CN110600637A - Method and device for improving brightness of CdSe/CdS nanosheet LED device - Google Patents
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Abstract
The invention discloses a method and a device for improving the brightness of a CdSe/CdS nanosheet LED device, which solve the problem that the brightness of the device is improved due to the quenching of the fluorescence of a nanosheet light emitting layer by a ZnO electron transport layer in the LED device. The brightness of the device is improved by introducing a PFN layer. The preparation process mainly introduces PFN suspension coating between the CdSe/CdS nanosheet luminescent layer and the ZnO electron transport layer in the device. The CdSe/CdS nanosheet LED device prepared by the preparation method disclosed by the invention has the advantages of stable structure, excellent electroluminescent property and the like, has great application potential in the fields of photoelectric devices and displays, and has the advantages of simple preparation process, strong controllability, high efficiency and the like.
Description
Technical Field
The invention belongs to the technical field of quantum dot LEDs, and relates to a method and a device for improving the brightness of a CdSe/CdS nanosheet LED device.
Background
Colloidal semiconductor quantum dot LEDs are the most promising next generation of LEDs display devices with low production cost, high color purity, high quantum yield, and tunable emission wavelength over the entire visible to near-infrared range. These advantages make quantum dots play an important role in the development of various led materials and configurations. However, the further development of quantum dot LEDs is hindered by the non-uniform spectral broadening of the commonly spherical CdSe quantum dots due to their limited size distribution. In contrast, CdSe Nanosheets (NPLs) have zero dimensional deviation along the quantum confinement direction due to their atomic, thin platelet surface and Cd-Se monolayers with thicknesses precisely controllable at ± 1. And the absorption and emission bands of the spherical CdSe quantum dots are about three times of those of CdSe nanosheets. While narrow-spectrum excitation photoluminescence and electroluminescence bands are key to monochromatic LEDs. In addition, due to the two-dimensional nature of quantum confinement, CdSe nanosheets have a large exciton binding energy and an in-plane electron effective mass, as well as a relatively small dielectric constant. Thus, CdSe nanoplates may exhibit weaker coulombic interaction between carriers compared to quantum dots, thereby enabling more efficient charge injection without affecting confinement and recombination mechanisms. LEDs with CdSe/CdZnS core-shell nanoplates were first reported in 2014, and subsequently researchers developed and demonstrated various nanoplate-based LEDs.
However, to improve efficiency, further optimization of nanosheet based LEDs is required. ZnO nanoparticles are considered to be an ideal electron transport layer for nanosheet LEDs due to their ability to balance the injection and recombination of carriers, and to improve environmental stability. However, spontaneous charge transfer from the CdSe nanoplatelets to the adjacent ZnO layer can suppress the emission of the nanoplatelets, thereby limiting the performance of the overall led device. On the other hand, charge carriers trapped by surface defects may create local electric fields that impede further transport of charge.
Disclosure of Invention
The invention provides a method and a device for improving the brightness of a CdSe/CdS nanosheet LED device, which solve the problem that the brightness of the device is improved due to the quenching of the fluorescence of a nanosheet light emitting layer by a ZnO electron transport layer in the LED device.
The technical scheme of the invention is as follows:
a method for improving the brightness of a CdSe/CdS nanosheet LED device is realized by introducing a polymer layer into the structure of a traditional LED device.
The CdSe/CdS nanosheet LED device adopts ITO as an anode, PEDOT, PSS as a hole injection layer, poly-TPD as a hole transport layer, CdSe/CdS nanosheets as a light emitting layer, a polymer interface layer, ZnO as an electron transport layer and LiF/Al as a cathode.
According to the invention, the method for improving the brightness of the liquid CdSe/CdS nanosheet LED device comprises the following steps:
(1) synthesizing CdSe/CdS nanosheets, and dispersing the obtained nanosheets into n-hexane for later use;
(2) reacting potassium hydroxide with zinc acetate to generate ZnO nanoparticles, and dispersing the final nanoparticles in a mixed solvent of n-butanol/methanol/chloroform;
(3) sequentially carrying out ultrasonic cleaning on the ITO glass substrate in ionized water, acetone, deionized water and isopropanol, then treating with ultraviolet rays/ozone to enrich oxygen on the ITO surface, and removing the heat;
(4) spin-coating PEDOT, namely a PSS hole injection layer, a poly-TPD hole transport layer, a CdSe/CdS nanosheet light-emitting layer, a polymer interface layer and a ZnO electron transport layer on the cleaned ITO glass substrate in the step (3) in sequence;
(5) and (4) evaporating a LiF/Al cathode by adopting a vacuum thermal evaporation method on the basis of the step (4).
