CN116367681A - Method for testing and screening decay rate of light-emitting device - Google Patents

Method for testing and screening decay rate of light-emitting device Download PDF

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CN116367681A
CN116367681A CN202111611835.7A CN202111611835A CN116367681A CN 116367681 A CN116367681 A CN 116367681A CN 202111611835 A CN202111611835 A CN 202111611835A CN 116367681 A CN116367681 A CN 116367681A
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light
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林雄风
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TCL Technology Group Co Ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • H10K50/115OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
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Abstract

The application provides a test method and a screening method of a light-emitting device attenuation rate, wherein the test method is characterized in that a solution to be tested containing a material of a light-emitting layer, a material of a carrier transmission layer and a free radical indicator is provided, then quantum dots in the light-emitting layer are excited by illumination and react with the material of the carrier transmission layer to generate free radicals, and the concentration of the free radicals in the solution to be tested is represented by the free radical indicator, so that the test of the quantum dot light-emitting diode attenuation rate is realized.

Description

Method for testing and screening decay rate of light-emitting device
Technical Field
The application relates to the field of photoelectric devices, in particular to a testing method and a screening method for attenuation rate of a light-emitting device.
Background
QLED (Quantum Dots Light-emission Diode) is an emerging display device, which has a structure similar to OLED (Organic Light-emission Diode), that is, a sandwich structure composed of a hole transport layer, a Light Emitting layer, and an electron transport layer. This is a new technology between liquid crystal and OLED, the QLED core technology is "Quantum Dot" which is composed of zinc, cadmium, selenium and sulfur atoms. As early as 1983, scientists in the bell laboratories in the united states conducted intensive studies, and after a few years, the physicist mark-reed at the university of us formally named "quantum dots". The quantum dot is a particle with particle diameter less than 10nm, and is composed of zinc, cadmium, sulfur and selenium atoms. This material has an extremely specific property: when the quantum dot is stimulated by photoelectricity, colored light is emitted, and the color is determined by the materials composing the quantum dot and the size and shape of the quantum dot. Because of this property, it is possible to change the color of the light emitted from the light source. The light-emitting wavelength range of the quantum dots is very narrow, the color is pure, and the color can be adjusted, so that the picture of the quantum dot display is clearer and brighter than that of the liquid crystal display.
Compared with OLED, QLED has the characteristic that the luminescent material adopts inorganic quantum dots with more stable performance. The unique quantum size effect, macroscopic quantum tunneling effect, quantum size effect and surface effect of quantum dots make them exhibit excellent physical properties, especially their optical properties. Compared with organic fluorescent dye, the quantum dot prepared by the colloid method has the advantages of adjustable spectrum, high luminous intensity, high color purity, long fluorescence life, capability of exciting multicolor fluorescence by a single light source, and the like. In addition, the QLED has long service life, simple packaging process or no need of packaging, and is expected to become a next-generation flat panel display, thereby having wide development prospect. QLED is electroluminescent based on inorganic semiconductor quantum dots, which theoretically have higher stability than small organic molecules and polymers; on the other hand, due to the quantum confinement effect, the light-emitting line width of the quantum dot material is smaller, so that the quantum dot material has better color purity. Currently, the light emitting efficiency of QLEDs has substantially reached the commercial demand.
However, the free radicals in QLEDs can have an impact on the device, and thus a method of characterizing the content of free radicals is needed.
Disclosure of Invention
The application provides a test method and a screening method for the decay rate of a light emitting device, which can be used for
In a first aspect, embodiments of the present application provide a method for testing a decay rate of a light emitting device, where the light emitting device includes a light emitting layer and a carrier transport layer, the method including:
providing a solution to be detected, wherein the solution to be detected comprises a material of the light-emitting layer, a material of the carrier transmission layer, a free radical indicator and an organic solvent, the material of the light-emitting layer comprises quantum dots, and the free radical indicator has the characteristic of representing the concentration of free radicals in the solution to be detected; and
and carrying out illumination treatment on the solution to be detected for a preset time to enable the material of the light-emitting layer and the material of the carrier transmission layer to react to generate free radicals, and obtaining the attenuation rate of the light-emitting device according to the representation of the concentration of the free radicals in the solution to be detected by the free radical indicator.
