CN114854392A - Quantum dot, preparation method thereof, quantum dot light-emitting diode and preparation method thereof - Google Patents

Quantum dot, preparation method thereof, quantum dot light-emitting diode and preparation method thereof Download PDF

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CN114854392A
CN114854392A CN202210420798.XA CN202210420798A CN114854392A CN 114854392 A CN114854392 A CN 114854392A CN 202210420798 A CN202210420798 A CN 202210420798A CN 114854392 A CN114854392 A CN 114854392A
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汪鹏生
龚克
宋斌
孙笑
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Dachen Display Technology Quzhou Co ltd
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Abstract

The invention discloses a quantum dot, a preparation method thereof, a quantum dot light-emitting diode and a preparation method thereof. Therefore, the invention adopts the cinnamic acid ligand with high carrier mobility and strong electrochemical stability to replace the ligand on the surface of the traditional quantum dot, the cinnamic acid has excellent carrier mobility and strong chemical polarity, and after the cinnamic acid forms coordination with the metal ions on the surface of the core-shell structure, the injection rate of the carrier of the QLED device can be greatly improved, and the performance of the QLED device can be improved.

Description

Quantum dot, preparation method thereof, quantum dot light-emitting diode and preparation method thereof
Technical Field
The invention belongs to the technical field of quantum dot devices, and particularly relates to quantum dots, a preparation method of the quantum dots, a quantum dot light-emitting diode and a preparation method of the quantum dot light-emitting diode.
Background
The quantum dot material has the advantages of easy synthesis, low cost, high quantum yield, continuously adjustable wavelength, high color purity and the like, and is a popular research material in the photoelectric field. Existing quantum dot materials typically have a core-shell structure. In the preparation process of the quantum dot, in order to ensure the stability of the quantum dot, an inorganic shell layer is generally grown on the outer layer of the core, and an alkyl chain ligand is added.
The conventional QLED (quantum dot light emitting diode) is generally formed by stacking thin film structures such as an electrode, an electron injection layer, a quantum dot light emitting layer, a hole injection layer and a hole transport layer, electrons and holes are injected into the quantum dot layer by the electrode after the current is switched on, so that the electrons and the holes are combined to emit light in the quantum dot, the internal quantum efficiency of the QLED is 100%, but the External Quantum Efficiency (EQE) of the QLED and the service life of a device are still main factors for restricting the application of the QLED. One important factor is that the insulating property of these alkyl ligands on the quantum dots limits the transport of carriers between quantum dots, resulting in the degradation of the performance of the final quantum dot device. Although the current scheme can improve the carrier transport property of the quantum dot device by optimizing the concentration of the alkyl ligand or the length of the alkyl chain, the stability of the quantum dot is reduced, and the performance of the device is reduced, namely the current scheme cannot improve the stability of the quantum dot and the carrier transport property between the quantum dots at the same time.
Therefore, there is a need for an improved quantum dot light emitting diode.
Disclosure of Invention
The inventor finds that in the QLED device, because the carrier mobility of the long-chain alkane ligand on the surface of the quantum dot is low, the injection of the carrier and the recombination of the carrier in the luminescent layer of the quantum dot are seriously influenced, and excessive non-radiative auger recombination can be formed, so that the service life of the device is reduced.
The present invention aims to ameliorate at least one of the above technical problems to at least some extent.
The invention provides a quantum dot, which comprises a core-shell structure and a first ligand connected with the core-shell structure, wherein the first ligand is cinnamic acid. Therefore, the invention adopts the cinnamic acid ligand with high carrier mobility and strong electrochemical stability to replace the ligand on the surface of the traditional quantum dot, the cinnamic acid has excellent carrier mobility and strong chemical polarity, and after the cinnamic acid forms coordination with the metal ions on the surface of the core-shell structure, the injection rate of the carrier of the QLED device can be greatly improved, and the performance of the QLED device can be improved. Moreover, the quantum dot provided by the invention has the characteristic of stable structure, and the stability of the quantum dot can be ensured. That is, the invention solves the problem that the stability of the quantum dots and the carrier transmission characteristics among the quantum dots cannot be simultaneously improved in the existing scheme.
