CN113831920B - Quantum dot solution purification method, quantum dot purification solution and device - Google Patents
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Abstract
The embodiment of the application provides a quantum dot solution purification method, a quantum dot purification solution and a quantum dot device, and relates to the technical field of quantum dots. The quantum dot solution purification method comprises the following steps: pouring a quantum dot solution into an electrophoresis tank, wherein the quantum dot solution comprises an organic solution, and quantum dots, organic ligand anions and inorganic nano cations which are dissociated in the organic solution, and the electrophoresis tank is placed in an inert gas protection atmosphere; an electric field is applied between the cathode and the anode of the electrophoresis cell, so that inorganic nano cations are deposited on the surface of the cathode. The quantum dot solution purification method, the quantum dot purification solution and the quantum dot device can remove excessive inorganic nano particles, and meet the production requirement of quantum dot luminescent devices.
Description
Technical Field
The application relates to the technical field of quantum dots, in particular to a quantum dot solution purification method, a quantum dot purification solution and a device.
Background
Quantum Dot (QD) is a semiconductor nanostructure that confines excitons in three spatial directions, and is composed of different inorganic nanoparticles, typically metallic or non-metallic nanoparticles. Based on the characteristics of quantum dots, quantum dot light emitting devices have been developed, and quantum dot light emitting diodes (Quantum Dot Light Emitting Diodes, QLEDs) are expected to become a new generation of high-performance, large-area and high-benefit electroluminescent devices, and can be used for display and illumination technologies.
When the quantum dot is applied to an electroluminescent device, in order to passivate defects on the surface of the quantum dot, an organic ligand is generally wrapped on the surface of the quantum dot, and the organic ligand is generally insulating. The quantum dot light emitting device is usually prepared by depositing a quantum dot solution into a film, wherein the quantum dot solution is a solution containing quantum dots prepared by a chemical solution growth method, but inorganic nano particles added in the preparation process of the quantum dot solution cannot completely react to generate quantum dots, so that the excessive positively charged inorganic nano particles are easy to combine with negatively charged ligand particles to generate agglomerates. In the process of preparing the quantum dot luminescent device, the agglomerates and the quantum dots in the quantum dot solution are deposited into films at the same time, and although the electroluminescent effect of the device is not obviously affected when the particle size of the agglomerates is smaller, after the particle size of the agglomerates reaches a certain size, the position is free of the quantum dots or the quantum dots are extremely few due to the occupation of the agglomerates, and the electroluminescent macroscopic appearance of the device is black. The existence of black dots not only affects the display effect of the device, but also reduces the service life of the device, and severely limits the commercialization process of the quantum dot light-emitting device.
Therefore, it is necessary to purify the quantum dot solution to meet the production requirements of the quantum dot light emitting device.
Disclosure of Invention
The embodiment of the application aims to provide a quantum dot solution purification method, a quantum dot purification solution and a quantum dot device, which can remove excessive inorganic nano particles and meet the production requirement of a quantum dot light-emitting device.
In a first aspect, embodiments of the present application provide a method for purifying a quantum dot solution, comprising the steps of:
pouring a quantum dot solution into an electrophoresis tank, wherein the quantum dot solution comprises an organic solution, and quantum dots, organic ligand anions and inorganic nano cations which are dissociated in the organic solution, and the electrophoresis tank is placed in an inert gas protection atmosphere;
an electric field is applied between the cathode and the anode of the electrophoresis cell, so that inorganic nano cations are deposited on the surface of the cathode.
In the technical scheme, a certain electric field is applied to the specific quantum dot solution, so that excessive inorganic nano cations in the quantum dot solution, namely, positively charged inorganic nano particles, are promoted to move to the cathode of the electrophoresis cell and are deposited on the surface of the cathode, and the aim of removing impurities is fulfilled. The electrophoresis method can remove excessive inorganic nano particles in the quantum dot solution, thereby achieving the purpose of purifying the quantum dot solution, improving the black dot problem of the quantum dot light-emitting device and meeting the production requirement of the quantum dot light-emitting device.
In one possible implementation, the electric field is direct current, the voltage is 3-20V, and the power is applied for 10-60min.
In the technical scheme, the inorganic nano elements of the quantum dots of different types are basically the same, and the electrophoresis condition can remove the redundant inorganic nano particles for synthesizing the quantum dots of different types.
In one possible implementation, the temperature of the quantum dot solution is 20-80 ℃.
In the technical scheme, the temperature of the quantum dot solution is controlled within a certain range, so that the ionization effect of inorganic nano cations and organic ligand anions can be increased, and separation is realized.