Optionally, the providing a solution to be tested includes:
in the light-emitting device, taking a sample of the light-emitting layer and a sample of the carrier transport layer with preset areas, and dispersing the sample of the light-emitting layer and the sample of the carrier transport layer in the organic solvent to obtain a dispersion liquid; and
and adding a free radical indicator into the dispersion liquid to obtain the solution to be detected.
Optionally, the performing light treatment on the solution to be detected for a predetermined time, and obtaining the attenuation rate of the light emitting device according to the representation of the concentration of the free radical in the solution to be detected by the free radical indicator includes: and carrying out illumination treatment on the solution to be detected for a preset time, detecting the absorbance of the free radical indicator in the solution to be detected under a specific wavelength, and obtaining the attenuation rate of the light emitting device according to the absorbance of the free radical indicator under the specific wavelength.
Optionally, the performing light treatment on the solution to be detected for a predetermined time, and obtaining the attenuation rate of the light emitting device according to the representation of the concentration of the free radical in the solution to be detected by the free radical indicator includes: carrying out illumination treatment on the solution to be detected for a preset time, and taking a plurality of time points in the preset time to detect the absorbance of the free radical indicator in the solution to be detected under a specific wavelength; calculating to obtain the clearance rate of the free radical indicator in the solution to be detected in a preset time according to the absorbance of the free radical indicator at a plurality of time points under a specific wavelength; and obtaining the decay rate of the light emitting device based on the scavenging rate of the free radical indicator.
Optionally, in the solution to be detected, the concentration of the radical indicator is 0.01mg/mL to 1mg/mL, and/or the total concentration of the material of the light emitting layer and the material of the carrier transporting layer is 0.001mg/mL to 1mg/mL.
Optionally, the free radical indicator is DPPH.
Optionally, the organic solvent is selected from methanol.
Optionally, the wavelength of the illumination is 400 nm-450 nm, and/or the predetermined time of the illumination treatment is 10 min-1 h.
Optionally, the light emitting device is a blue quantum dot light emitting diode.
Optionally, the carrier transport layer includes an electron transport layer, and/or a hole transport layer.
Optionally, the hole transport layer material includes: poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine), polyvinylcarbazole, poly (N, N '-bis (4-butylphenyl) -N, N' -bis (phenyl) benzidine), poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-phenylenediamine), 4',4 "-tris (carbazol-9-yl) triphenylamine, 4' -bis (9-carbazol) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, 15N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, graphene, C 60 At least one of, and/or,
the electron transport layer material includes: znO, tiO 2 、SnO 2 、Ta 2 O 3 、ZrO 2 At least one of NiO, tiLiO, znAlO, znMgO, znSnO, znLiO and InSnO; and/or the number of the groups of groups,
the light emitting layer is selected from at least one of II-VI compound, III-V compound and I-III-VI compound; the II-VI compound is at least one selected from CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSte; the III-V compound is at least one selected from InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of them.
In a second aspect, the present application provides a method for screening a light emitting device, the method comprising:
providing a plurality of light emitting devices;
the test method according to any embodiment of the first aspect is used to obtain the decay rate of each light emitting device, compare the decay rates of each light emitting device, and screen out the target light emitting device.
Optionally, the screening out the target light emitting device includes: and screening out the light-emitting devices with relatively slow decay rate from the plurality of light-emitting devices to obtain the target light-emitting device.
The beneficial effects are that:
the application provides a test method of a decay rate of a light emitting device, the light emitting device comprises a light emitting layer and a carrier transmission layer, and the decay rate of a quantum dot light emitting diode is related to free radicals.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings that are required to be used in the description of the embodiments will be briefly described below.
