CN112467044B - Rare earth electro-induced deep blue light device - Google Patents
Rare earth electro-induced deep blue light device Download PDFInfo
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Abstract
The invention belongs to the field of photoelectric devices, and discloses a rare earth electro-generated deep blue light device which sequentially comprises a top electrode, an electron transport layer, a light-emitting layer, a hole transport layer and a bottom electrode from top to bottom, wherein the light-emitting layer is made of Eu-based perovskite material, Eu element occupies perovskite ABX in the Eu-based perovskite material3B site in the structure and does not contain Pb; the electron transport layer and the hole transport layer serve to localize electrons or holes in the light emitting layer and to adjust injection balance of the electrons and holes. The invention is achieved by using Eu-based perovskite-type materials (e.g., CsEuBr)3) The rare earth electro-generated deep blue light device is constructed as a luminescent layer material, and the material is an inorganic material, so that the rare earth electro-generated deep blue light device is good in stability, difficult to age and long in service life, can broaden the color gamut of the existing display, and solves the technical problem that the blue light color distortion is easily caused by poor stability and easy aging of an OLED (organic light emitting diode).
Description
Technical Field
The invention belongs to the field of photoelectric devices, and particularly relates to a rare earth electro-generated deep blue light device, which is particularly suitable for deep blue electro-luminescence in a wavelength range of 420nm to 450 nm.
Background
The high-efficiency and stable electro blue light (blue light LED) technology is an important point and difficulty to be overcome in the scientific research and industrial circles, and has great scientific research and application values and great national strategic significance. Currently, displays based on Organic Light Emitting Diodes (OLEDs) are becoming the mainstream advanced display technology and occupy the middle and high-end display market. However, the OLED display still suffers from the low efficiency and short lifetime of the blue light device, the external quantum efficiency of the blue light LED in the AMOLED display is less than 10%, and the lifetime of the blue light LED is less than one tenth of that of the red and green LEDs under the same brightness, which leads to the serious color shift problem of the display after long-time operation. And the core OLED materials and patents are mostly held in the united states, korea and japan (UDC, samsung in korea, japanese shinning), which severely restricts the national strategic goals of rapid development and surpassing in the advanced display field. Although the emerging blue light quantum dot light emitting diode (QLED) is developed rapidly, the quantum dot contains cadmium, the current immature printing process is needed, and the stability does not reach the standard; blue perovskite light emitting diodes (pelds) still have a lack of efficiency, spectral stability and operational stability are a great distance away from practical use, and commercial application is difficult to achieve in a short period of time. Therefore, the electro-blue technology needs a new breakthrough to meet the urgent requirements of high efficiency and high stability.
Disclosure of Invention
In view of the above-mentioned drawbacks or needs for improvement of the prior art, it is an object of the present invention to provide a rare earth electroluminescent deep blue light device by using a Eu-based perovskite type material (Eu element occupying perovskite ABX)3B site in the structure and does not contain Pb; such as CsEuBr3) The material is an inorganic material, so that the rare earth electro-generated deep blue light device has good stability, is not easy to age and has long service life; in addition, the invention preferably adopts a method of passivating the grain boundary, thereby effectively inhibiting defect luminescence and obtaining pure deep blue light emission with narrower half-peak width. The invention can widen the color gamut of the existing display and solve the technical problems that the OLED has poor stability and is easy to age and easily causes blue light color distortion. Compared with other rare earth materials, the invention has higher laser mobility, can realize large charge injection, has advantages in stability and nontoxicity compared with Pb-based perovskite materials, and is an ideal deep blue electroluminescent device.
To achieve the above object, according to the present invention, there is provided a rare earth electro-deep blue light device comprising, in order from top to bottom, a top electrode, an electron transport layer, a light emitting layer, a hole transport layer, and a bottom electrode, wherein,the material adopted by the luminescent layer is Eu-based perovskite material; in the Eu-based perovskite type material, Eu occupies perovskite ABX3B site in the structure and does not contain Pb;
the electron transport layer and the hole transport layer serve to localize electrons or holes in the light emitting layer and to adjust injection balance of the electrons and holes.
As a further preferred aspect of the present invention, the Eu-based perovskite-type material is CsEuBr3A material.