In one possible implementation, the concentration of quantum dots in the quantum dot solution is 5-100g/L.
In one possible implementation, the preparation method of the quantum dot solution is as follows:
preparing corresponding inorganic nano element precursor solutions by adopting element sources corresponding to inorganic nano elements in the quantum dots respectively;
and reacting the inorganic nano element precursor solution with an organic ligand to generate a quantum dot solution.
In one possible implementation manner, the inorganic nano elements in the quantum include metal nano elements and semi-metal nano elements, and the corresponding inorganic nano element precursor solution is a metal nano element precursor solution and a semi-metal nano element precursor solution, and the preparation method of the quantum dot solution is as follows: uniformly mixing a semi-metal nano element precursor solution and an organic ligand, heating to 250-300 ℃ under the protection of inert gas, adding a metal nano element precursor, and cooling to 230-280 ℃ to grow the quantum dots.
In one possible implementation, the preparation method of the metal nano element precursor solution is as follows: uniformly mixing the oxide of the metal nano element with halichondrin acid and octadecene, heating to 120-180 ℃, and vacuumizing to react until the solution is clear.
In one possible implementation, the preparation method of the precursor solution of the semi-metal nano element is as follows: uniformly mixing semi-metal nano particles and octadecene, heating to 120-180 ℃, vacuumizing for more than half an hour, and heating to 250-300 ℃ under the protection of inert gas to react until the solution is completely clarified.
In a second aspect, an embodiment of the present application provides a quantum dot purification solution, which is prepared by using the quantum dot solution purification method provided in the first aspect.
In the technical scheme, the quantum dot purification solution can remove redundant inorganic nanoparticle element particles, so that the generation of black dots is reduced when the quantum dot solution is deposited to form a quantum dot film, and the size of the black dots is prevented from being too large.
In a third aspect, an embodiment of the present application provides a quantum dot light emitting device, which includes a transparent anode substrate, a hole injection layer, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode that are sequentially stacked from bottom to top, where the quantum dot light emitting layer is deposited by using the quantum dot purification solution provided in the second aspect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of a quantum dot solution purification process according to an embodiment of the present application.
Icon: 110-an electrophoresis cell; 120-anode; 130-cathode; 140-quantum dot solution.
Detailed Description
The inventors found in the course of implementing the present application that: the quantum dots used for preparing the quantum dot light emitting device are inorganic nano-particles wrapped by organic ligands, the inorganic nano-particles are general quantum dots with a core-shell structure, the inorganic nano-particles are usually cadmium Cd, selenium Se, tellurium Te and the like and contain metal elements and semi-metal elements, and the organic ligands are usually long-chain oleic acid, oleylamine and thiols, such as oleic acid, trioctylphosphine, malonic acid derivatives, thiothiol compounds, thiocarboxylic acid compounds, compounds containing ester groups and thiol groups and the like. In order to synthesize the quantum dot, an excessive amount of inorganic nano cations, such as Cd, se, te and/or the like, which contain both metal elements and semi-metal elements, are often present in the obtained quantum dot solution, and are easily combined with anions of the ligand to form agglomerates. As previously mentioned, these agglomerates are a major cause of black spots in QLEDs devices.
For the quantum dot solution, the use requirement of the QLEDs can be met by taking the excessive positively charged inorganic nano particles as impurity particles to be removed without specially extracting the quantum dots.
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The quantum dot solution purification method, the quantum dot solution purification solution and the device according to the embodiment of the application are specifically described below.
The embodiment of the application provides a quantum dot solution purification method, which comprises the following steps:
(1) The synthesized quantum dot solution comprises an organic solution and quantum dots and organic ligands which are dissociated in the organic solution, wherein the organic ligands in the quantum dot solution are organic matters such as TOP, halichondrin OA and the like, anions can be hydrolyzed or ionized, and quantum dot core-shell elements such as cadmium salt and antimony salt in the quantum dot solution can be hydrolyzed or ionized to obtain cations. The concentration of quantum dots in the quantum dot solution is generally 5-100g/L.
The preparation method of the quantum dot solution meeting the above conditions comprises the following steps:
s1, preparing corresponding inorganic nano element precursor solutions by adopting element sources corresponding to inorganic nano elements in quantum dots; typically, the inorganic nano-elements in the quantum include metal nano-elements and semi-metal nano-elements, for example, the metal nano-elements are Cd and Zn, the semi-metal nano-elements are Se and Te, and the corresponding inorganic nano-element precursor solutions are a metal nano-element precursor solution and a semi-metal nano-element precursor solution.