Fig. 1 is a flow chart of a method for testing a decay rate of a light emitting device according to an embodiment of the present disclosure;
fig. 2 is a schematic view of a front structure of a light emitting device according to an embodiment of the present application;
fig. 3 is a schematic view of an inverted structure of a light emitting device provided in an embodiment of the present application;
fig. 4 is a flowchart of a screening method of a light emitting device according to an embodiment of the present disclosure;
FIG. 5 is a schematic diagram of absorption spectra of test sample 1, test sample 2 and comparison sample at different times in dark environment according to the embodiment of the present application; in fig. 5, a is an absorption change curve of a comparative sample, b is an absorption change curve of a test sample 1, c is an absorption change curve of a test sample 2, and d is a change curve of the test sample after absorption normalization at 513nm along with illumination time;
FIG. 6 is a schematic diagram of absorption spectra of test sample 1, test sample 2 and comparison sample at different times under 400nm illumination provided in the examples of the present application; in fig. 6, a is the absorption change curve of the comparative sample, b is the absorption change curve of the test sample 1, c is the absorption change curve of the test sample 2, and d is the change curve of the test sample after absorption normalization at 513nm with the irradiation time.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
The embodiment of the application provides a test method and a screening method for the attenuation rate of a light-emitting device. The following will describe in detail. The following description of the embodiments is not intended to limit the preferred embodiments. In addition, in the description of the present application, the term "comprising" means "including but not limited to". Various embodiments of the present application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. Whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the range referred to.
First, as shown in fig. 1, an embodiment of the present application provides a method for testing a decay rate of a light emitting device, where the light emitting device includes a light emitting layer and a carrier transport layer, the method includes:
s10, providing a solution to be detected, wherein the solution to be detected comprises a material of the light-emitting layer, a material of the carrier transmission layer, a free radical indicator and an organic solvent, the material of the light-emitting layer comprises quantum dots, and the free radical indicator has the characteristic of representing the concentration of free radicals in the solution to be detected; and
s20, carrying out illumination treatment on the solution to be detected for a preset time, enabling the material of the light-emitting layer and the material of the carrier transmission layer to react to generate free radicals, and obtaining the attenuation rate of the light-emitting device according to the representation of the concentration of the free radicals in the solution to be detected by the free radical indicator.
The quantum dots have the common characteristics of large specific surface area and strong surface activity, so that OH and oxygen combined with other functional layers in an excited state are easy to generate free radicals with strong oxidability, and the existence of the free radicals can generate irreversible damage to organic matters in the device, so that the device is attenuated. However, the currently commonly used method for characterizing free radicals cannot reliably characterize the content of the free radicals, so that research on the influence of the content of the free radicals of the device on attenuation cannot be performed. It should be noted that, the decay rate in the embodiments of the present application does not refer to the decay rate of the device itself, but rather refers to the decay rate represented by other parameters (concentration of the free radical in the solution to be detected or other characterization parameters related to the concentration, such as absorbance or clearance rate of the free radical indicator). According to the embodiment of the application, the free radical content of the device and the decay rate of the device can be laterally represented by detecting the concentration of the free radical in the solution to be detected, so that the test of the decay rate of the light-emitting device is completed. After illumination, if the number of free radicals generated by the light emitting layer and the carrier transport layer in unit time is large, the concentration of the free radicals in the solution to be measured is high, which means that the free radical content of the device is high, the attenuation rate of the device is high, and if the number of free radicals generated by the light emitting layer and the carrier transport layer in unit time is small, the concentration of the free radicals in the solution to be measured is low, which means that the free radical content of the device is low, and the attenuation rate of the device is low.
The embodiment of the application provides a solution to be tested containing a material of a light emitting layer, a material of a carrier transport layer and a free radical indicator, and then utilizes illumination to excite quantum dots in the light emitting layer to form excitons, free electrons in the excitons are separated from holes and react with the material of the carrier transport layer to generate free radicals (if the material of the carrier transport layer is not present in the test, electrons and holes in an excited state cannot be converted into free radicals). The free radical indicator has the characteristic of representing the concentration of the free radical in the solution to be detected, so that the concentration of the free radical in the solution to be detected can be represented through the free radical indicator, the content of the free radical in the quantum dot light emitting diode is indirectly researched, and the test of the attenuation rate of the quantum dot light emitting diode is realized.
In some embodiments, the providing a solution to be tested includes:
s11, in the light-emitting device, taking a sample of the light-emitting layer and a sample of the carrier transmission layer with preset areas, and dispersing the sample of the light-emitting layer and the sample of the carrier transmission layer in the organic solvent to obtain dispersion liquid; and
s12, adding a free radical indicator into the dispersion liquid to obtain the solution to be detected.
In some embodiments, the free radical indicator has the characteristic of changing color with the reaction of the free radical, so when the free radical indicator is used as the free radical indicator, the concentration of the free radical in the solution to be detected can be represented by detecting the absorbance or the clearance rate of the solution to be detected, namely the free radical indicator, in the visible light range, thereby indirectly researching the content of the free radical in the quantum dot light emitting diode and realizing the test of the attenuation rate of the quantum dot light emitting diode.