According to an embodiment of the invention, the core-shell structure comprises a core structure and a shell structure coated on the outer surface of the core structure, and the material forming the core structure comprises at least one of CdS, CdSe, CdTe, HgS, HgSe, HgTe, PbS, PbSe, PbTe, GaP, GaAs, InP, InAs and CuInS; the material forming the shell structure comprises at least one of ZnS, ZnSe, ZnTe.
The present invention also provides a method of preparing a quantum dot as hereinbefore described, the method comprising: mixing the first quantum dot solution with a cinnamic acid solution, and reacting under a heating condition;
the first quantum dot comprises a core-shell structure and a second ligand connected with the core-shell structure, wherein the second ligand comprises at least one of oleic acid, oleylamine and thiol.
According to an embodiment of the invention, the temperature of the reaction is 90-120 ℃; the reaction time is 20-30 hours; the ratio of the amount of the substance of the cinnamic acid to the first quantum dot is (90-110): 1.
According to an embodiment of the present invention, the first quantum dot solution is obtained by dissolving the first quantum dots in a first non-polar solvent.
According to an embodiment of the invention, the cinnamic acid solution is prepared by mixing cinnamic acid with a second non-polar solvent at a temperature of 30-50 ℃.
According to an embodiment of the present invention, after the reaction is finished, the reaction further includes: adding polar solvent to make quantum point form precipitate.
The invention also provides a quantum dot light-emitting diode which comprises an anode, a hole injection layer, a hole transport layer, a quantum dot layer, an electron transport layer and a cathode which are sequentially stacked; the material forming the quantum dot layer comprises quantum dots as described hereinbefore. Therefore, the quantum dot light emitting diode has all the features and advantages of the quantum dots, and the description is omitted here.
The present invention also provides a method of making a quantum dot light emitting diode as described above, the method comprising: forming a hole injection layer on one side of the anode; forming a hole transport layer on the side of the hole injection layer away from the anode; forming a quantum dot layer on one side of the hole transport layer far away from the hole injection layer; forming an electron transport layer on one side of the quantum dot layer away from the hole transport layer; and forming a cathode on the side of the electron transport layer far away from the quantum dot layer. Thus, the method has all the features and advantages of the quantum dot light emitting diode described above, and thus, the description thereof is omitted.
Drawings
FIG. 1 is a schematic structural diagram of a quantum dot material of the present invention;
fig. 2 is a schematic structural diagram of a quantum dot light-emitting diode according to the present invention.
Detailed Description
In order to solve the above technical problems, the present invention provides a quantum dot, and referring to fig. 1, the quantum dot includes a core-shell structure and a first ligand connected thereto, and the first ligand is cinnamic acid. Therefore, the invention adopts the cinnamic acid ligand with high carrier mobility and strong electrochemical stability to replace the ligand on the surface of the traditional quantum dot, the cinnamic acid has excellent carrier mobility and strong chemical polarity, and after the cinnamic acid forms coordination with the metal ions on the surface of the core-shell structure, the injection rate of the carrier of the QLED device can be greatly improved, and the performance of the QLED device can be improved. Moreover, the quantum dot provided by the invention has the characteristic of stable structure, and the stability of the quantum dot can be ensured.
According to an embodiment of the invention, the core-shell structure comprises a core structure and a shell structure coated on the outer surface of the core structure, and the material forming the core structure comprises at least one of CdS, CdSe, CdTe, HgS, HgSe, HgTe, PbS, PbSe, PbTe, GaP, GaAs, InP, InAs and CuInS; the material forming the shell structure comprises at least one of ZnS, ZnSe, ZnTe.