As a further preferred aspect of the invention, said CsEuBr3Material coating Cs4EuBr6And (5) passivating the material.
As a further preferred aspect of the present invention, said Cs for passivation4EuBr6Materials and said CsEuBr3The molar ratio of the materials is (10-20%): 1.
as a further preferred mode of the present invention, the luminescent layer is prepared by a dual-source co-evaporation method using CsBr and EuBr as evaporation sources2。
As a further preferred aspect of the present invention, the hole transport layer is made of an inorganic hole transport layer material; preferably NiOx or MoO3The material, x, satisfies 1 to 3/2.
As a further preferred aspect of the present invention, the electron transport layer is made of an organic electron transport material; TPBi or Bphen materials are preferably used.
As a further preferred aspect of the present invention, the top electrode is a LiF-modified Al electrode.
In a further preferred embodiment of the present invention, the bottom electrode is an ITO electrode.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a rare earth electro-generated deep blue light device, wherein the material of a light-emitting layer is Eu-based perovskite type material, such as CsEuBr3A material; the material is an inorganic material, and has good stability, difficult aging and long service life. Meanwhile, the material has high mobility and is suitable for being used as a light emitting layer of an electroluminescent material. Hair of corresponding deviceThe radiation wavelength is 440nm, and the deep blue electroluminescent device is particularly suitable for deep blue electroluminescence in the wavelength range of 420nm to 450nm (the color gamut of deep blue light is wider than that of the blue light which is produced). The method can prepare CsEuBr by using a double-source co-evaporation thermal evaporation method3Luminescent materials, and especially Cs4EuBr6Passivated CsEuBr3Luminescent material is prepared into a film electroluminescent device.
2. Compared with the traditional OLED material, the luminescent layer material of the rare earth electro-deep blue device provided by the invention has higher mobility which is about 0.1-1cm2the/V.s, about 1-2 orders of magnitude higher than OLEDs, is expected to achieve higher injection and greater brightness. The defect that the brightness of the existing OLED is inferior to that of the traditional electrodeless luminescent material can be overcome.
3. The invention also preferably utilizes suitable hole transport layers and electron transport layers to achieve a highly efficient electroluminescent device. According to the rare earth electro-deep blue light device provided by the invention, preferably, NiOx is used as a hole transport layer, TPBi is used as an electron transport layer, and considering that a conduction band is dominated by a d orbit of Eu, a valence band is dominated by an f orbit of Eu, the f orbit is local to the d orbit, the mobility of electrons is far higher than that of holes, the mobility of an electrodeless transport layer is higher than that of an organic transport layer, and hole transport with high mobility and electron transport with low mobility are selected, so that injection balance can be effectively adjusted, and efficiency is improved.
4. The rare earth electro-generated deep blue light device provided by the invention can effectively widen the color gamut, and meanwhile, has the advantages of high brightness, high purity, long service life, no toxicity, no harm and the like.
5. The luminescent layer of the rare earth blue electroluminescent device provided by the invention can be prepared by adopting a thermal evaporation method, and can be effectively and controllably prepared by combining with the existing OLED industry chain.
The invention can especially adopt a double-source co-evaporation thermal evaporation method to prepare the quilt Cs4EuBr6Material passivated CsEuBr3The material is used as a luminescent layer, the process is simple, and the evaporation source is preferably CsBr and EuBr2. Compared with pure CsEuBr3Material, the present invention additionally adds Cs4EuBr6Second phase, CsBr and EuBr during double-source co-evaporative evaporation2The molar ratio of (a) needs to be more than 1: 1 (i.e., excess CsBr), and the evaporation sources CsBr and EuBr can be easily adjusted by double-source co-evaporation2To further control CsEuBr3Materials and Cs4EuBr6The proportions of the materials. Cs4EuBr6The material belongs to a low-dimensional material (the electron and hole have stronger locality), and encapsulates CsEuBr3The light-emitting diode is easier to play a role in limiting the area and enhance the light emission. The most obvious disadvantage of thermal evaporation processes is the tendency to generate vacancy defects, such as EuBr2The substance is not EuBr2This structure is evaporated, possibly in the form of EuBr +, which facilitates the formation of halogen vacancies, excess CsBr reducing the concentration of such vacancies, passivating CsEuBr3And (5) a defect. Taking into account the heating required during the deposition of the light-emitting layer (CsEuBr)3The deposition film needs higher crystallization temperature), the deposited substrate needs certain heat resistance, and the invention preferably adopts inorganic hole transport materials to realize the substrate with better heat resistance.