As one embodiment, the preparation method of the metal nano element precursor solution comprises the following steps: uniformly mixing the oxide of the metal nano element with the halichondrin OA and the octadeceneODE, heating to 120-180 ℃, and vacuumizing to completely clarify the solution.
As an embodiment, the preparation method of the precursor solution of the semi-metal nano element comprises the following steps: uniformly mixing the semi-metal nano particles and octadeceneode, heating to 120-180 ℃, vacuumizing for more than half an hour, heating to 250-300 ℃ under the protection of inert gas, and reacting until the solution is completely clear.
S2, reacting an inorganic nano element precursor solution with an organic ligand to generate a quantum dot solution, wherein the preparation method specifically comprises the following steps: uniformly mixing a semi-metal nano element precursor solution and an organic ligand, heating to 250-300 ℃ under the protection of inert gas, adding a metal nano element precursor, cooling to 230-280 ℃ to grow quantum dots, sampling at different times, and performing fluorescence test absorption to monitor the growth condition of the quantum dots until the quantum dots grow to a preset size.
(2) Electrophoresis: electrophoresis refers to the directional movement of colloid particles in a dispersion medium towards a cathode or an anode under the action of an externally applied direct current power supply.
Referring to fig. 1, a quantum dot solution 140 is poured into an electrophoresis cell 110, an anode 120 and a cathode 130 are provided in the electrophoresis cell 110, an electric field can be applied between the anode 120 and the cathode 130 by an external power source, the temperature of the quantum dot solution 140 is 20-80 ℃, and the electrophoresis cell is placed in an inert gas protective atmosphere.
Applying an electric field between the cathode 130 and the anode 120 of the electrophoresis cell 110, wherein the electric field is direct current, the voltage is 3-20V, and the electricity is applied for 10-60min, and inorganic nano cations R + Will move toward the cathode 130, thereby causing inorganic nano-cations R + Deposited on the surface of cathode 130, organic ligand anion X - Will move toward the anode 120 but only the charge will move and will not deposit on the anode 120.
The embodiment of the application also provides a quantum dot purifying solution, which is prepared by adopting the quantum dot purifying method.
The embodiment of the application also provides a quantum dot luminescent device, which comprises a transparent anode substrate, a hole injection layer, a hole transmission layer, a quantum dot luminescent layer, an electron transmission layer and a cathode which are sequentially overlapped from bottom to top, wherein the quantum dot luminescent layer is deposited by adopting the quantum dot purification solution.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
The embodiment provides a quantum dot light emitting device (QD-LED device), wherein the quantum dot is CdSe red quantum dot and is externally wrapped with a paraffin layer, and the preparation method comprises the following steps:
(1) Synthesis of Quantum dot solutions
S1, synthesizing a Cd precursor solution: to a 100mL three-necked flask was added CdO:6mmol, OA:6mL, ODE:54mL, the reaction is heated to 150 ℃, then the air is exhausted for 30min until the solution is completely clear, and the temperature is reduced to 50 ℃ for standby.
S2, synthesis of Se precursor solution: to a 100mL three-necked flask was added Se powder: 6mol, ODE:60mL, heating the reaction solution to 150 ℃, evacuating the gas for 30min, heating to 280 ℃ under the protection of nitrogen, keeping for 10min until the solution is completely clear, and cooling to 50 ℃ for standby;
s3, synthesizing quantum dots: 2mL of Se precursor solution and 6mL of liquid paraffin are added into a 25mL three-necked flask and mixed uniformly, N 2 Heating to 280 ℃ under protection, rapidly adding 4mL of Cd precursor solution, cooling to 250 ℃ for quantum dot growth, sampling at different times for fluorescence test absorption, and monitoring the quantum dotAnd growing until a quantum dot solution containing the preset quantum dots is obtained.
(2) Purification of quantum dot solutions
Pouring the synthesized quantum dot solution into an electrophoresis tank, placing the electrophoresis tank in a nitrogen protection atmosphere, and electrifying a direct current between an anode and a cathode at a voltage of 10V, wherein the temperature of the quantum dot solution is 50 ℃, electrifying for 30min, and directly pulling out an electrode after electrifying is completed to obtain the quantum dot purified solution.
The composition of the quantum dot solution before and after purification is basically consistent, but most metal cations in the quantum dot solution before purification are precipitated on the cathode after purification, so that the generation of precipitation caused by precipitation in the solution is reduced.