The present invention also provides a method of preparing a quantum dot as hereinbefore described, the method comprising: mixing the first quantum dot solution with an acrylic acid solution, and reacting under a heating condition; the first quantum dot comprises a core-shell structure and a second ligand connected with the core-shell structure, wherein the second ligand comprises at least one of oleic acid, oleylamine and thiol. Therefore, the quantum dots prepared by the method have all the characteristics and advantages of the quantum dots, and are not described in detail herein. In addition, the method has the advantages of simple operation and easy ligand exchange.
According to an embodiment of the invention, the temperature of the reaction is 90-120 ℃; if the reaction temperature is too low, part of the ligand is precipitated from the surface of the quantum dot, and ligand exchange cannot be completed. If the reaction temperature is too high, self-reaction in the quantum dots can be promoted, the quantum dots are quenched, and the stability of the quantum dots is reduced.
The reaction time is 20-30 hours; if the reaction time is too short, poor ligand exchange results. If the reaction time is too long, the possibility that the external water oxygen destroys the stability of the quantum dots is increased.
The ratio of the amount of the substance of the cinnamic acid to the first quantum dot is (90-110): 1. If the ratio is too small, the second ligand remains and the exchange effect is insignificant. If the ratio is too large, too much cinnamic acid may cause the surface of the quantum dot to be etched, and the performance is reduced.
According to an embodiment of the present invention, the first quantum dot solution is obtained by dissolving the first quantum dots into a first non-polar solvent.
According to an embodiment of the invention, the cinnamic acid solution is prepared by mixing cinnamic acid with a second non-polar solvent at a temperature of 30-50 ℃.
According to an embodiment of the present invention, after the reaction is finished, the reaction further includes: adding polar solvent to make quantum point form precipitate.
The invention also provides a quantum dot light-emitting diode which comprises an anode, a hole injection layer, a hole transport layer, a quantum dot layer, an electron transport layer and a cathode which are sequentially stacked; the material forming the quantum dot layer comprises quantum dots as described hereinbefore. Therefore, the quantum dot light emitting diode has all the features and advantages of the quantum dots, and the description is omitted here.
In some embodiments of the present invention, referring to fig. 2, the material forming the anode may be ITO, and the material forming the hole injection layer may be PEDOT: PSS, a material forming the hole transport layer may be TFB, QDs in the drawing represents a quantum dot layer, a material forming the electron transport layer may be ZnO, a material forming the cathode may be Al, and electrons and holes are recombined in the quantum dot layer to emit light.
The present invention also provides a method of making a quantum dot light emitting diode as described above, the method comprising:
s100, forming a hole injection layer on one side of the anode;
the material forming the anode comprises ITO.
The material forming the hole injection layer may be PEDOT: PSS.
S200, forming a hole transport layer on one side, far away from the anode, of the hole injection layer;
the material forming the hole transport layer may be TFB.
S300, forming a quantum dot layer on one side, far away from the hole injection layer, of the hole transport layer;
the materials for forming the quantum dot layer are the quantum dots described above, and the structure of the quantum dots and the preparation method of the quantum dots are described in detail above and will not be described herein again.
S400, forming an electron transport layer on one side, far away from the hole transport layer, of the quantum dot layer;
the material forming the electron transport layer includes ZnO.
And S500, forming a cathode on one side of the electron transport layer far away from the quantum dot layer.
The material forming the cathode includes Al.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
Preparation of Quantum dots
(1) Preparing an n-octane solution of the cinnamic acid, dissolving 3g of the cinnamic acid in 6ml of an n-octane solvent, heating to 40 ℃, and uniformly stirring to obtain a clear solution.
(2) Adding 2ml of prepared phenylpropenoic acid solution into 3ml of nonpolar solution of first quantum dots with the amount of 0.01mmol/ml of substance, wherein the first quantum dots are CdSe/ZnS (the core structure is CdSe and the shell structure is ZnS), and the second ligand is oleic acid. The mass ratio of the cinnamic acid to the first quantum dot is 100:1, the mixed solution is heated to 110 ℃ and stirred for 24h, and the quantum dot solution taking the cinnamic acid as the ligand is obtained. Then adding a polar solvent such as ethanol and the like for precipitation, centrifuging, pouring out the mixed solution, and adding 3ml of n-octane into the precipitate to redissolve the quantum dots.
