source with an organic reagent to form a lead precursor, and reacting the lead precursor with elemental sulfur to synthesize the transition metal element-doped lead sulfide quantum dot. (CN 114933898A) provides a preparation method of lead sulfide quantum dot fluorescent powder: the proportion of the sulfur source and the lead source and the reaction temperature are accurately controlled, and the photoluminescence performance of the lead sulfide quantum dots is effectively improved. (CN 106566526A) provides a quantum dot with a multi-well core-shell structure and a preparation method thereof: the multi-well quantum well structure is realized by a cation exchange method, and although the performances of the lead sulfide quantum well are improved to a certain degree by the methods, the flexibility of the methods in the aspects of material structures and material components is not high. Therefore, the synergistic effect of all components in the core-shell structure material in the process that the quantum dots are excited by energy is effectively exerted by artificially designing the material structure and the material components, so that the improvement of the overall performance of the lead sulfide material is realized and the like, and further research is needed.
In summary, most of the lead sulfide quantum dot materials mentioned in the literature or the patent can not effectively eliminate the lattice mismatch caused by the core-shell structure theoretically, thereby affecting the application of the lead sulfide quantum dot material in the aspect of display. Meanwhile, the core-shell structure of the lead sulfide quantum dot in the current patent is single, and the research progress in the visible light range is poor, so that the prepared lead sulfide quantum dot has a limited effect on improving the optical performance due to the simple structure and the large energy band span of the core-shell material.
Disclosure of Invention
The invention aims to provide a PN junction CdSe/PbS/CdS quantum well material with a one-dimensional core-shell heterostructure and a preparation method thereof. In order to achieve the purpose, the invention adopts the following technical scheme:
a core-shell heterostructure CdSe/PbS/CdS quantum well material is a one-dimensional shell-core structure material which is formed by taking a lead sulfide material as an intermediate layer and coating the lead sulfide material and a cadmium selenide material, wherein the cadmium selenide is taken as a core, the lead sulfide is taken as the intermediate layer, and the cadmium sulfide is taken as a shell.
A preparation method of a PN junction CdSe/PbS/CdS quantum well material with a one-dimensional core-shell heterostructure comprises the following steps:
(1) Mixing cadmium oxide, oleic acid and 1-octadecene, vacuumizing for 2min at normal temperature, maintaining for 10min under an inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a cadmium oleate precursor; mixing lead acetate, oleic acid and 1-octadecene, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a lead oleate precursor;
(2) Mixing sulfur powder and trioctylphosphine TOP, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain an S-TOP precursor; mixing selenium powder and trioctylphosphine TOP, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a Se-TOP precursor;
(3) Adding a cadmium oleate precursor into a three-neck flask, heating and dissolving under inert atmosphere, injecting the Se-TOP precursor obtained in the step (2), sequentially washing with absolute ethyl alcohol and n-hexane, and drying to obtain the quantum dot material with the cadmium selenide core;
(4) Adding the cadmium selenide quantum dot material obtained in the step (3) into n-hexane, heating and stirring the mixture under an inert atmosphere, sequentially injecting the lead oleate precursor obtained in the step (1) and the S-TOP precursor obtained in the step (2), sequentially washing the mixture with absolute ethyl alcohol and n-hexane, and drying the washed mixture to obtain a one-dimensional core-shell cadmium selenide/lead sulfide quantum dot material with cadmium selenide as a core and lead sulfide as a shell;
(5) And (3) adding the one-dimensional core-shell cadmium selenide/lead sulfide quantum dot material obtained in the step (4) into n-hexane, heating and stirring the mixture in an inert atmosphere, sequentially injecting the cadmium oleate precursor in the step (1) and the S-TOP precursor in the step (2), cleaning the mixture by absolute ethyl alcohol and n-hexane, and drying the cleaned mixture to obtain the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure.
Further, in the preparation of the cadmium oleate precursor in the step (1), the dosage of cadmium oxide, oleic acid and 1-octadecene is 1-5mmol, 10ml and 12ml respectively; in the preparation of the lead oleate precursor, the dosages of the lead acetate, the oleic acid and the 1-octadecene are 1-5mmol, 10ml and 10ml respectively.