According to the present invention, it is preferable that the concentration of CdSe/CdS nanosheets dispersed in the n-hexane solution in step (1) is 8 to 20 mg/ml.
According to the present invention, preferably, the ZnO nanoparticle synthesis process of step (2) is: respectively dissolving potassium hydroxide and zinc acetate in methanol, and dripping the potassium hydroxide solution into the zinc acetate solution at the reaction temperature of 30-80 ℃ for 2-4 hours.
According to the present invention, it is preferable that the ultrasonic time in the ITO cleaning process in step (3) is 10 to 20 minutes.
According to the present invention, it is preferable that the ITO UV/ozone treatment time in step (3) is 5 to 15 minutes.
According to the present invention, preferably, the ITO annealing temperature in step (3) is 100-.
According to the invention, the spin coating speed of the PEDOT: PSS hole injection layer in the step (4) is 3000-5000rpm/min, and the spin coating time is 40-80 seconds.
According to the present invention, it is preferable that the spin coating speed of the poly-TPD hole transport layer in the step (4) is 2000-4000rpm/min, and the spin coating time is 10-30 seconds.
According to the invention, the spin coating speed of the CdSe/CdS nanosheet light-emitting layer in the step (4) is preferably 1000-2000rpm/min, and the spin coating time is preferably 40-60 seconds.
According to the present invention, it is preferable that the spin coating speed of the polymer interface layer in step (4) is 2000-4000rpm/min and the spin coating time is 20-40 seconds.
According to the present invention, it is preferred that the polymer in step (4) is PFN and its derivatives.
According to the invention, preferably, the spin coating speed of the ZnO electron transport layer in the step (4) is 1000-2000rpm/min, and the spin coating time is 40-80 seconds.
According to the present invention, preferably, the evaporation rate of the LiF/Al cathode in the step (5) is
The technical advantages of the invention are as follows:
(1) the preparation method has the advantages of simple preparation process, strong controllability, high efficiency and the like.
(2) The method for improving the brightness of the CdSe/CdS nanosheet LED device effectively solves the problem that the fluorescence quenching of a ZnO electron transmission layer in the nanosheet LED device on a nanosheet light emitting layer improves the brightness of the device.
Drawings
FIG. 1 is a structural diagram of a CdSe/CdS nanosheet LED device in all the examples.
FIG. 2 is a matching diagram of the energy levels of CdSe/CdS nanosheet LED devices in all embodiments.
FIG. 3 is an electroluminescence diagram of a CdSe/CdS nanosheet LED device prepared in embodiment 4 of the present invention.
FIG. 4 is a graph of luminance versus voltage for a CdSe/CdS nanosheet LED device prepared in embodiment 4 of the present invention.
