CN111384302A - Full-solution preparation method of fibrous inorganic perovskite quantum dot light-emitting diode - Google Patents
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- CN111384302A CN111384302A CN201811622059.9A CN201811622059A CN111384302A CN 111384302 A CN111384302 A CN 111384302A CN 201811622059 A CN201811622059 A CN 201811622059A CN 111384302 A CN111384302 A CN 111384302A
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Abstract
The invention discloses a preparation method of a full solution of a fibrous inorganic perovskite quantum dot light-emitting diode. The method comprises the steps of dipping, pulling and depositing a hole injection layer on a flexible fiber, and then dipping, pulling and depositing a hole transport layer, namely CsPbX in sequence3The fibrous inorganic perovskite quantum dot light-emitting diode with uniform light emission is obtained by mixing perovskite quantum dots, a small molecular material and a polymer material to form a light-emitting layer, an electron transport layer and a thermal evaporation deposition electrode material. The invention has simple process, high material utilization rate and low cost, the prepared quantum dot light-emitting diode can emit light uniformly, and the halogen proportion of the material of the quantum dot light-emitting layer can be adjusted to obtain the light-emitting fibers with different colors.
Description
Technical Field
The invention relates to a fiberUygur CsPbX3A full-solution preparation method of an inorganic perovskite quantum dot light-emitting diode belongs to the technical field of preparation of an electroluminescent quantum dot light-emitting device.
Background
In recent years, perovskite materials have been widely studied in the fields of solar cells, light emitting diodes, photodetectors, and the like, because of their excellent photoelectric properties. Compared with the traditional organic-inorganic hybrid perovskite (CH)3NH3PbX3) All inorganic perovskites (CsPbX)3) They are attracting attention because of their excellent light and heat stability.
At present, the preparation of quantum dot light-emitting diodes mostly adopts spin coating, evaporation coating and other processes to prepare the light-emitting diodes, and has the defects of low material utilization rate and the like. The current trend is mainly how to prepare efficient and stable perovskite light emitting diodes, and the preparation methods of flexible and full solution processes are less studied. With the improvement of living standard of people, the development of display technology also faces new challenges. With the advent of curved screens and flexible screen products, the research on flexible wearable devices is also widely researched. However, the technology adopted for preparing the flexible wearable device is still the traditional processes of spin coating, evaporation and the like.
The dipping and pulling method has the unique advantages of high material utilization rate, simple operation and the like in various preparation processes, and is particularly suitable for preparing fibrous wearable flexible devices. At present, the fiber-shaped light-emitting devices are mainly divided into two types from the device structure: one type is an ac driven light emitting device, for example, the literature (adv. mater, 2016,28,4490.) uses ZnS: mn and other materials as a luminescent material have the defects of high driving voltage, uneven luminescence and the like; another type is a light emitting diode using an organic material, and for example, the literature (nat. photo, 2015,9,233., Nano lett.,2018,18, 347) uses an organic material as a light emitting material, but has disadvantages of a wide emission peak, an expensive material, and the like. These drawbacks have hindered the development of flexible, high definition electroluminescent devices. Therefore, it is urgently needed to develop a preparation method of a quantum dot fiber light-emitting device which is suitable for high quality, wide color gamut, high repetition rate, simple process and low cost.
Disclosure of Invention
The invention aims to provide a wide-color-gamut fibrous CsPbX mainly based on a full-solution method of dip-drawing3A preparation method of a full solution of an inorganic perovskite quantum dot light-emitting diode.
The technical scheme for realizing the purpose of the invention is as follows:
the preparation method of the full solution of the fibrous inorganic perovskite quantum dot light-emitting diode comprises the following specific steps:
step 2, depositing a hole transport layer solution on the surface of the hole injection layer by adopting a dip-coating method, and carrying out heat treatment at the temperature of 100-150 ℃ to obtain a hole transport layer;
step 3, CsPbX is processed by adopting a dipping pulling method3Depositing a luminescent layer solution formed by mixing inorganic perovskite quantum dots, a small molecular material and a polymer material on the surface of the hole transport layer, and carrying out heat auxiliary treatment at 70-120 ℃ to obtain a luminescent layer;
in the step 4, depositing the electron transport layer on the surface of the light-emitting layer by adopting a dip-coating method to obtain the electron transport layer;
in step 5, thermally evaporating and depositing an electrode material on the surface of the electron transport layer to obtain fibrous CsPbX3An inorganic perovskite quantum dot light emitting diode.