Example 2
Quantum dots were prepared according to the method of example 1, except that: the ratio of the amount of the substance of the cinnamic acid to the first quantum dot is 90:1, and other conditions are the same.
Example 3
Quantum dots were prepared according to the method of example 1, except that: the ratio of the amount of the substance of the cinnamic acid to the first quantum dot is 110:1, and other conditions are the same.
Example 4
Quantum dots were prepared according to the method of example 1, except that: the first quantum dot in example 4 was InP/ZnSe (core structure InP and shell structure ZnSe).
Example 5
Quantum dots were prepared according to the method of example 1, except that: the first quantum dot in example 5 was CuInS/ZnS (core structure was CuInS, shell structure was ZnS).
Example 6
Quantum dots were prepared according to the method of example 1, except that: the first quantum dot in example 6 is an inorganic perovskite quantum dot CsPbI 3 。
Example 7
Quantum dots were prepared according to the method of example 1, except that: the first quantum dot in example 7 is an organic-inorganic hybrid quantum dot CH 3 NH 3 SnI 3 。
Comparative example 1
The first quantum dot in the example 1 is used as the quantum dot of the comparative example 1, namely the existing quantum dot is used as the comparative example 1, and the ligand exchange is carried out without adding cinnamic acid in the preparation process of the quantum dot in the comparative example 1.
In comparative example 1, the core structure of the quantum dot is CdSe, the shell structure is ZnS, and the ligand on the surface of the quantum dot is oleic acid.
Comparative example 2
The first quantum dot in example 4 is used as the quantum dot of comparative example 2, that is, the existing quantum dot is used as comparative example 2, and no cinnamic acid is added in the preparation process of the quantum dot in comparative example 2 for ligand exchange.
In comparative example 2, the core structure of the quantum dot was InP, the shell structure was ZnSe, and the ligand on the surface of the quantum dot was oleic acid.
Comparative example 3
The first quantum dot in example 5 is used as the quantum dot of comparative example 3, that is, the existing quantum dot is used as comparative example 3, and no cinnamic acid is added in the preparation process of the quantum dot in comparative example 3 for ligand exchange.
In comparative example 3, the core structure of the quantum dot is CuInS, the shell structure is ZnS, and the ligand on the surface of the quantum dot is oleic acid.
The quantum dots prepared in all the examples and comparative examples 1 to 3 were used to prepare quantum dot light emitting diodes by the following method:
(1) and preparing a proper amount of the quantum dot solution into a quantum dot n-octane solution with the concentration of 20mg/ml and 0.5ml for later use.
Spin coating PEDOT on an ITO glass substrate: PSS with the rotation speed of 4000 r/min-6000 r/min, and after the spin coating is finished, heat treatment is carried out for 20-30 min at 150 ℃.
(2) In the PEDOT: and (3) spinning TFB on the PSS layer at the rotating speed of 2000 r/min-4000 r/min, and performing heat treatment at 140 ℃ for 20-30 min after the spinning is finished.
(3) And (3) spin-coating the prepared quantum dots on the TFB to form a quantum dot layer, wherein the rotating speed is 2000 r/min-4000 r/min.
(4) And (3) coating ZnO on the quantum dot layer in a spin mode at the rotating speed of 2000-4000 r/min and treating for 30min at the temperature of 80 ℃.
(5) And evaporating an Al electrode, and then packaging, thus completing the preparation of the QLED device.
The QLED devices prepared using the examples and comparative examples were tested to obtain the lifetime and external quantum efficiency of each device, and the test results are shown in table 1 below.
The life test method comprises the following steps: the service life is tested in the ocean optical EQE test system, and the time used when the maximum brightness of the film layer is reduced to 95% along with the change of time is taken, and the value obtained by multiplying the time by a proportionality coefficient is recorded as the service life of the device T95 (namely the service life of the device in the table 1).