FIG. 5 is a graph of the luminance-voltage curve of a CdSe/CdS nanosheet LED device prepared in comparative example 2.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125ml of methanol and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into the zinc acetate solution, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture (mixing ratio 1:1: 1). Then, the ITO glass substrate was subjected to ultrasonic cleaning in deionized water, acetone, deionized water, and isopropyl alcohol in this order for 15 minutes, then treated with ultraviolet rays/ozone for 10 minutes to enrich the oxygen on the ITO surface, and then the substrate was annealed at 130 ℃ for 20 minutes. Then will bePEDOT PSS hole injection layer was spin coated at 4000rpm/min for 60 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 8mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PFN-Br film on the CdSe/CdS nanosheet film at the speed of 2000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
Example 2:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125ml of methanol and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into the zinc acetate methanol solution, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. Then, the ITO glass substrate was subjected to ultrasonic cleaning in deionized water, acetone, deionized water, and isopropyl alcohol in this order for 15 minutes, then treated with ultraviolet rays/ozone for 10 minutes to enrich the oxygen on the ITO surface, and then the substrate was annealed at 130 ℃ for 20 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 60 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 16mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PFN-OX film on the nanosheet film at the speed of 2000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
Example 3:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125ml of methanol and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into the zinc acetate methanol solution, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. Then, the ITO glass substrate was subjected to ultrasonic cleaning in deionized water, acetone, deionized water, and isopropyl alcohol in this order for 15 minutes, then treated with ultraviolet rays/ozone for 10 minutes to enrich the oxygen on the ITO surface, and then the substrate was annealed at 130 ℃ for 20 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 40 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 20mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PFN-PEI film on the nanosheet film at the speed of 2000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
Example 4:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125 and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into zinc acetate, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol.The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. Then, the ITO glass substrate was subjected to ultrasonic cleaning in deionized water, acetone, deionized water, and isopropyl alcohol in this order for 15 minutes, then treated with ultraviolet rays/ozone for 10 minutes to enrich the oxygen on the ITO surface, and then the substrate was annealed at 130 ℃ for 20 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 40 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 16mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PFN film on the nanosheet film at the speed of 3000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
An electroluminescent photo of the CdSe/CdS nanosheet LED device manufactured by the example is shown in FIG. 3, and the manufactured device is a red LED as can be seen from FIG. 3.
The luminance-voltage curve of the CdSe/CdS nanosheet LED device manufactured by the example is shown in FIG. 4, and it can be known from FIG. 4 that the luminance of the manufactured LED device is enhanced along with the increase of the voltage, wherein the maximum luminance is 5833cd/m2。
Example 5:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125 and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into zinc acetate, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. Then, the ITO glass substrate is sequentially subjected to ultrasonic cleaning for 15 minutes in deionized water, acetone, deionized water and isopropanol, and then ultraviolet rays are used for cleaningWire/ozone treatment was performed for 10 minutes to enrich the ITO surface with oxygen, and then the substrate was annealed at 130 ℃ for 20 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 40 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 16mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PFN film on the nanosheet film at the speed of 4000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
Comparative example 1:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125ml of methanol and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into zinc acetate, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. And then, sequentially carrying out ultrasonic cleaning on the ITO glass substrate in deionized water, acetone, deionized water and isopropanol for 15 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 40 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 16mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, spin-coating a PET film on the nanosheet film at the speed of 4000rpm/min for 30 seconds, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
The CdSe/CdS nanosheet LED device prepared by the comparative example has poor effect, and part of quantum dots are agglomerated on the PET film and have poor dispersibility.
Comparative example 2:
dispersing CdSe/CdS nanosheets in n-hexane. Meanwhile, methanol is used as a solvent, and the potassium hydroxide reacts with the zinc acetate to generate ZnO nano-particles. Zinc acetate and potassium hydroxide were dissolved in 125 and 65ml of methanol at 65 ℃ respectively. Then, a potassium hydroxide solution was dropped into zinc acetate, and the mixture was maintained at 65 ℃ for 3 hours to grow ZnO nanoparticles. Then, ZnO nanoparticles were precipitated by centrifugation and washed twice with methanol. The final ZnO nanoparticles were dispersed in an n-butanol/methanol/chloroform mixture. Then, the ITO glass substrate was subjected to ultrasonic cleaning in deionized water, acetone, deionized water, and isopropyl alcohol in this order for 15 minutes, then treated with ultraviolet rays/ozone for 10 minutes to enrich the oxygen on the ITO surface, and then the substrate was annealed at 130 ℃ for 20 minutes. The PEDOT: PSS hole injection layer was spin coated at 4000rpm/min for 40 seconds onto the ITO surface and then annealed in a nitrogen-filled glove box at 140 ℃ for 30 minutes. Subsequently, a hole transport layer of poly-TPD was spin-coated on the PEDOT: PSS film at a speed of 2000rpm/min for 10 seconds. Spin-coating CdSe/CdS nanosheet 16mg/ml n-hexane solution on a poly-TPD film at the speed of 1000rpm/min, and then spin-coating a ZnO electron transport layer film at the speed of 1500rpm/min for 60 seconds. Finally, the evaporation speed is adoptedAnd (4) carrying out vacuum thermal evaporation on a LiF/Al cathode.