In step 1, the flexible fiber is flexible fiber conventionally used in the art, and may be polyester fiber (PET), polyvinyl alcohol fiber (PVA), or the like.
In the step 1, the concentration of the poly (ethylenedioxythiophene) -poly (styrenesulfonate) solution is 1.3-1.7 wt%.
In step 2, the hole transport layer solution is a hole transport layer material conventionally used in the art, and may be selected from poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine ], poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine ] or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ]; the deposition thickness is 20-100 nm.
In step 3, CsPbX3X in the quantum dots is any one or combination of Cl, Br and I, CsPbX3The solvent adopted by the quantum dot dispersion liquid is selected from toluene, tetrahydrofuran or chloroform, and the concentration of the dispersion liquid is 10-30 mg/mL.
In step 3, the small molecule material is selected from 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, 2' - (1, 3-phenyl) bis [5- (4-tert-butylphenyl) -1,3, 4-oxadiazole ], 1,3, 5-tri [ (3-pyridyl) -3-phenyl ] benzene or 2- (4-biphenyl) -5-phenyl-1, 3, 4-oxadiazole, which is conventionally used in the art.
In step 3, the polymer material is a polymer material conventionally used in the art, and may be selected from poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine ], poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine ], or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ].
In step 4, the electron transport layer is made of an electron transport layer material conventionally used in the art, and may be selected from 1,3, 5-tris [ (3-pyridyl) -3-phenyl ] benzene or 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene.
In the step 4, the deposition thickness of the electron transport layer is 30-100 nm.
In the step 5, the electrode material is conventionally used in the field, and can be LiF/Al, Liq/Al and the like, and the deposition thickness is 1 nm/80-100 nm.
Compared with the prior art, the invention has the following advantages:
1) the invention adopts the dipping and pulling method, has simple process, high material utilization rate and low cost;
2) compared with the traditional light-emitting diode, the fibrous inorganic perovskite light-emitting diode prepared by the invention has higher light extraction efficiency and higher color purity compared with a fibrous light-emitting device based on an organic material and an alternating current driven fibrous light-emitting device.
Drawings
FIG. 1 is a scanning electron micrograph of the electrode layer thin film prepared in example 1.
FIG. 2 is a schematic process flow diagram of the present invention.
Fig. 3 is an electroluminescence spectrum of the fibrous quantum dot light emitting diode prepared in example 1.
Fig. 4 is a color coordinate diagram of the fibrous quantum dot light emitting diode prepared in example 1.
Fig. 5 is a picture of an electroluminescent material of the fiber quantum dot light-emitting diode prepared in example 1.
Fig. 6 is a light emission spectrum of the fibrous quantum dot light emitting diode prepared in example 4.
Fig. 7 is a picture of an electroluminescent real object of the fibrous quantum dot light-emitting diode prepared in comparative example 1.
Detailed Description
The invention is further described below by means of specific examples and figures.
Example 1
The fibrous inorganic perovskite quantum dot light-emitting diode specifically comprises the following steps:
1) depositing poly (ethylenedioxythiophene) -poly (styrene sulfonate) solution on clean PET fiber by a dip-coating method, and carrying out heat treatment at 90 ℃. A hole injection layer film was deposited to a thickness of 300nm as shown in fig. 1.
2) Pulling and depositing the solution of [ bis (4-phenyl) (4-butylphenyl) amine ], performing heat treatment at 100 ℃, and depositing a hole transport layer with a thickness of 20nm to 50 nm;
3) CsPbBr by pulling deposition3Perovskite quantum dots, poly [ bis (4-phenyl) (4-butylphenyl) amine]And 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, and depositing a light-emitting layer having a thickness of 50nm by heat treatment at 70 ℃;
4) carrying out lift deposition on 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene to deposit an electron transport layer with the thickness of 60 nm;
5) the electrode material LiF/Al was deposited by thermal evaporation to a thickness of 1/100 nm.
Example 2
Analogously to example 1, except for the poly [ bis (4-phenyl) (4-butylphenyl) amine in step 2) of example 1]Poly (9-vinyl carbazole) is changed, other conditions are kept consistent, and fibrous CsPbX is prepared3An inorganic perovskite quantum dot light emitting diode.