(3) Preparation of quantum dot light-emitting device
S1, depositing a hole injection layer on a transparent anode substrate, wherein the thickness of the hole injection layer is about 35nm, and annealing for 15min at 160 ℃;
s2, depositing a hole transport layer on the hole injection layer, wherein the thickness of the hole transport layer is about 30nm, and annealing the hole transport layer at 150 ℃ for 10min;
s3, depositing a quantum dot luminescent layer on the hole transport layer by adopting a quantum dot purification solution, wherein the thickness of the quantum dot luminescent layer is about 5nm, and annealing is carried out for 60min at the temperature of 250 ℃;
s4, depositing ZnO solution as an electron transport layer on the quantum dot luminescent layer, wherein the thickness of the ZnO solution is 40nm, and annealing the ZnO solution for 30min at 80 ℃;
s5, depositing a metal cathode on the electron transport layer, wherein the thickness of the metal cathode is about 150nm, and the reflection of the cathode to visible light is not less than 98%;
s6, packaging the whole layer structure by using UV resin, and curing by using a UV lamp with the power of 0.2W/cm 2 Curing time was 10s.
Comparative example 1
This comparative example provides a quantum dot light emitting device (QD-LED device) which is prepared in substantially the same manner as in example 1, except that: the quantum dot solution synthesized in the step (1) is adopted to deposit and form a quantum dot luminescent layer instead of the purification step of the quantum dot solution in the step (2).
The QD-LED devices of example 1 and comparative example 1 were tested below, and the test structures are shown in table 1.
TABLE 1 QD-test structure for LED devices
| Group of | Black dots are a percentage of the light emitting area (%) | Lifetime (h) |
| Comparative example 1 | 4.5％ | 72000 |
| Example 1 | 1％ | 96000 |
Note that: the service life of the device is 100cd/m 2 The corresponding time when the luminance is reduced to 50% at the initial luminance.
As can be seen from the data in table 1, compared with the quantum dot light emitting device prepared from the quantum dot solution without purification treatment, the device black dot and the device lifetime prepared from the quantum dot purification solution purified by using the electrophoresis tank according to the embodiment of the application are improved to different degrees, wherein the area of the device black dot is reduced by 3.5%, and the device lifetime is improved by 33.3%.
Example 2
The embodiment provides a quantum dot light emitting device (QD-LED device), wherein the quantum dot is ZnSe/CdSe core-shell quantum dot and is externally wrapped with a paraffin layer, and the preparation method comprises the following steps:
(1) Synthesis of Quantum dot solutions
S1, synthesizing a Cd precursor solution: to a 100mL three-necked flask was added CdO:6mmol, OA:6mL, ODE:54mL, the reaction is heated to 150 ℃, then the air is exhausted for 30min until the solution is completely clear, and the temperature is reduced to 50 ℃ for standby.
Synthesizing Zn precursor solution: to a 100mL three necked flask was added ZnO:6mmol, OA:6mL, ODE:54mL, the reaction is heated to 150 ℃, then the air is exhausted for 30min until the solution is completely clear, and the temperature is reduced to 50 ℃ for standby.
S2, synthesis of Se precursor solution: to a 100mL three-necked flask was added Se powder: 6mol, ODE:60mL, heating the reaction solution to 150 ℃, evacuating the gas for 30min, heating to 280 ℃ under the protection of nitrogen, keeping for 10min until the solution is completely clear, and cooling to 50 ℃ for standby;
s3, synthesizing quantum dots: 2mL of Se precursor solution and 6mL of liquid paraffin are added into a 25mL three-necked flask and mixed uniformly, N 2 Heating to 280 ℃ under protection, rapidly adding 4mL of Cd precursor solution, cooling to 250 ℃ for quantum dot growth, sampling at different times for fluorescence test absorption, and monitoring the quantum dot growth.
(2) Purification of quantum dot solutions
Pouring the synthesized quantum dot solution into an electrophoresis tank, placing the electrophoresis tank in a nitrogen protection atmosphere, and electrifying direct current between an anode and a cathode with voltage of 20V and temperature of the quantum dot solution of 50 ℃ for 30min to obtain the quantum dot purification solution.
(3) Preparation of quantum dot light-emitting device
S1, depositing a hole injection layer on a transparent anode substrate, wherein the thickness of the hole injection layer is about 35nm, and annealing for 15min at 160 ℃;
s2, depositing a hole transport layer on the hole injection layer, wherein the thickness of the hole transport layer is about 30nm, and annealing the hole transport layer at 150 ℃ for 10min;
s3, depositing a quantum dot luminescent layer on the hole transport layer by adopting a quantum dot purification solution, wherein the thickness of the quantum dot luminescent layer is about 5nm, and annealing is carried out for 60min at the temperature of 250 ℃;
s4, depositing ZnO solution as an electron transport layer on the quantum dot luminescent layer, wherein the thickness of the ZnO solution is 40nm, and annealing the ZnO solution for 30min at 80 ℃;
s5, depositing a metal cathode on the electron transport layer, wherein the thickness of the metal cathode is about 150nm, and the reflection of the cathode to visible light is not less than 98%;
s6, packaging the whole layer structure by using UV resin, and curing by using a UV lamp with the power of 0.2W/cm 2 Curing time was 10s.