The mobility of holes and electrons of the luminescent material of the invention is different by two orders of magnitude (with CsEuBr)3For example, the electron mobility is 0.5cm2V.s, hole mobility 0.03cm2V · s), it is preferable to use an inorganic hole transport layer having a higher mobility and an electron transport layer having a lower mobility to balance the injection and adjust the recombination region so that the electron mobility is too fast and the recombination region reaches the hole transport layer to roll off the efficiency. According to the invention, through the design of a top electrode-electron transport layer-luminescent layer-hole transport layer-bottom electrode layer structure from top to bottom, the electron mobility of the luminescent layer material is higher than the hole mobility, and the electron hole recombination zone is mainly at the interface of the hole transport layer, so that the arrangement of the hole transport layer below the luminescent layer is beneficial to the arrangement of the hole transport layerThe invention can regulate and control on the hole transport layer, for example, an electron blocking layer and the like can be added. With CsEuBr3For example, since the electron mobility is 0.5cm2V.s, hole mobility 0.03cm2The top electrode, the electron transport layer, the luminescent layer, the hole transport layer and the bottom electrode are arranged from top to bottom, preferably, the inorganic hole transport layer and the organic electron transport layer are arranged, and the injection of carriers can be balanced more effectively by utilizing the characteristic that the inorganic material has stronger transport capability to corresponding carriers compared with the organic material (namely, the inorganic hole transport layer has stronger transport capability to holes and the organic electron transport layer has weaker transport capability to electrons). Further, the present invention may preferably be carried out by using Cs4EuBr6The material passivates Eu-based perovskite type material, and the Cs for passivation4EuBr6Materials and hosts CsEuBr3The molar ratio of the material can be preferably 10-20%, defects can be further effectively passivated, and carriers can be limited, so that the recombination rate of the carriers is improved.
The invention uses inorganic material to form the luminescent layer and the inorganic hole transport layer, and has better stability, especially thermal stability, and can widen the working temperature range compared with organic material. Compared with OLED, the OLED has lower blue light application efficiency and shorter service life, and the invention uses inorganic material as the light-emitting layer, the inorganic material is more stable than organic material, the heat-resisting range is higher, the fluorescence quenching is more stable, and the working temperature range is higher. The maximum efficiency is verified to reach 10%, while the exciton utilization rate of the material is theoretically 100%, because the existence of single triplet state is higher than the maximum theoretical efficiency of 25% of the current organic fluorescent LED material. Whereas with QLED, the QLED printing process is immature; based on the invention, the evaporation process and the OLED production line can be combined, and the method is more beneficial to industrial production. Compared with the PeLED, the invention can greatly improve the efficiency and stability.
Drawings
Fig. 1 is a structural diagram of a rare earth electro-deep blue light device according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a dual-source co-evaporation of materials according to an embodiment of the present invention.
FIG. 3 shows example 1 of the present invention (i.e., CsEuBr)3Is coated with 10 mol% of Cs4EuBr6Passivating) provided CsEuBr3Spectrogram in the electroluminescent state.
FIG. 4 shows CsEuBr provided in example 1 of the present invention3Performance diagram of an electro-blue device as a luminescent layer material.
FIG. 5 shows Cs used in example 1 of the present invention4EuBr6Spectra before and after passivation of defects.
FIG. 6 is a spectrum diagram of example 1 of the present invention at different voltages and a CIE diagram thereof (the voltage condition has little effect on the CIE diagram).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The rare earth electroluminescent deep blue light device in the invention, as shown in fig. 1, comprises: a top electrode, an electron transport layer, a luminescent layer, a hole transport layer and a bottom electrode;
wherein, the top electrode material can be an Al electrode modified by LiF;
the material of the luminescent layer is Eu-based perovskite material; in the Eu-based perovskite-type material, Eu occupies perovskite ABX3B site in the structure and does not contain Pb;
the electron transport layer and the hole transport layer are used for locally locating electrons or holes in the light-emitting layer and regulating the injection balance of the electrons and the holes;
the bottom electrode is an ITO electrode and can be a substrate obtained by etching an ITO substrate.