Example 3
Analogously to example 1, except for the poly [ bis (4-phenyl) (4-butylphenyl) amine in step 2) of example 1]Modified poly [ bis (4-phenyl) (4-butylphenyl) amine]The other conditions are kept consistent, and the fibrous CsPbX is prepared3An inorganic perovskite quantum dot light emitting diode.
Example 4
Similar to example 1, except that CsPbBr in step 3) of example 1 was added3Modified to CsPbI3The other conditions are kept consistent, and the fibrous CsPbX is prepared3An inorganic perovskite quantum dot light emitting diode.
The corresponding luminescence spectrum is shown in fig. 6.
Example 5
Similar to example 1, except that the heat treatment temperature in step 1) of example 1 was changed to 140 ℃, the heat treatment temperature in step 2) was changed to 140 ℃, and the heat treatment temperature in step 3) was changed to 100 ℃. Other conditions are kept consistent, and the fibrous CsPbX is prepared3An inorganic perovskite quantum dot light emitting diode.
Fibrous CsPbX3The schematic diagram of the preparation process of the inorganic perovskite quantum dot light-emitting diode is shown in fig. 2.
The above embodiments are merely representative embodiments. It should be understood that, in the present invention, the flexible fiber used in step 1 is a flexible fiber conventionally used in the art, and may be polyester fiber (PET), polyvinyl alcohol fiber (PVA), etc., and the above example takes PET as an example. The concentration of the poly (ethylenedioxythiophene) -poly (styrenesulfonate) solution is in the concentration range conventionally used in the field, specifically 1.3-1.7 wt%. The hole transport layer solution adopts a hole transport layer material conventionally used in the field, and can be selected from poly (9-vinyl carbazole), poly [ bis (4-phenyl) (4-butyl phenyl) amine]Poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine]Or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]The deposition thickness is 20-100 nm. CsPbX3X in the quantum dots is any one or combination of Cl, Br and I, CsPbX3The solvent adopted by the quantum dot dispersion liquid is selected from toluene, tetrahydrofuran or chloroform, and the concentration of the dispersion liquid is 10-30 mg/mL. The small molecular material is conventionally used in the field and can be selected from 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, 2' - (1, 3-phenyl) di [5- (4-tert-butylphenyl) -1,3, 4-oxadiazole]1,3, 5-tris [ (3-pyridyl) -3-phenyl)]Benzene or 2- (4-biphenyl) -5-phenyl-1, 3, 4-oxadiazole, the above examples taking 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene as an example. The polymer material is a polymer material conventionally used in the field and can be selected from poly (9-vinyl carbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine]Poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine]Or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]The above examples use poly [ bis (4-phenyl) (4-butylphenyl) amine]For example. The electron transport layer is made of electron transport layer material conventionally used in the art and can be selected from 1,3, 5-tri [ (3-pyridyl) -3-phenyl)]Benzene or 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene, and the deposition thickness is 30-100 nm. The electrode material is conventionally used in the field, and can be LiF/Al, Liq/Al and the like, and the deposition thickness is 1 nm/80-100 nm. Under the above conditions, the fibrous CsPbX prepared in each example3The performances of the inorganic perovskite quantum dot light-emitting diode are similar, the electroluminescent spectrum is basically as shown in figure 3, the full width at half maximum is 23nm, the width is narrower than that of a common green organic light-emitting material, and the inorganic perovskite quantum dot light-emitting diode has higher color purity. The color coordinate (CIE1931) diagram is shown in fig. 4, where the color coordinate is closer to pure green. The electroluminescent real image is shown in fig. 5, and it can be seen from the image that the luminescence is uniform.
Comparative example 1
Similar to example 1, except that the mixed light-emitting layer in step 3) of example 1 was changed to pure CsPbX3The perovskite quantum dots are kept consistent with other conditions to prepare the fibrous CsPbX3An inorganic perovskite quantum dot light emitting diode. The luminous material object is shown in figure 7The device has poor luminous performance, difficult measurement, short service life, uneven luminescence and a spectrum with a mixed peak, and is reflected in that a real object luminous image is not pure green.