Further, in the preparation of the S-TOP precursor in the step (2), the dosages of the sulfur powder and the trioctylphosphine TOP are respectively 20mmol and 20ml; in the preparation of the Se-TOP precursor, the dosages of selenium powder and trioctylphosphine TOP are respectively 20mmol and 20ml.
Further, the heating temperature in the step (3) is 250-310 ℃, and the time is 10-30min.
Further, in the step (4), the heating temperature is 240-260 ℃ and the time is 10-30min.
Further, in the step (5), the heating temperature is 240-270 ℃ and the time is 10-30min.
Further, it is possible to provideThe inert atmosphere described in steps (1) - (5) is high purity nitrogen or argon or volume fraction 90% Ar +10% 2 。
The invention has the beneficial effects that: the lead sulfide quantum well material prepared by the invention is a one-dimensional core-shell structure consisting of a cadmium selenide material and a cadmium sulfide material interlayer lead sulfide, and compared with the prior art, the invention adopts a heat injection method to enable the shell to be a well region, thereby having the advantages of controllable core-shell structure and high overlap of electron hole wave functions and having the structural characteristics of a one-dimensional nano functional material. Meanwhile, lead sulfide is effectively wrapped and isolated by a cadmium selenide core and a cadmium sulfide shell to form a special N-P-N type core-shell structure, the energy band structure and the luminescence interval of the quantum well are adjusted, the generation of interface defects and exciton quenching are effectively prevented, and the structural stability, quantum efficiency and photoluminescence intensity of the quantum well material are improved. In addition, the invention has simple and convenient process, easy control of operation steps and easy regulation and control of material components, and is an effective method for preparing the nano functional material including the high-performance luminescent quantum well material.
According to the invention, the excellent energy band adjusting capability of the lead sulfide material in the aspect of quantum well luminescence can be fully utilized to prepare the PN junction type quantum well material taking lead sulfide as a well region; the defect that the quantum yield of the lead sulfide quantum dots is low when the lead sulfide quantum dots are excited by energy and the surface defects are overcome; the core-shell heterostructure CdSe/PbS/CdS quantum well material with high photoluminescence quantum yield, high photoluminescence intensity and excellent photoelectric property and the preparation method thereof are obtained.
Drawings
FIG. 1 is a schematic diagram of a precursor thermal injection process.
FIG. 2 is a diagram of a CdSe/PbS/CdS quantum well material structure.
Note: wherein 1 is an anion/cation precursor, 2 is a CdSe core, 3 is a PbS well, and 4 is a CdS shell.
Detailed Description
The invention aims to provide a PN junction CdSe/PbS/CdS quantum well material with a one-dimensional core-shell heterostructure and a preparation method thereof, and the invention is described by combining the attached drawings and specific embodiments
Example 1
1) Preparing a cadmium oleate precursor: adding 1mmol of cadmium oxide, 10ml of oleic acid and 12ml of 1-octadecene into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly pumping and releasing for 2 times, and heating to 120 ℃ for later use.
2) Preparing a lead oleate precursor: 1mmol of lead acetate, 10ml of oleic acid and 10ml of 1-octadecene are added into a three-neck flask, firstly, the three-neck flask is vacuumized for 2min at normal temperature, the vacuum is maintained for 10min under the nitrogen atmosphere, then, the vacuum pumping is repeated for 2 times, and the temperature is increased to 120 ℃ for later use.
3) Preparation of S-TOP precursor: adding 20mmol of sulfur powder and TOP20ml into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use.
4) Preparation of Se-TOP precursor: adding 20mmol of selenium powder and TOP20ml into a three-neck flask, vacuumizing at normal temperature for 2min, maintaining for 10min under nitrogen atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use.
5) Extracting 5ml of cadmium oleate precursor, injecting into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly pumping and charging for 2 times, raising the temperature to 300 ℃, extracting 3ml of Se-TOP precursor, injecting into the three-neck flask, reacting for 10min, rapidly cooling by using a cold water bath to obtain cadmium selenide quantum dots, centrifugally separating and cleaning the quantum dots by using ethanol and n-hexane, and drying. FIG. 1 is a schematic diagram of a precursor thermal injection process, wherein 1 is an anionic/cationic precursor solution.