Comparative example 2
This comparative example provides a quantum dot light emitting device (QD-LED device) which is prepared in substantially the same manner as in example 1, except that: the quantum dot solution synthesized in the step (1) is adopted to deposit and form a quantum dot luminescent layer instead of the purification step of the quantum dot solution in the step (2).
The QD-LED devices of example 1 and comparative example 1 were tested below, and the test structures are shown in table 1.
Table 2 QD-test structure of LED device
| Group of | Black dots are a percentage of the light emitting area (%) | Lifetime (h) |
| Comparative example 2 | 4.8％ | 79000 |
| Example 2 | 0.8％ | 99000 |
Note that: the service life of the device is 100cd/m 2 The corresponding time when the luminance is reduced to 50% at the initial luminance.
As can be seen from the data in table 2 above, the black dots and the lifetime of the devices prepared by using the quantum dot purification solution purified by the electrophoresis tank according to the embodiments of the present application are improved to different extents compared to the quantum dot light emitting devices prepared by using the quantum dot solution not purified.
In summary, the quantum dot solution purification method, the quantum dot purification solution and the quantum dot device provided by the embodiment of the application can remove excessive inorganic nano particles, and meet the production requirements of quantum dot light emitting devices.
The above description is only an example of the present application and is not intended to limit the scope of the present application, and various modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (9)
1. The quantum dot solution purification method is characterized by comprising the following steps of:
pouring a quantum dot solution into an electrophoresis tank, wherein the quantum dot solution comprises an organic solution, and quantum dots, organic ligand anions and inorganic nano cations which are dissociated in the organic solution, and the electrophoresis tank is placed in an inert gas protection atmosphere;
and applying an electric field between the cathode and the anode of the electrophoresis tank to deposit the inorganic nano cations on the surface of the cathode, wherein the electric field is direct current, the voltage is 3-20V, and the electricity is conducted for 10-60min.
2. The method of claim 1, wherein the temperature of the quantum dot solution is 20-80 ℃.
3. The method of claim 1, wherein the concentration of quantum dots in the quantum dot solution is 5-100g/L.
4. The method for purifying a quantum dot solution according to claim 1, wherein the method for preparing the quantum dot solution comprises the steps of:
preparing corresponding inorganic nano element precursor solutions by adopting element sources corresponding to inorganic nano elements in the quantum dots respectively;
and reacting the inorganic nano element precursor solution with an organic ligand to generate a quantum dot solution.
5. The method for purifying a quantum dot solution according to claim 4, wherein the inorganic nano elements in the quantum include metal nano elements and semi-metal nano elements, the corresponding inorganic nano element precursor solution is a metal nano element precursor solution and a semi-metal nano element precursor solution, and the method for preparing the quantum dot solution comprises the following steps: uniformly mixing a semi-metal nano element precursor solution and an organic ligand, heating to 250-300 ℃ under the protection of inert gas, adding a metal nano element precursor, and cooling to 230-280 ℃ to grow the quantum dots.
6. The method for purifying a quantum dot solution according to claim 5, wherein the preparation method of the metal nano-element precursor solution comprises the steps of: uniformly mixing the oxide of the metal nano element with halichondrin acid and octadecene, heating to 120-180 ℃, and vacuumizing to react until the solution is clear.
7. The method for purifying a quantum dot solution according to claim 5, wherein the method for preparing the precursor solution of the semi-metallic nano-element comprises the steps of: uniformly mixing semi-metal nano particles and octadecene, heating to 120-180 ℃, vacuumizing for more than half an hour, and heating to 250-300 ℃ under the protection of inert gas to react until the solution is completely clarified.
8. A quantum dot purification solution prepared by the method of any one of claims 1 to 7.
9. The quantum dot luminescent device is characterized by comprising a transparent anode substrate, a hole injection layer, a hole transport layer, a quantum dot luminescent layer, an electron transport layer and a cathode which are sequentially overlapped from bottom to top, wherein the quantum dot luminescent layer is deposited by adopting the quantum dot purification solution as claimed in claim 8.
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