CN111584767B - Quantum dot light-emitting diode and preparation method thereof - Google Patents
Quantum dot light-emitting diode and preparation method thereof Download PDFInfo
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- CN111584767B CN111584767B CN202010459188.1A CN202010459188A CN111584767B CN 111584767 B CN111584767 B CN 111584767B CN 202010459188 A CN202010459188 A CN 202010459188A CN 111584767 B CN111584767 B CN 111584767B
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/115—OLEDs 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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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
Abstract
The invention relates to the technical field of quantum dots, in particular to a quantum dot light-emitting diode and a preparation method thereof. The preparation method of the quantum dot light-emitting diode comprises the following steps: after the quantum dot light emitting layer is deposited, the light emitting layer is treated at 70-80 ℃ for 3-5 min and then is heat treated at 150-300 ℃ for 2-30 s. According to the invention, after the quantum dot light-emitting layer is deposited, rapid heat treatment is carried out at a specific temperature, so that heat damage caused by conventional heat treatment can be avoided, residual solvent on an interface can be effectively removed, the contact angle between the electron transmission layer and the quantum dot light-emitting layer is reduced, the interface quality is improved, especially the interface film-forming quality between the quantum dot light-emitting layer and the electron transmission layer is improved, and thus the performance of the quantum dot light-emitting diode can be improved and the service life of the quantum dot light-emitting diode can be prolonged.
Description
Technical Field
The invention relates to the technical field of quantum dots, in particular to a quantum dot light-emitting diode and a preparation method thereof.
Background
Quantum dot light emitting diodes (QLEDs) are an important development direction for new displays in the future. The bottleneck in the current development of the pinch QLED is that the working life of the device still cannot meet the industrial requirements.
In the prior art, the functional layer material is prepared by a solution, the material of the functional layer is fully dissolved in the solvent at first, and then is deposited layer by a spin coating or printing method, and in order that the deposition of the upper layer material does not affect the film formation of the lower layer material, heating treatment is required to be performed between each process.
The existing heating method is to heat the whole device, which can bring thermal damage to the material, especially the quantum dot layer is easy to influence the performance by the heating treatment process. In order to avoid heat damage to the bottom layer material, the solvent on the outermost layer cannot be sufficiently removed, the film forming quality is influenced, the film forming flatness of the quantum dot layer is reduced after heating, the electron transport layer is not favorable for deposition in the next procedure, and the film forming quality is poorer towards the top layer, so that the performance and the service life of the device are influenced.
Taking a quantum dot device with a positive structure as an example, the quantum dot layer uses n-octane as a solvent, the boiling point of the n-octane is higher than 120 ℃, and if the device is heated integrally at 120 ℃, the quantum dot and a bottom layer material are damaged; on the other hand, if the heating is insufficient, the residual solvent cannot be removed well, and the contact angle of the electron transport layer increases, which is not favorable for forming a film.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of a quantum dot light-emitting diode, which is used for solving the technical problem of short service life of the quantum dot light-emitting diode in the prior art.
The second purpose of the invention is to provide a quantum dot light-emitting diode, and the interface film forming quality of the quantum dot light-emitting diode is excellent, and the service life of the quantum dot light-emitting diode is long.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the preparation method of the quantum dot light-emitting diode comprises the following steps:
after the quantum dot light emitting layer is deposited, the mixture is treated at 70-80 ℃ for 3-5 min and then is heat treated at 150-300 ℃ for 2-30 s.
According to the invention, after the quantum dot light-emitting layer is deposited, rapid heat treatment is carried out at a specific temperature, so that heat damage caused by conventional heat treatment can be avoided, residual solvent on an interface can be effectively removed, the contact angle between the electron transmission layer and the quantum dot light-emitting layer is reduced, the interface quality is improved, especially the interface film-forming quality between the quantum dot light-emitting layer and the electron transmission layer is improved, and thus the performance of the quantum dot light-emitting diode can be improved and the service life of the quantum dot light-emitting diode can be prolonged.
As in various embodiments, the heat treatment temperature can be 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃ and so on.
In a preferred embodiment of the present invention, the temperature of the heat treatment is 190 to 210 ℃, more preferably 195 to 205 ℃, and still more preferably 200 ℃.