For example: in the step S20, the performing light treatment on the solution to be detected for a predetermined time, and obtaining the attenuation rate of the light emitting device according to the representation of the concentration of the free radical in the solution to be detected by the free radical indicator includes: and carrying out illumination treatment on the solution to be detected for a preset time, detecting the absorbance of the free radical indicator in the solution to be detected under a specific wavelength, and obtaining the attenuation rate of the light emitting device according to the absorbance of the free radical indicator under the specific wavelength. The smaller the absorbance of the radical indicator over a period of time, the more radicals in the solution react with the radical indicator, the higher the radical content of the device, and the faster the decay rate of the device.
For another example: in the step S20, the performing light treatment on the solution to be detected for a predetermined time, and obtaining the attenuation rate of the light emitting device according to the representation of the concentration of the free radical in the solution to be detected by the free radical indicator includes:
(1) And carrying out light treatment on the solution to be detected for a preset time, and taking a plurality of time points in the preset time to detect the absorbance of the free radical indicator in the solution to be detected under a specific wavelength.
(2) And calculating the clearance rate of the free radical indicator in the solution to be detected in a preset time according to the absorbance of the free radical indicator at a plurality of time points under a specific wavelength.
(3) And obtaining the decay rate of the light-emitting device according to the clearance rate of the free radical indicator.
The greater the rate of scavenging of the free radical indicator over time, the higher the free radical content of the device, and the faster the decay rate. Obtaining the decay rate of the light emitting device using the rate of scavenging of the free radical indicator can prevent premature reaction of the free radical indicator with the free radical from affecting the degree of discrimination of the detection and can improve the accuracy of the detection.
In some embodiments, the free radical indicator is DPPH (1, 1-diphenyl-2-trinitrophenylhydrazine).
For a better understanding of the scavenging rate of the radical indicator mentioned in the examples, the following calculation of the scavenging rate of DPPH is exemplified:
when the predetermined time of the light treatment is 30 minutes, the absorbance of DPPH at a specific wavelength can be detected every 10 minutes within 30 minutes, namely, the absorbance of DPPH at a specific wavelength is detected at 10 minutes, 20 minutes and 30 minutes of the light treatment respectively, and the clearance rate of DPPH can be calculated according to the data of the absorbance at the three points and the recombination time.
In some embodiments, the absorbance at the particular wavelength is absorbance at any wavelength in the range of 513nm to 517nm, for example, absorbance at a wavelength of 513 nm. By recording the absorption of DPPH at a specific wavelength and correlating the absorption with the illumination time, the reaction rate of DPPH and free radicals, namely the absorption decay rate of DPPH, can be obtained, and the decay rate of the light-emitting device can be obtained indirectly.
In some embodiments, the organic solvent is selected from, but not limited to, methanol, and in the embodiments of the present application, methanol has a role of dispersing the light emitting layer and the carrier transporting layer, and since methanol has a low polarity, the methanol can be used as a solvent for dispersing the light emitting layer and the carrier transporting layer of the qd light emitting diode, and it is understood that the organic solvent may be any other solvent known in the art, so long as the solvent can disperse the light emitting layer and the carrier transporting layer, and the solvent is not specifically limited herein.
In some embodiments, the dispersion is obtained by dissolving a sample of the light emitting layer and a sample of the carrier transporting layer in an organic solvent by ultrasound.
In some embodiments, the illumination has a wavelength of 400nm to 450nm (nanometers). In this wavelength range, quantum dots are more easily excited to generate excitons. It will be appreciated that the wavelength of the illumination may take any value in the range 400nm to 450nm, for example 400nm, 405nm, 410nm, 415nm, 420nm, 425nm, 430nm, 435nm, 440nm, 445nm, 450nm, etc., or other non-listed values in the range 400nm to 450 nm.
In some embodiments, the predetermined time of the light treatment is 10min (minutes) to 1h (hours). In this illumination time range, the detection of the decay rate of DPPH is facilitated. It is understood that the illumination time may be any value within a range of 10min to 1h, for example, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min, etc., or other non-listed values within a range of 10min to 1h nanometers.