External Quantum Efficiency (EQE): external quantum efficiency, i.e., the luminous efficiency of the device, is the ratio of the number of photons emitted and the number of electrons injected by a quantum dot light emitting diode device in a certain direction.
Table 1 device efficiency and device lifetime results using QLED devices prepared in each example and comparative example
Figure BDA0003606681490000061
Figure BDA0003606681490000071
From examples 1 to 3, it can be seen that when the ratio of the amount of the substance of the cinnamic acid to the first quantum dot is (90-110):1, the device efficiency and the device efficiency of the QLED device are both high.
The core-shell structure of the quantum dots in the examples 1 to 3 is the same as that in the comparative example 1, and the efficiency and the service life of the device in the examples 1 to 3 are obviously higher than those in the comparative example 1; the core-shell structure of the quantum dots in the embodiment 4 is the same as that of the quantum dots in the comparative example 2, and the efficiency and the service life of the device in the embodiment 4 are obviously higher than those in the comparative example 2; the core-shell structure of the quantum dots in the embodiment 5 is the same as that in the comparative example 3, the efficiency and the service life of the device in the embodiment 5 are obviously higher than those in the comparative example 3, and the quantum dots can obviously improve the performance of the QLED device after being grafted with the cinnamic acid ligand.
The quantum dots of the embodiments 6 to 7 have no core-shell structure, the device efficiency and the device life of the manufactured QLED device are inferior to those of the embodiments 1 to 5, and the quantum dots have the core-shell structure, and the performance of the QLED device can be obviously improved only after the quantum dots are grafted with the cinnamic acid ligand.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. The quantum dot is characterized by comprising a core-shell structure and a first ligand connected with the core-shell structure, wherein the first ligand is phenylacrylic acid.
2. The quantum dot of claim 1, wherein the core-shell structure comprises a core structure and a shell structure coated on an outer surface of the core structure, and a material forming the core structure comprises at least one of CdS, CdSe, CdTe, HgS, HgSe, HgTe, PbS, PbSe, PbTe, GaP, GaAs, InP, InAs, and CuInS;
the material forming the shell structure comprises at least one of ZnS, ZnSe, ZnTe.
3. A method of preparing a quantum dot according to any of claims 1-2, comprising:
mixing the first quantum dot solution with a cinnamic acid solution, and reacting under a heating condition;
the first quantum dot comprises a core-shell structure and a second ligand connected with the core-shell structure, wherein the second ligand comprises at least one of oleic acid, oleylamine and thiol.
4. The method of claim 3, wherein the temperature of the reaction is 90-120 ℃;
the reaction time is 20 to 30 hours.
5. The method of claim 3, wherein the ratio of the amount of the material of the cinnamic acid to the first quantum dot is (90-110): 1.
6. The method of claim 3, wherein the first quantum dot solution is obtained by dissolving the first quantum dots in a first non-polar solvent.
7. The method of claim 3, wherein the cinnamic acid solution is prepared by mixing cinnamic acid with a second non-polar solvent at a temperature of 30-50 ℃.
8. The method of claim 3, further comprising: and after the reaction is finished, adding a polar solvent to enable the quantum dots to form precipitates.
9. The quantum dot light-emitting diode is characterized by comprising an anode, a hole injection layer, a hole transport layer, a quantum dot layer, an electron transport layer and a cathode which are sequentially stacked;
the material forming the quantum dot layer comprises the quantum dot of claim 1.
10. A method of making the quantum dot light emitting diode of claim 9, comprising:
forming a hole injection layer on one side of the anode;
forming a hole transport layer on the side of the hole injection layer away from the anode;
forming a quantum dot layer on one side of the hole transport layer far away from the hole injection layer;
forming an electron transport layer on one side of the quantum dot layer away from the hole transport layer;
and forming a cathode on the side of the electron transport layer far away from the quantum dot layer.
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