As in the different embodiments, the time of the heat treatment may be 2s, 3s, 4s, 5s, 6s, 7s, 8s, 9s, 10s, 11s, 12s, 13s, 14s, 15s, 16s, 17s, 18s, 19s, 20s, 21s, 22s, 23s, 24s, 25s, 26s, 27s, 28s, 29s, 30s, and so on.
In a preferred embodiment of the present invention, the heat treatment time is 2 to 10 seconds, more preferably 2 to 5 seconds, and still more preferably 5 seconds.
In a preferred embodiment of the present invention, the temperature of the heat treatment is 190 to 210 ℃, and the time of the heat treatment is 2 to 10s; preferably, the temperature of the heat treatment is 200 ℃, and the time of the heat treatment is 5s.
By adopting the heat treatment mode of the invention, the heating thickness is only acted on the surface layer by 2-5 nm, and the bottom layer is not damaged.
In a specific embodiment of the present invention, the heat treatment is performed using an infrared halogen lamp or a laser.
In a specific embodiment of the present invention, the thickness of the quantum dot light emitting layer is 10 to 100nm.
In a specific embodiment of the present invention, the deposition method of the quantum dot light emitting layer includes: and spin-coating the solution in which the quantum dots are dissolved on the hole transport layer to form the quantum dot light-emitting layer.
Specifically, the solvent of the solution is n-octane.
In a specific embodiment of the present invention, the quantum dot is a direct bandgap compound semiconductor with light emitting capability, including but not limited to one or more of group II-VI compounds, group III-V compounds, group II-V compounds, group III-VI compounds, group IV-VI compounds, group I-III-VI compounds, group II-IV-VI compounds, or group IV simple substance.
Specifically, the material of the quantum dots includes, but is not limited to, nanocrystals of II-VI compound semiconductors, such as CdS, cdSe, cdTe, znS, znSe, znTe, hgS, hgSe, hgTe, pbS, pbSe, pbTe and other binary, ternary, quaternary II-VI compounds;
materials for the quantum dots include, but are not limited to, nanocrystals of group III-V compound semiconductors such as GaP, gaAs, inP, inAs, and other binary, ternary, quaternary group III-V compounds.
In another embodiment of the present invention, the quantum dots may also be any one or more of doped or undoped inorganic perovskite type semiconductors, organic-inorganic hybrid perovskite type semiconductors.
Specifically, the structural general formula of the inorganic perovskite type semiconductor is AMX 3 Wherein A is Cs + Ion, M is a divalent metal cation, including but not limited to Pb 2+ 、Sn 2+ 、Cu 2+ 、Ni 2+ 、 Cd 2+ 、Cr 2+ 、Mn 2+ 、Co 2+ 、Fe 2+ 、Ge 2+ 、Yb 2+ 、Eu 2 + X is a halogen anion, including but not limited to Cl - 、Br - 、I - ；
The structural general formula of the organic-inorganic hybrid perovskite type semiconductor is BMX 3 Wherein B is an organic amine cation including but not limited to CH 3 (CH 2 ) n-2 NH 3+ (n.gtoreq.2) or NH 3 (CH 2 ) n NH 3 2+ (n.gtoreq.2). When n =2, the inorganic metal halide octahedron MX 6 4- The metal cations M are positioned in the center of a halogen octahedron through connection in a roof sharing mode, and the organic amine cations B are filled in gaps among the octahedrons to form an infinitely extending three-dimensional structure; when n > 2, inorganic metal halide octahedron MX connected in a common vertex mode 6 4- Extending in two-dimensional direction to form a layered structure, inserting an organic amine cation bilayer (protonated monoamine) or an organic amine cation monolayer (protonated diamine) between layers, and mutually overlapping the organic layer and the inorganic layer to form a stable two-dimensional layered structure; m is a divalent metal cation including, but not limited to, pb 2+ 、Sn 2+ 、Cu 2+ 、Ni 2+ 、Cd 2+ 、Cr 2+ 、Mn 2 + 、Co 2+ 、Fe 2+ 、Ge 2+ 、Yb 2+ 、 Eu 2+ (ii) a X is a halide anion, including but not limited to Cl - 、Br - 、I - 。
In a specific embodiment of the present invention, the concentration of the quantum dots in the solution is 15 to 20mg/mL.