In some embodiments, in the solution to be detected, the concentration of DPPH is 0.01mg/mL to 1mg/mL (milligrams per milliliter), the effect of the reaction on DPPH absorption is reduced due to the excessively thick DPPH, the excessively thin DPPH may cause the reaction to be excessively fast, and the distinction degree of the detection is affected due to the excessively thick DPPH or the excessively thin DPPH, so that the comparison of the concentration of the free radicals between later devices is not facilitated, and it is understood that the concentration of DPPH is arbitrarily selected from the range of 0.01mg/mL to 1mg/mL, for example: 0.01mg/mL, 0.1mg/mL, 0.2mg/mL, 0.3mg/mL, 0.4mg/mL, 0.5mg/mL, 0.6mg/mL, 0.7mg/mL, 0.8mg/mL, 0.9mg/mL, or 1.0mg/mL, etc., or other non-listed values in the range of 0.01mg/mL to 1mg/mL.
In some embodiments, the total concentration of the material of the light emitting layer and the material of the carrier transporting layer is 0.001mg/mL to 1mg/mL, and too high a content of the material of the light emitting layer and the material of the carrier transporting layer may cause too fast reaction with DPPH, so that the experimental differentiation is lowered, too low may cause too slow reaction, affecting the sensitivity of the experiment. It is understood that the total concentration of the material of the light emitting layer and the material of the carrier transporting layer may be any value in the range of 0.01mg/mL to 1mg/mL, for example: 0.01mg/mL, 0.1mg/mL, 0.2mg/mL, 0.3mg/mL, 0.4mg/mL, 0.5mg/mL, 0.6mg/mL, 0.7mg/mL, 0.8mg/mL, 0.9mg/mL, or 1.0mg/mL, etc., or other non-listed values in the range of 0.01mg/mL to 1mg/mL.
In some embodiments, the light emitting device is a quantum dot light emitting diode, specifically a red quantum dot light emitting diode, a blue quantum dot light emitting diode or a green quantum dot light emitting diode, particularly a blue quantum dot light emitting diode, and since the blue quantum dot light emitting diode is easier to attenuate, the performance is still to be further improved, therefore, compared with the red quantum dot light emitting diode or the green quantum dot light emitting diode, the method provided by the application is used for testing the blue quantum dot light emitting diode, thereby helping to test the attenuation rate of the blue quantum dot light emitting diode.
In some embodiments, the carrier transport layer comprises an electron transport layer, and/or a hole transport layer.
The light emitting device in the embodiment of the present application may have a positive type structure or an inverse type structure. In the light emitting device, the cathode or anode further comprises a substrate on a side away from the quantum dot layer, the anode being disposed on the substrate in a positive configuration and the cathode being disposed on the substrate in an negative configuration. Whether in a positive type structure or an inverse type structure, a hole functional layer such as a hole injection layer and an electron blocking layer can be arranged between the anode and the quantum dot layer, and an electron functional layer such as an electron injection layer and a hole blocking layer can be arranged between the cathode and the quantum dot layer.
Fig. 2 shows a schematic diagram of a front structure of a light emitting device 10 according to an embodiment of the present application, as shown in fig. 1, the front structure light emitting device 10 includes a substrate 1, an anode 2 disposed on a surface of the substrate 1, a hole injection layer 3 disposed on a surface of the anode 2, a hole transport layer 4 disposed on a surface of the hole injection layer 3, a light emitting layer 5 disposed on a surface of the hole transport layer 4, an electron transport layer 6 disposed on a surface of the light emitting layer 5, and a cathode 7 disposed on a surface of the electron transport layer 6.
Fig. 3 shows a schematic diagram of an inverted structure of the light emitting device 10 according to the embodiment of the present application, as shown in fig. 2, the inverted structure light emitting device 10 includes a substrate 1, a cathode 7 disposed on a surface of the substrate 1, an electron transport layer 6 disposed on a surface of the cathode 7, a light emitting layer 5 disposed on a surface of the electron transport layer 6, a hole transport layer 4 disposed on a surface of the light emitting layer 5, a hole injection layer 3 disposed on a surface of the hole transport layer 4, and an anode 2 disposed on a surface of the hole injection layer 3.
In the embodiments of the present application, the materials of the respective functional layers are common materials in the art, for example:
the substrate may be a rigid substrate or a flexible substrate. Specific materials may include at least one of glass, silicon wafer, polycarbonate, polymethyl methacrylate, polyethylene terephthalate, polyethylene naphthalate, polyamide, polyethersulfone.