6) 100mg of prepared cadmium selenide quantum dots are taken and dissolved in n-hexane, normal-temperature exhaust is firstly carried out for l0min, then the temperature is raised to 240 ℃ under the nitrogen atmosphere, 2.5ml of lead oleate precursor is extracted and injected into a three-neck flask, 1ml of S-TOP precursor is extracted after reaction for 10min and injected into the three-neck flask at the speed of 5ml/h, cooling is rapidly carried out by using a cold water bath after reaction for 10min, the cadmium selenide/lead sulfide quantum dots are obtained, the quantum dots are centrifugally separated and cleaned by using ethanol and n-hexane, and then drying treatment is carried out.
7) 100mg of prepared cadmium selenide/lead sulfide quantum dots are dissolved in n-hexane, normal-temperature exhaust is firstly carried out for l0min, then the temperature is increased to 270 ℃ under the nitrogen atmosphere, 4ml of cadmium oleate precursor is extracted and injected into a three-neck flask, after reaction for 10min, the temperature is reduced to 240 ℃, 2ml of S-TOP precursor is extracted and injected into the three-neck flask at the speed of 2ml/h, the cadmium selenide/lead sulfide/cadmium sulfide quantum well is obtained, the quantum dots are centrifugally separated and cleaned by using ethanol and n-hexane, and 3.5ml of n-octane is used for dispersion, so that the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure can be obtained. FIG. 2 is a diagram of a CdSe/PbS/CdS quantum well material structure, where 2 is a CdSe core, 3 is a PbS shell, and 4 is a CdS shell.
Example 2
1) Preparing a cadmium oleate precursor: adding 5mmol of cadmium oxide, 10ml of oleic acid and 12ml of 1-octadecene into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly pumping and releasing for 2 times, and heating to 120 ℃ for later use.
2) Preparing a lead oleate precursor: adding 5mmol of lead acetate, 10ml of oleic acid and 10ml of 1-octadecene into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly pumping and releasing for 2 times, and heating to 120 ℃ for later use.
3) Preparation of S-TOP precursor: adding 20mmol of sulfur powder and TOP20ml into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use.
4) Preparation of Se-TOP precursor: adding selenium powder 20mmol and TOP20ml into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use.
5) Extracting 3.5ml of cadmium oleate precursor, injecting into a three-neck flask, vacuumizing for 2min at normal temperature, maintaining for 10min under nitrogen atmosphere, repeatedly pumping and charging for 2 times, raising the temperature to 300 ℃, extracting 2ml of Se-TOP precursor, injecting into the three-neck flask, reacting for 10min, rapidly cooling by using a cold water bath to obtain cadmium selenide quantum dots, centrifugally separating and cleaning the quantum dots by using ethanol and n-hexane, and drying. FIG. 1 is a schematic diagram of a precursor thermal injection process, wherein 1 is an anionic/cationic precursor solution.
6) 80mg of prepared cadmium selenide quantum dots are dissolved in n-hexane, normal-temperature exhaust is firstly carried out for l0min, then the temperature is raised to 260 ℃ under the nitrogen atmosphere, 1ml of lead oleate precursor is extracted and injected into a three-neck flask, after reaction for 10min, 1ml of S-TOP precursor is extracted and injected into the three-neck flask at the speed of 5ml/h, after reaction for 10min, cooling is rapidly carried out by using a cold water bath to obtain the cadmium selenide/lead sulfide quantum dots, the quantum dots are centrifugally separated and cleaned by using ethanol and n-hexane, and then drying treatment is carried out.
7) 100mg of the prepared cadmium selenide/lead sulfide quantum dots are dissolved in n-hexane, normal-temperature exhaust is firstly carried out for l0min, then the temperature is increased to 270 ℃ under the nitrogen atmosphere, 3ml of cadmium oleate precursor is extracted and injected into a three-neck flask, 2ml of S-TOP precursor is extracted after reaction for 10min and injected into the three-neck flask at the speed of 2ml/h to obtain a cadmium sulfide/lead sulfide cadmium sulfide quantum well, the quantum dots are centrifugally separated and cleaned by using ethanol and n-hexane, and 3.5ml of n-octane is used for dispersion, thus obtaining the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional heterostructure. FIG. 2 is a diagram of a CdSe/PbS/CdS quantum well material structure, where 2 is a CdSe core, 3 is a PbS shell, and 4 is a CdS shell.