In the specific embodiment of the invention, the spin speed is 2000-2500 rpm, and the spin time is 30-35 s.
In a specific embodiment of the present invention, the quantum dot light emitting diode may be a quantum dot light emitting diode with a bottom light emitting structure, a top light emitting structure, or an inverted structure. Taking a bottom-emitting positive-type quantum dot light-emitting diode as an example, the quantum dot light-emitting diode specifically includes, from bottom to top, a bottom electrode, a hole injection layer, a hole transport layer, a quantum dot light-emitting layer, an electron transport layer, and a top electrode.
In a specific embodiment of the present invention, before depositing the quantum dot light emitting layer, the method further comprises: depositing a hole injection layer on the bottom electrode; depositing a hole transport layer on the hole injection layer.
In a specific embodiment of the present invention, an electron transport layer is deposited on the quantum dot light emitting layer after the heat treatment; depositing a top electrode on the electron transport layer.
In a specific embodiment of the present invention, the bottom electrode is ITO. The thickness of the bottom electrode is 60-120 nm.
Specifically, the material of the hole injection layer is spin-coated or evaporated on the bottom electrode. Further, after spin coating, the mixture is treated for 10 to 15min at the temperature of between 140 and 150 ℃. The rotating speed of the spin coating can be 4500-5000 rpm, and the time of the spin coating is 25-30 s. The thickness of the hole injection layer is 15 to 30nm, preferably 20 to 25nm.
The material of the hole injection layer comprises but is not limited to one or more of PEDOT PSS, cuPc, F4-TCNQ, HATCN, transition metal oxide and transition metal chalcogenide compound. Wherein the transition metal oxide comprises NiO x 、MoO x 、WO x 、CrO x One or more of CuO, e.g. MoO 3 . The transition metal chalcogenide compound comprises MoS x 、MoSe x 、WS x 、WSe x And CuS.
Specifically, the material of the hole transport layer is spin-coated or evaporated on the hole injection layer. Further, after spin coating, the mixture is treated at 70-80 ℃ for 25-30 min. The spin coating speed is 2500-3000 rpm, and the spin coating time is 25-30 s.
In a specific embodiment of the present invention, the material of the hole transport layer includes, but is not limited to, at least one of TFB 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-carbazole) biphenyl, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, graphene, C60.
In another embodiment of the present invention, the material of the hole transport layer is an inorganic material with hole transport capability, including but not limited to NiO x 、MoO x 、WO x 、CrO x 、CuO、MoS x 、 MoSe x 、WS x 、WSe x And CuS.
In the process of actually selecting materials, the optical band gaps of the materials of the hole injection layer and the hole transport layer cannot be smaller than the optical band gap of the material of the quantum dot, otherwise, the light extraction efficiency is influenced.
In an actual spin coating operation, the concentration of the hole transport layer, such as TFB, may be 5-10 mg/mL, such as 8mg/mL. The thickness of the hole transport layer is 10 to 50nm, preferably 15 to 30nm.
Specifically, the material of the electron transport layer is coated on the quantum dot light emitting layer in a spinning way and is treated for 25-30 min at 70-80 ℃. The spin coating speed is 2500-3000 rpm, and the spin coating time is 25-30 s.
The electron transport layer is made of oxide semiconductor nano-particle materials, has electron transport capacity, and has a band gap larger than that of the quantum dot materials. Specifically, the material of the electron transport layer includes but is not limited to ZnO, tiO 2 、SnO 2 、Ta 2 O 3 、ZrO 2 One or more of NiO, tiLiO, znAlO, znMgO, znSnO, znLiO and InSnO.
In an actual spin coating operation, the concentration of the material of the electron transport layer, such as ZnO, may be 25 to 30mg/mL, such as 30mg/mL. The thickness of the electron transport layer is 20-50 nm, preferably 25-50 nm.