The hole transport layer material includes: poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine), polyvinylcarbazole, poly (N, N '-bis (4-butylphenyl) -N, N' -bis (benzene)Group) benzidine), poly (9, 9-dioctylfluorene-co-bis-N, N-phenyl-1, 4-phenylenediamine), 4',4 "-tris (carbazol-9-yl) triphenylamine, 4' -bis (9-carbazol) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, 15N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, graphene, C 60 At least one of them.
The electron transport layer material includes: znO, tiO 2 、SnO 2 、Ta 2 O 3 、ZrO 2 At least one of NiO, tiLiO, znAlO, znMgO, znSnO, znLiO and InSnO.
The light emitting layer is selected from at least one of II-VI compound, III-V compound and I-III-VI compound; the II-VI compound is at least one selected from CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSte; the III-V compound is at least one selected from InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of them.
The anode and cathode materials are selected from one or more of metal, carbon material and metal oxide, and the metal is selected from one or more of Al, ag, cu, mo, au, ba, ca and Mg; the carbon material is selected from one or more of graphite, carbon nano tube, graphene and carbon fiber; the metal oxide is selected from doped/undoped metal oxide or composite electrode, the doped/undoped metal oxide is selected from one or more of ITO, FTO, ATO, AZO, GZO, IZO, MZO and AMO, the composite electrode is selected from AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO 2 /Ag/TiO 2 、TiO 2 /Al/TiO 2 、ZnS/Ag/ZnS、ZnS/Al/ZnS、TiO 2 /Ag/TiO 2 TiO 2 /Al/TiO 2 One or more of the following.
Because the attenuation rate in the embodiment of the application does not refer to the attenuation rate of the device itself, the attenuation rate is not obtained quantitatively, but is represented by other parameters (concentration of free radicals in the solution to be detected or other characterization parameters related to concentration, such as absorbance or DPPH clearance rate), so that the embodiment of the application can also compare the parameters of a plurality of light emitting devices capable of representing the attenuation rate, and qualitatively compare the relative attenuation rate of each device, thereby screening out the target device. Accordingly, as shown in fig. 4, the present application further provides a method for screening a light emitting device, the method including:
s100. providing a plurality of light emitting devices.
S200, respectively obtaining the attenuation rate of each light-emitting device by using the testing method in any embodiment, comparing the attenuation rate of each light-emitting device, and screening out the target light-emitting device.
In some embodiments, the screening out the target light emitting device includes: and screening out the light-emitting devices with relatively slow decay rate from the plurality of light-emitting devices to obtain the target light-emitting device.
For example, when the number of the quantum dot light emitting diodes is two, the two light emitting devices can be subjected to the test method described in the embodiment to obtain the absorption and attenuation rate of DPPH, and the test conditions (such as illumination time and illumination wavelength and concentration of DPPH) of the two light emitting devices are the same except that the two light emitting devices are different during the test. The specific steps can be as follows:
taking samples of the same preset area of the light-emitting layer and the carrier transmission layer from the two light-emitting devices, ensuring that the proportion of the samples to the materials in the actual devices is consistent, dispersing the samples of the two devices in an organic solvent by utilizing ultrasonic waves to obtain a dispersion liquid in which the light-emitting layer material and the carrier transmission layer material are dispersed, and adding DPPH into the dispersion liquid to obtain a solution to be detected. The quantum dots in the light-emitting layer are excited by illumination to form excitons, free electrons in the excitons are separated from holes and react with the material of the carrier transmission layer to generate free radicals, the free radicals react with DPPH to change color, the absorbance of the solution to be detected in the visible light range is detected, at the moment, the absorption spectrum of the DPPH is recorded, the absorption of the DPPH under specific wavelength is measured, and the absorption and the illumination time are related to each other, so that the absorption and attenuation rates of the DPPH in the solution to be detected corresponding to the two devices, namely the removal rate, can be obtained.
After the DPPH removal rate of the solution to be detected corresponding to the two devices is obtained, the relative proportion of the free radical content of the two devices can be indirectly obtained, and the attenuation rates of the two devices can be compared by comparing the relative proportion of the free radical content, so that the target device is screened.
The present application is described in detail by examples below.