The brightness-voltage curve of the CdSe/CdS nanosheet LED device prepared by the comparative example is shown in FIG. 5, and it can be known from FIG. 5 that the brightness of the prepared LED device is enhanced along with the increase of voltage, wherein the maximum brightness is 3153cd/m2。
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. A method for improving the brightness of a CdSe/CdS nanosheet LED device is characterized by comprising the following steps:
(1) synthesizing CdSe/CdS nanosheets, and dispersing the obtained nanosheets in n-hexane for later use;
(2) reacting potassium hydroxide with zinc acetate to generate ZnO nanoparticles, and dispersing the final nanoparticles in a mixed solvent of n-butanol/methanol/chloroform;
(3) sequentially carrying out ultrasonic cleaning on the ITO glass substrate in deionized water, acetone, deionized water and isopropanol, then treating with ultraviolet rays/ozone to enrich oxygen on the ITO surface, and removing the heat;
(4) spin-coating PEDOT, namely a PSS hole injection layer, a poly-TPD hole transport layer, a CdSe/CdS nanosheet light-emitting layer, a polymer interface layer and a ZnO electron transport layer on the cleaned ITO glass substrate in the step (3) in sequence; the polymer is PFN or a derivative thereof;
(5) and (4) evaporating a LiF/Al cathode by adopting a vacuum thermal evaporation method on the basis of the step (4).
2. The method according to claim 1, wherein the concentration of CdSe/CdS nanosheets dispersed in the n-hexane solution is from 8 to 20 mg/ml.
3. The method according to claim 1, wherein the ZnO nanoparticles synthesized in step (2) are prepared by the following steps: respectively dissolving potassium hydroxide and zinc acetate in methanol, and dripping the potassium hydroxide solution into the zinc acetate solution at the reaction temperature of 30-80 ℃ for 2-4 hours.
4. The method as claimed in claim 1, wherein the ITO cleaning process in step (3) comprises ultrasonic treatment for 10-20 min, ITO UV/ozone treatment for 5-15 min, ITO annealing temperature for 100 ℃ and annealing time for 10-30 min.
5. The method as claimed in claim 1, wherein the ITO annealing temperature in step (3) is 100 ℃ and 140 ℃, and the annealing time is 10-30 minutes.
6. The method as claimed in claim 1, wherein the spin coating speed of the PEDOT: PSS hole injection layer in step (4) is 3000-5000rpm/min, the spin coating time is 40-80 seconds, the spin coating speed of the poly-TPD hole transport layer is 2000-4000rpm/min, and the spin coating time is 10-30 seconds.
7. The method as claimed in claim 1, wherein the spin coating speed of the CdSe/CdS nanosheet light-emitting layer in step (4) is 1000-2000rpm/min, and the spin coating time is 40-60 seconds.
8. The method as claimed in claim 1, wherein the spin coating speed of the polymer interface layer in step (4) is 2000-4000rpm/min, and the spin coating time is 20-40 seconds.
9. The method as claimed in claim 1, wherein the spin coating speed of the ZnO electron transport layer in step (4) is 1000-2000rpm/min, and the spin coating time is 40-80 seconds.
10. A CdSe/CdS nanosheet LED device prepared according to any one of claims 1 to 9.
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| US20170125172A1 (en) * | 2015-10-30 | 2017-05-04 | The University Of Akron | Perovskite hybrid solar cells |
| CN108630814A (en) * | 2017-03-15 | 2018-10-09 | Tcl集团股份有限公司 | A kind of nucleocapsid colloidal nano piece, QLED devices and preparation method |
| CN109713098A (en) * | 2017-10-26 | 2019-05-03 | 乐金显示有限公司 | Light emitting diode and luminaire including the light emitting diode |
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| US20170125172A1 (en) * | 2015-10-30 | 2017-05-04 | The University Of Akron | Perovskite hybrid solar cells |
| CN105720206A (en) * | 2016-05-06 | 2016-06-29 | Tcl集团股份有限公司 | QLED device and preparation method thereof |
| CN108630814A (en) * | 2017-03-15 | 2018-10-09 | Tcl集团股份有限公司 | A kind of nucleocapsid colloidal nano piece, QLED devices and preparation method |
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