Specifically, a top electrode is deposited on the electron transport layer by means of thermal evaporation coating. The material of the top electrode may be silver. Wherein the reflection of the top electrode to visible light is not less than 98%. The conditions of the thermal evaporation coating comprise: vacuum degree is less than or equal to 3 multiplied by 10 -4 Pa, speed of
The time is 180-200 s, and the thickness is 15-20 nm.
The invention also provides the quantum dot light-emitting diode prepared by the preparation method.
The quantum dot light-emitting diode prepared by the invention has good interface quality, particularly good interface film forming quality between the quantum dot light-emitting layer and the electron transmission layer, excellent performance and long service life.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, after the quantum dot light-emitting layer is deposited, rapid heat treatment is carried out at a specific temperature, so that heat damage caused by conventional heat treatment can be avoided, residual solvent on an interface can be effectively removed, a contact angle between the electron transmission layer and the quantum dot light-emitting layer is reduced, the interface quality is improved, and especially the interface film forming quality between the quantum dot light-emitting layer and the electron transmission layer is improved;
(2) The quantum dot light-emitting device prepared by the invention has excellent performance and long service life of 1000 cd.m -2 The lifetime of the device can reach T95 5000 hours at the emission intensity of (3).
Detailed Description
While the technical solutions of the present invention will be described clearly and completely with reference to the specific embodiments, those skilled in the art will understand that the following described examples are some, but not all, examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any inventive step, are within the scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Example 1
The quantum dot light emitting diode provided by this embodiment uses Ag as a top electrode, znO as an electron transport layer, cdSe/ZnS as a quantum dot layer, TFB as a hole transport layer, PEDOT: PSS as a hole injection layer, and ITO as a transparent anode substrate.
The embodiment provides a preparation method of a quantum dot light-emitting diode, which comprises the following steps:
(1) PSS is spin-coated on an ITO substrate with the thickness of 100nm, the spin-coating speed is 5000rpm, and the spin-coating time is 30s; then, the mixture was heat-treated at 150 ℃ for 15min to form a hole injection layer of PEDOT, PSS having a thickness of 30nm.
(2) Spin-coating TFB on the hole injection layer formed in the step (1), wherein the concentration of the TFB is 8mg/mL, the spin-coating rotation speed is 3000rpm, and the spin-coating time is 30s; then, the film was heat-treated at 80 ℃ for 30min to form a TFB hole transport layer having a thickness of 30nm.
(3) Spin-coating CdSe/ZnS quantum dots on the hole transport layer formed in the step (2), wherein the concentration of the quantum dots is 20mg/mL, the solvent is n-octane, the spin-coating rotation speed is 2000rpm, and the spin-coating time is 30s; then heating at 80 deg.C for 5min, and thermally annealing at 200 deg.C for 5s to form 30nm quantum dot light-emitting layer.
(4) Spin-coating ZnO on the quantum dot light-emitting layer formed in the step (3), wherein the concentration of ZnO is 30mg/mL, the solvent is ethanol, the spin-coating rotation speed is 2000rpm, and the spin-coating time is 30s; then, the mixture was heat-treated at 80 ℃ for 30min to form an electron transport layer having a thickness of 40 nm.
(5) Performing evaporation plating of Ag on the electron transport layer formed in the step (4) in a thermal evaporation plating mode; wherein the vacuum degree is less than or equal to 3 multiplied by 10 -4 Pa, speed of
The time was 200s, and an Ag top electrode was formed to a thickness of 20nm.
And after the evaporation is finished, carrying out conventional packaging on the quantum dot light-emitting diode device to obtain the quantum dot light-emitting diode device.
Wherein, each layer of material in the device can be adjusted conventionally according to actual requirements, and different materials meeting the conditions are adopted.
Example 2
This example refers to the preparation of example 1, with the only difference that:
in the step (3), the mixture is heated at 80 ℃ for 5min and then thermally annealed at 150 ℃ for 30s.
Example 3
This example refers to the preparation of example 1, with the only difference that:
in the step (3), the annealing is carried out for 5min at the temperature of 80 ℃ and then the annealing is carried out for 2s at the temperature of 300 ℃.
Example 4
This example refers to the preparation of example 1, with the only difference that:
in the step (3), the mixture is heated for 5min at the temperature of 80 ℃ and then is thermally annealed for 10s at the temperature of 190 ℃.