Examples:
(1) Providing two different QLED devices, namely a device A and a device B, wherein the device A is a blue QLED device, the device B is a red QLED device, the thickness of a luminescent layer in a film layer of the device A is 25nm, the luminescent wavelength is 470nm, the material of a hole transport layer is TFB, the thickness is 25nm, the material of an electron transport layer is ZnO, and the thickness is 40nm; the thickness of the luminescent layer in the film layer of the device B is 10nm, and the luminescent wavelength is 630nm. The hole transport layer is made of TFB with the thickness of 25nm, the electron transport layer is made of ZnO with the thickness of 40nm.
Take 2X 2cm in device A and device B 2 The surface area of each film material was ultrasonically dispersed in 10mL of methanol, device A was formulated as dispersion 1 and device B was formulated as dispersion 2.
(2) DPPH solution (methanol solvent) with concentration of 0.02mg/mL was prepared, and a portion of the solution was diluted to 0.002mg/mL and subjected to exhaust treatment (dry inert gas was introduced thereinto, oxygen gas and water were discharged) to serve as a comparative sample.
(3) 1mL of a DPPH solution of 0.02mg/mL was taken, 2mL of a QLED dispersion solution was added thereto, 7mL of methanol was added thereto, and the mixture was subjected to an exhaust treatment (dry inert gas was introduced thereinto, oxygen and water were exhausted), thereby giving test samples (device A and device B were formulated as test sample 1 and test sample 2, respectively).
(4) The absorption spectrum of the comparative sample, sample 1 and sample 2 in the initial state was measured.
(5) And (3) simultaneously placing the comparison sample and the test sample 1 under the shortwave of 400nm for illumination, wherein the illumination time is 10min, immediately testing the absorption spectrum after the illumination is finished, and simultaneously taking the comparison sample, the test sample 1 and the test sample 2 to be placed in a dark state for comparing the absorption spectrum.
(6) Repeating the step (5) for 3 times.
(7) The absorbance spectra were aligned to compare the concentration of free radical generation in system a and system B.
As shown in fig. 5 and 6, fig. 5 is a schematic diagram of absorption spectra of a test sample 1, a test sample 2 and a comparison sample at different times in a dark state environment; in fig. 5, a is an absorption change curve of a comparative sample, b is an absorption change curve of a test sample 1, c is an absorption change curve of a test sample 2, and d is a change curve of the test sample after absorption normalization at 513nm along with illumination time; FIG. 6 is a schematic diagram of absorption spectra of test sample 1, test sample 2 and comparison sample at different times under 400nm light; in fig. 6, a is the absorption change curve of the comparative sample, b is the absorption change curve of the test sample 1, c is the absorption change curve of the test sample 2, and d is the change curve of the test sample after absorption normalization at 513nm with the irradiation time.
As can be seen from fig. 5, in the dark state environment, the absorption spectra of the test sample 1, the test sample 2 and the comparison sample in different times (10 minutes, 20 minutes and 30 minutes) overlap, and the absorbance at 513nm does not change, which means that no free radical is generated in the test sample 1, the test sample 2 and the comparison sample in the dark state environment.
As can be seen from fig. 6, under the illumination of 400nm, the absorbance of the test sample 1, the test sample 2 and the comparison sample at 513nm changes at different times (10 minutes, 20 minutes and 30 minutes), and the absorbance is continuously reduced with time, which indicates that the free radical reacts with DPPH to attenuate the DPPH, and the removal rate of DPPH is compared, as shown by d in fig. 6, the removal rate of DPPH of the device a is significantly faster than that of the device B, which indicates that the content of the generated free radical of the device a is higher than that of the device B, so that the attenuation rate of the device a can be deduced to be greater than that of the device B.
The foregoing describes in detail a method for testing and screening the decay rate of a light emitting device provided in the embodiments of the present application, and specific examples are applied herein to illustrate the principles and embodiments of the present application, where the foregoing examples are only for aiding in understanding the method and core ideas of the present application; meanwhile, those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, and the present description should not be construed as limiting the present application in view of the above.