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (8)
1. A PN junction CdSe/PbS/CdS quantum well material with a one-dimensional core-shell heterostructure is characterized in that: the one-dimensional core-shell structure material is formed by a cadmium selenide material and a cadmium sulfide material interlayer lead sulfide, wherein the cadmium selenide is used as a core, the lead sulfide is used as an interlayer, and the cadmium sulfide is used as a shell.
2. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure according to claim 1, is characterized in that: the method comprises the following steps:
(1) Mixing cadmium oxide, oleic acid and 1-octadecene, vacuumizing for 2min at normal temperature, maintaining for 10min under an inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a cadmium oleate precursor; mixing lead acetate, oleic acid and 1-octadecene, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a lead oleate precursor;
(2) Mixing sulfur powder and trioctylphosphine TOP, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain an S-TOP precursor; mixing selenium powder and trioctylphosphine TOP, vacuumizing for 2min at normal temperature, maintaining for 10min under inert atmosphere, repeatedly vacuumizing for 2 times, and heating to 120 ℃ for later use to obtain a Se-TOP precursor;
(3) Adding a cadmium oleate precursor into a three-neck flask, heating and dissolving the cadmium oleate precursor in an inert atmosphere, injecting the Se-TOP precursor obtained in the step (2), sequentially cleaning the Se-TOP precursor with absolute ethyl alcohol and n-hexane, and drying to obtain the quantum dot material with the cadmium selenide core;
(4) Adding the cadmium selenide quantum dot material obtained in the step (3) into n-hexane, heating and stirring under an inert atmosphere, sequentially injecting the lead oleate precursor obtained in the step (1) and the S-TOP precursor obtained in the step (2), then sequentially washing with absolute ethyl alcohol and the n-hexane, and drying to obtain a one-dimensional core-shell cadmium selenide/lead sulfide quantum dot material with cadmium selenide as a core and lead sulfide as a shell;
(5) And (3) adding the one-dimensional core-shell cadmium selenide/lead sulfide quantum dot material obtained in the step (4) into n-hexane, heating and stirring the mixture under an inert atmosphere, sequentially injecting the cadmium oleate precursor in the step (1) and the S-TOP precursor in the step (2), cleaning the mixture by absolute ethyl alcohol and the n-hexane, and drying the cleaned mixture to obtain the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure.
3. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure as claimed in claim 2, wherein: in the preparation of the cadmium oleate precursor in the step (1), the dosage of cadmium oxide, oleic acid and 1-octadecene is 1-5mmol, 10ml and 12ml respectively; in the preparation of the lead oleate precursor, the dosages of lead acetate, oleic acid and 1-octadecene are respectively 1-5mmol, 10ml and 10ml.
4. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure as claimed in claim 2, wherein: in the preparation of the S-TOP precursor in the step (2), the using amounts of sulfur powder and trioctylphosphine TOP are respectively 20mmol and 20ml; in the preparation of the Se-TOP precursor, the dosages of selenium powder and trioctylphosphine TOP are respectively 20mmol and 20ml.
5. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure as claimed in claim 2, wherein: in the step (3), the heating temperature is 250-310 ℃ and the time is 10-30min.
6. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure as claimed in claim 2, wherein: in the step (4), the heating temperature is 240-260 ℃ and the time is 10-30min.
7. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure according to claim 2, is characterized in that: in the step (5), the heating temperature is 240-270 ℃ and the time is 10-30min.
8. The preparation method of the PN junction CdSe/PbS/CdS quantum well material with the one-dimensional core-shell heterostructure as claimed in claim 2, wherein: the inert atmosphere described in steps (1) to (5) is high purity nitrogen or argon or the volume fraction 90% Ar +10% H 2 。
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