Example 5
This example refers to the preparation of example 1, with the only difference that:
in the step (3), the annealing is carried out for 5min at the temperature of 80 ℃ and then the annealing is carried out for 2s at the temperature of 210 ℃.
Example 6
This example refers to the preparation of example 1, with the only difference that:
in the step (3), the mixture is heated at 80 ℃ for 5min and then thermally annealed at 150 ℃ for 5s.
Example 7
This example refers to the preparation of example 1, with the only difference that:
and (4) replacing the CdSe/ZnS quantum dots in the step (3) with ZnSe/ZnS quantum dots.
Comparative example 1
Comparative example 1 the preparation process of example 1 was referenced, with the following differences:
in the step (3), the steel is heated and treated for 5min at the temperature of 80 ℃ and then is thermally annealed for 5s at the temperature of 120 ℃.
Comparative example 2
Comparative example 2 the preparation process of example 1 was referenced, with the following differences:
in the step (3), the mixture is heated at 80 ℃ for 5min and then thermally annealed at 120 ℃ for 5min.
Comparative example 3
Comparative example 3 the preparation of example 1 was referred to, except that:
in the step (3), the mixture is heated at 80 ℃ for 20min.
Experimental example 1
In order to comparatively illustrate the performance of the quantum dot light emitting diodes of different examples and comparative examples of the present invention, the performance and the operating life of the quantum dot light emitting diodes prepared in examples 1 to 7 and comparative examples 1 to 3 were tested, and the test results are shown in table 1.
TABLE 1 different Quantum dot light emitting diode test results
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present invention as defined by the appended claims.
Claims (13)
1. The preparation method of the quantum dot light-emitting diode is characterized by comprising the following steps:
after the quantum dot light emitting layer is deposited, the mixture is treated for 3 to 5min at a temperature of between 70 and 80 ℃ and then is heat treated for 2 to 30s at a temperature of between 150 and 300 ℃;
the deposition method of the quantum dot light-emitting layer comprises the following steps: spin-coating the solution dissolved with the quantum dots on the hole transport layer to form a quantum dot light-emitting layer; the quantum dots are CdSe/ZnS or ZnSe/ZnS quantum dots;
before depositing the quantum dot light-emitting layer, the method further comprises the following steps: depositing a hole injection layer on the bottom electrode; depositing a hole transport layer on the hole injection layer;
depositing an electron transport layer on the quantum dot light emitting layer after the heat treatment; depositing a top electrode on the electron transport layer;
the thickness of the hole transport layer is 10-50 nm;
the thickness of the hole injection layer is 15-30 nm;
the thickness of the bottom electrode is 60-120 nm;
the thickness of the electron transmission layer is 20-50 nm;
the thickness of the top electrode is 60-120 nm.
2. The method of claim 1, wherein the temperature of the heat treatment is 190-210 ℃.
3. The method of claim 2, wherein the temperature of the heat treatment is 195-205 ℃.
4. The method of claim 3, wherein the temperature of the heat treatment is 200 ℃.
5. The method of claim 1, wherein the heat treatment time is 2-10 s.
6. The method for preparing a quantum dot light-emitting diode according to claim 5, wherein the time of the heat treatment is 2 to 5s.
7. The method of claim 6, wherein the heat treatment is performed for 5s.
8. The method for preparing a quantum dot light-emitting diode according to claim 1, wherein the temperature of the heat treatment is 190-210 ℃, and the time of the heat treatment is 2-10 s.
9. The method for preparing a quantum dot light-emitting diode according to claim 8, wherein the temperature of the heat treatment is 200 ℃ and the time of the heat treatment is 5s.
10. The method of any one of claims 1 to 9, wherein the heat treatment is performed using an infrared halogen lamp or a laser.
11. The method for preparing a quantum dot light-emitting diode according to any one of claims 1 to 9, wherein the thickness of the quantum dot light-emitting layer is 10 to 100nm.
12. The method of claim 1, wherein the solvent of the solution is n-octane.
13. A quantum dot light emitting diode prepared by the method of any one of claims 1 to 12.
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