Claims (13)

1. A method of testing a decay rate of a light emitting device comprising a light emitting layer and a carrier transport layer, the method comprising:
providing a solution to be detected, wherein the solution to be detected comprises a material of the light-emitting layer, a material of the carrier transmission layer, a free radical indicator and an organic solvent, the material of the light-emitting layer comprises quantum dots, and the free radical indicator has the characteristic of representing the concentration of free radicals in the solution to be detected; and
and carrying out illumination treatment on the solution to be detected for a preset time to enable the material of the light-emitting layer and the material of the carrier transmission layer to react to generate free radicals, and obtaining the attenuation rate of the light-emitting device according to the representation of the concentration of the free radicals in the solution to be detected by the free radical indicator.
2. The method of testing according to claim 1, wherein said providing a solution to be tested comprises:
in the light-emitting device, taking a sample of the light-emitting layer and a sample of the carrier transport layer with preset areas, and dispersing the sample of the light-emitting layer and the sample of the carrier transport layer in the organic solvent to obtain a dispersion liquid; and
and adding a free radical indicator into the dispersion liquid to obtain the solution to be detected.
3. The method according to claim 1, wherein the subjecting the solution to be tested to light treatment for a predetermined time, and the light emitting device decay rate is obtained according to the characterization of the concentration of the free radicals in the solution to be tested by the free radical indicator, comprises:
and carrying out illumination treatment on the solution to be detected for a preset time, detecting the absorbance of the free radical indicator in the solution to be detected under a specific wavelength, and obtaining the attenuation rate of the light emitting device according to the absorbance of the free radical indicator under the specific wavelength.
4. The method according to claim 1, wherein the subjecting the solution to be tested to light treatment for a predetermined time, and the light emitting device decay rate is obtained according to the characterization of the concentration of the free radicals in the solution to be tested by the free radical indicator, comprises:
carrying out illumination treatment on the solution to be detected for a preset time, and taking a plurality of time points in the preset time to detect the absorbance of the free radical indicator in the solution to be detected under a specific wavelength; calculating to obtain the clearance rate of the free radical indicator in the solution to be detected in a preset time according to the absorbance of the free radical indicator at a plurality of time points under a specific wavelength; and obtaining the decay rate of the light-emitting device according to the clearance rate of the free radical indicator.
5. The test method according to claim 2, wherein the concentration of the radical indicator in the solution to be detected is 0.01mg/mL to 1mg/mL, and/or the total concentration of the material of the light-emitting layer and the material of the carrier transport layer is 0.001mg/mL to 1mg/mL.
6. The method of any one of claims 1 to 5, wherein the free radical indicator is DPPH.
7. The test method according to claim 1, wherein the organic solvent is selected from methanol.
8. The test method according to claim 1, wherein the wavelength of the light is 400nm to 450nm, and/or the predetermined time of the light treatment is 10min to 1h.
9. The method of testing according to claim 1, wherein the light emitting device is a blue quantum dot light emitting diode.
10. The test method according to claim 1, wherein the carrier transport layer comprises an electron transport layer, and/or a hole transport layer.
11. The test method of claim 10, wherein the hole transport layer material comprises: poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine), polyvinylcarbazole, poly (N, N '-bis (4-butylphenyl) -N, N' -bis (phenyl) benzidine), poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-phenylenediamine), 4',4 "-tris (carbazol-9-yl) triphenylamine, 4' -bis (9-carbazol) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, 15N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, graphene, C 60 At least one of, and/or,
the electron transport layer material includes: znO, tiO 2 、SnO 2 、Ta 2 O 3 、ZrO 2 At least one of NiO, tiLiO, znAlO, znMgO, znSnO, znLiO and InSnO; and/or the number of the groups of groups,
the light emitting layer is selected from at least one of II-VI compound, III-V compound and I-III-VI compound; the II-VI compound is at least one selected from CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeS, cdZnSeTe and CdZnSte; the III-V compound is at least one selected from InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP and InAlNP; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of them.
12. A method of screening a light emitting device, the method comprising:
providing a plurality of light emitting devices;
obtaining the attenuation rate of each light-emitting device by the method of any one of claims 1 to 11, comparing the attenuation rates of each light-emitting device, and screening out the target light-emitting device.
13. The method of screening for a target light emitting device according to claim 12, comprising: and screening out the light-emitting devices with relatively slow decay rate from the plurality of light-emitting devices to obtain the target light-emitting device.
CN202111611835.7A 2021-12-27 2021-12-27 Method for testing and screening decay rate of light-emitting device Pending CN116367681A (en)

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