Referring to the prior art, as shown in fig. 2, the evaporation method of the light-emitting layer adopts a double-source co-evaporation method to obtain the target material through a crystal growth reaction deposited on the substrate.
The present invention will be described in detail below by taking the apparatus of Fangji FS-300 as an example of the dual source co-evaporation.
Examples 1,
This example uses the luminescent layer material as the passivated CsEuBr3The preparation method of the electroluminescent blue light device comprises the following steps:
a) ultrasonically cleaning a substrate ITO by using detergent, deionized water, acetone and absolute ethyl alcohol in sequence, wherein each time is half an hour; wherein, the ITO adopts two etched substrates, and the light-emitting area of the ITO is about 2mm x 2 mm;
b) sputtering Li-doped p-type NiO with the thickness of about 40nm on ITO by adopting a magnetron sputtering method, wherein the doping concentration is 1016-1017cm-3；
c) Putting the NiO film plated substrate into an evaporation glove box, and pumping the vacuum degree to 4 x 10-5Heating the substrate to 200 deg.C below Pa, and evaporating EuBr at 0.11nm/s by co-evaporation2CsBr was evaporated at a rate of 0.14nm/s, and a thickness of 100nm was co-evaporated. In the dual source co-evaporation process, two phases are formed by the reaction of excess Cs with Eu, i.e., CsEuBr, using a spontaneous crystallization process3Phase with Cs4EuBr6Phase, thereby forming a coated Cs4EuBr6Passivated CsEuBr3。
d) Taking the wafer, replacing TPBi, and evaporating TPBi with the thickness of 20nm at the speed of 0.01-0.02 nm/s.
e) Transferring the device to a thermal evaporation device, evaporating a 1nm LiF film at a speed of 0.1nm/s, and evaporating at a speed of 5 x 10 at a speed of 1nm/s-4And (4) evaporating an Al film with the thickness of 600nm under the condition of Pa or less to obtain the finished device.
The obtained device has the following detection results:
as shown in FIG. 3, the peak position of the emission was 440nm and the half-value width was 31 nm.
As shown in fig. 4, the device efficiency has been supported by preliminary experimental data and can work well.
As shown in FIG. 5, Cs was used4EuBr6The passivation can be effectively inhibited inDefects generated in the process of film evaporation. And defective luminescence is reduced.
As shown in fig. 6, the device has stable spectral shape under different voltages, and its CIE coordinate (0.15, 0.04) value is smaller than that of conventional blue light around 470nm, so that it is easy to form a wider color gamut area with the existing red and green lights.
Also, since CsEuBr is known in the prior art3The material has good thermal stability, and is beneficial to the service life and stability of devices.
Examples 2,
This example uses the luminescent layer material as the passivated CsEuBr3The preparation method of the electroluminescent blue light device comprises the following steps:
a) ultrasonically cleaning a substrate ITO by using detergent, deionized water, acetone and absolute ethyl alcohol in sequence, wherein each time is half an hour; wherein, the ITO adopts two etched substrates, and the light-emitting area of the ITO is about 2mm x 2 mm;
b) sputtering Li-doped p-type NiO with the thickness of about 40nm on ITO by adopting a magnetron sputtering method, wherein the doping concentration is 1016-1017cm-3；
c) Putting the NiO film plated substrate into an evaporation glove box, and pumping the vacuum degree to 4 x 10-5Heating the substrate to 200 deg.C below Pa, and evaporating EuBr at 0.12nm/s by co-evaporation2CsBr was evaporated at a rate of 0.18nm/s, and a thickness of 100nm was co-evaporated.
d) Taking the wafer, replacing TPBi, and evaporating TPBi with the thickness of 20nm at the speed of 0.01-0.02 nm/s.
e) Transferring the device to a thermal evaporation device, evaporating a 1nm LiF film at a speed of 0.1nm/s, and evaporating at a speed of 5 x 10 at a speed of 1nm/s-4And (4) evaporating an Al film with the thickness of 600nm under the condition of Pa or less to obtain the finished device.