Claims (10)
1. The preparation method of the full solution of the fibrous inorganic perovskite quantum dot light-emitting diode is characterized by comprising the following specific steps of:
step 1, depositing a poly (ethylenedioxythiophene) -poly (styrene sulfonate) solution on a clean flexible fiber by adopting a dip-coating method, and carrying out heat treatment at 90-140 ℃ to obtain a hole injection layer with the thickness of 100-500 nm;
step 2, depositing a hole transport layer solution on the surface of the hole injection layer by adopting a dip-coating method, and carrying out heat treatment at the temperature of 100-150 ℃ to obtain a hole transport layer;
step 3, CsPbX is processed by adopting a dipping pulling method3Depositing a luminescent layer solution formed by mixing inorganic perovskite quantum dots, a small molecular material and a polymer material on the surface of the hole transport layer, and carrying out heat auxiliary treatment at 70-120 ℃ to obtain a luminescent layer;
in the step 4, depositing the electron transport layer on the surface of the light-emitting layer by adopting a dip-coating method to obtain the electron transport layer;
in step 5, thermally evaporating and depositing an electrode material on the surface of the electron transport layer to obtain fibrous CsPbX3An inorganic perovskite quantum dot light emitting diode.
2. The method according to claim 1, wherein in step 1, the flexible fibers are selected from polyester fibers or polyvinyl alcohol fibers; the concentration of the poly (ethylenedioxythiophene) -poly (styrene sulfonate) solution is 1.3-1.7 wt%.
3. The method according to claim 1, wherein in step 2, the hole transport layer is selected from poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine ], poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine ], or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ]; the deposition thickness is 20-100 nm.
4. The method according to claim 1, wherein in step 3, the CsPbX is added3X in the quantum dots is any one or combination of Cl, Br and I, CsPbX3The solvent adopted by the quantum dot dispersion liquid is selected from toluene, tetrahydrofuran or chloroform, and the concentration of the dispersion liquid is 10-30 mg/mL.
5. The method according to claim 1, wherein in step 3, the small molecule material is selected from 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, 2' - (1, 3-phenyl) bis [5- (4-tert-butylphenyl) -1,3, 4-oxadiazole ], 1,3, 5-tris [ (3-pyridyl) -3-phenyl ] benzene or 2- (4-biphenyl) -5-phenyl-1, 3, 4-oxadiazole.
6. The method according to claim 1, wherein in step 3, the polymer material is selected from poly (9-vinylcarbazole), poly [ bis (4-phenyl) (4-butylphenyl) amine ], poly [ (9, 9-di-n-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (4-n-butyl) phenyl) -diphenylamine ], and poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ].
7. The method according to claim 1, wherein in step 4, the electron transport layer is selected from 1,3, 5-tris [ (3-pyridyl) -3-phenyl ] benzene or 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene.
8. The method according to claim 1, wherein the electron transport layer is deposited to a thickness of 30 to 100nm in step 4.
9. The preparation method according to claim 1, wherein in the step 5, the electrode material is LiF/Al or Liq/Al, and the deposition thickness is 1 nm/80-100 nm.
10. The fibrous inorganic perovskite quantum dot light-emitting diode prepared by the preparation method according to any one of claims 1 to 9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111952474A (en) * | 2020-08-18 | 2020-11-17 | 福州大学 | Quantum dot light-emitting diode based on organic matter polymerization and preparation method thereof |
| CN112186117A (en) * | 2020-11-26 | 2021-01-05 | 江汉大学 | Alternating current driving type quantum dot light-emitting diode and preparation method thereof |
| WO2022214038A1 (en) * | 2021-04-07 | 2022-10-13 | 浙江光昊光电科技有限公司 | Mixture and application thereof in photoelectric field |
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2018
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111952474A (en) * | 2020-08-18 | 2020-11-17 | 福州大学 | Quantum dot light-emitting diode based on organic matter polymerization and preparation method thereof |
| CN111952474B (en) * | 2020-08-18 | 2023-11-03 | 福州大学 | Quantum dot light emitting diode based on organic matter polymerization and preparation method thereof |
| CN112186117A (en) * | 2020-11-26 | 2021-01-05 | 江汉大学 | Alternating current driving type quantum dot light-emitting diode and preparation method thereof |
| WO2022214038A1 (en) * | 2021-04-07 | 2022-10-13 | 浙江光昊光电科技有限公司 | Mixture and application thereof in photoelectric field |
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