Examples 3,
This example uses the luminescent layer material as the passivated CsEuBr3The preparation method of the electroluminescent blue light device comprises the following steps:
a) ultrasonically cleaning a substrate ITO by using detergent, deionized water, acetone and absolute ethyl alcohol in sequence, wherein each time is half an hour; wherein, the ITO adopts two etched substrates, and the light-emitting area of the ITO is about 2mm x 2 mm;
b) sputtering Li-doped p-type NiO with the thickness of about 40nm on ITO by adopting a magnetron sputtering method, wherein the doping concentration is 1016-1017cm-3；
c) Putting the NiO film plated substrate into an evaporation glove box, and pumping the vacuum degree to 4 x 10-5Heating the substrate to 200 deg.C below Pa, and evaporating EuBr at 0.115nm/s by co-evaporation2CsBr was evaporated at a rate of 0.16nm/s, and a thickness of 100nm was co-evaporated.
d) Taking the wafer, replacing TPBi, and evaporating TPBi with the thickness of 20nm at the speed of 0.01-0.02 nm/s.
e) Transferring the device to a thermal evaporation device, evaporating a 1nm LiF film at a speed of 0.1nm/s, and evaporating at a speed of 5 x 10 at a speed of 1nm/s-4And (4) evaporating an Al film with the thickness of 600nm under the condition of Pa or less to obtain the finished device.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. The rare earth electro-induced deep blue light device is characterized by being used for realizing deep blue electro-luminescence within the wavelength range of 420nm-450nm and sequentially comprising a top electrode, an electron transport layer, a light-emitting layer, a hole transport layer and a bottom electrode from top to bottom, wherein the light-emitting layer is made of Eu-based perovskite type material; in the Eu-based perovskite type material, Eu occupies perovskite ABX3B site in the structure and does not contain Pb;
the electron transport layer and the hole transport layer are used for localizing electrons or holes in the light-emitting layer and adjusting the injection balance of the electrons and the holes;
the Eu-based perovskite type material is CsEuBr3A material;
the CsEuBr3Material coating Cs4EuBr6Passivating the material; the Cs for passivation4EuBr6Materials and said CsEuBr3The molar ratio of the materials is (10-20%): 1.
2. the rare earth electroluminescent deep blue light device as claimed in claim 1, wherein the light-emitting layer is prepared by a dual-source co-evaporation method using CsBr and EuBr as evaporation sources2。
3. The rare earth electro-deep blue light device as claimed in claim 1, wherein the hole transport layer is made of an inorganic hole transport layer material.
4. The rare earth electro-deep blue device as claimed in claim 3, wherein said hole transport layer is NiOx or MoO3The material, x, satisfies 1 to 3/2.
5. The rare earth electro-deep blue light device as claimed in claim 1, wherein the electron transport layer is made of an organic electron transport material.
6. The rare earth electro-deep blue device as claimed in claim 5, wherein the electron transport layer is made of TPBi or Bphen material.
7. The rare earth electro-deep blue device of claim 1, wherein the top electrode is a LiF-modified Al electrode.
8. The rare earth electro-deep blue device as claimed in any one of claims 1 to 7, wherein the bottom electrode is an ITO electrode.
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| CN109054806A (en) * | 2018-08-09 | 2018-12-21 | 华南理工大学 | The metal halogen perovskite quantum dot and its preparation method and application of FAX modification |
| WO2020012194A1 (en) * | 2018-07-13 | 2020-01-16 | Oxford University Innovation Limited | Tunable blue emitting lead halide perovskites |
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| WO2020012194A1 (en) * | 2018-07-13 | 2020-01-16 | Oxford University Innovation Limited | Tunable blue emitting lead halide perovskites |
| CN109054806A (en) * | 2018-08-09 | 2018-12-21 | 华南理工大学 | The metal halogen perovskite quantum dot and its preparation method and application of FAX modification |
| CN111834501A (en) * | 2020-06-16 | 2020-10-27 | 华中科技大学 | Rare earth electro-induced blue light device |
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| Blue electroluminescent metal halide perovskites;Sudhir Kumar等;《JOURNAL OF APPLIED PHYSICS》;20200928;第128卷(第12期);第120901页 * |
| Eu2+: A suitable substituent for Pb2+ in CsPbX3 perovskite nanocrystals?;Firoz Alam等;《JOURNAL OF CHEMICAL PHYSICS》;20191217;第151卷(第23期);第231101页 * |
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