WO2022143435A1 - Procédé de criblage de points quantiques et diode électroluminescente à points quantiques - Google Patents

Procédé de criblage de points quantiques et diode électroluminescente à points quantiques Download PDF

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WO2022143435A1
WO2022143435A1 PCT/CN2021/141020 CN2021141020W WO2022143435A1 WO 2022143435 A1 WO2022143435 A1 WO 2022143435A1 CN 2021141020 W CN2021141020 W CN 2021141020W WO 2022143435 A1 WO2022143435 A1 WO 2022143435A1
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quantum dots
quantum dot
quantum
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particle
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周礼宽
杨一行
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Tcl科技集团股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
    • C09K11/881—Chalcogenides
    • C09K11/883—Chalcogenides with zinc or cadmium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
    • 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]
    • H10K50/11—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
    • 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

Definitions

  • the present disclosure relates to the field of quantum dot preparation, and in particular, to a quantum dot screening method and a quantum dot light-emitting diode.
  • Quantum dots are a low-dimensional nano-semiconductor material. By applying a certain electric field or light pressure to the nano-semiconductor material, they will emit light of a specific wavelength, and the wavelength of the emitted light will vary with the size of the semiconductor. change to change. In recent years, quantum dots have attracted extensive attention from researchers at home and abroad due to their narrow emission half-peak width, high color purity, wide spectral coverage, high luminous efficiency, and good stability. Quantum dots are generally spherical or spherical-like semiconductor nanocrystals with diameters between 2 and 20 nm. Due to the small particle size, large specific surface area and strong surface activity of quantum dots, agglomeration between quantum dots is prone to occur.
  • the problem of particle agglomeration is avoided by connecting organic ligands on the surface of quantum dots.
  • the quantum dots can be stable without agglomeration because the repulsive force provided by the encapsulation layer formed by the organic ligands is equivalent to the van der Waals force between them, and the encapsulation layer and the solvent provide a potential barrier to prevent the agglomeration between the quantum dots.
  • the preparation of quantum dots is divided into two processes: nucleation and growth, mainly through the adjustment of reaction time and temperature to obtain the desired size of quantum dot particles.
  • the resulting particle size deviation is about 20%, which is the half-peak of the quantum dot emission spectrum.
  • the large particle size deviation of quantum dots leads to poor film flatness of the light-emitting layer, increased leakage current of the device, and may cause short-circuit problems in the functional layer.
  • the purpose of the present disclosure is to provide a method for sieving quantum dots, which aims to solve the problem that the particle size deviation of the quantum dots prepared in the prior art is large, which causes the quality of the film formation of the light-emitting layer of the quantum dot light-emitting diode device. poor, resulting in poor optoelectronic properties.
  • a method for sieving quantum dots comprising the steps of:
  • the insoluble solvent is miscible with the first solvent and immiscible with the organic ligand.
  • a quantum dot light-emitting diode comprising a cathode, an anode, and a quantum dot light-emitting layer disposed between the cathode and the anode, and the quantum dot light-emitting layer material is the sieved quantum dots described in the present disclosure.
  • the present disclosure gradually adds an insoluble solvent that is mutually soluble with the first solvent but immiscible with the organic ligand into the initial quantum dot solution, and in a state of constant stirring, when the insoluble solvent is added dropwise to a certain amount , the initial quantum dot solution begins to flocculate, continue to stir to make the large particles completely precipitate, and then separate them by centrifugation, and then continue to add the insoluble solvent dropwise to the supernatant, repeat this several times, and collect the particles in sections
  • the size deviation of the separated quantum dots can be controlled within 5%, so as to obtain uniform size quantum dot materials; using the uniform size quantum dots as the quantum dot light-emitting layer material can effectively Improve the optoelectronic properties of quantum dot light-emitting diodes.
  • FIG. 1 is a flow chart of a preferred embodiment of a method for sieving quantum dots provided by the present disclosure.
  • FIG. 2 is a schematic structural diagram of a quantum dot light-emitting diode provided by the present disclosure.
  • FIG. 3 is a scanning electron microscope photograph of the original sample in Example 1 provided by the present disclosure.
  • FIG. 4 is a scanning electron microscope photograph of the sample of the front section in Example 1 provided by the present disclosure.
  • FIG. 5 is a scanning electron microscope photograph of the middle-section sample in Example 1 provided by the present disclosure.
  • FIG. 6 is a scanning electron microscope photograph of the back-end sample in Example 1 provided by the present disclosure.
  • FIG. 7 is a fluorescence emission spectrum diagram of the original sample of Example 1 and the quantum dots after sieving provided by the present disclosure.
  • the present disclosure provides a method for sieving quantum dots and a quantum dot light-emitting diode.
  • a method for sieving quantum dots and a quantum dot light-emitting diode In order to make the purpose, technical solutions and effects of the present disclosure clearer and clearer, the present disclosure will be described in further detail below. It should be understood that the specific embodiments described herein are only used to explain the present disclosure, but not to limit the present disclosure.
  • the synthesis and preparation of quantum dots is divided into two processes: nucleation and growth.
  • nucleation and growth By controlling the reaction time, reaction temperature and composition ratio, quantum dot particles of different wavelengths can be obtained;
  • the difference in activity, as the size of the quantum dot particles grows, the size deviation of each quantum dot particle is about 20%, which is directly manifested as the increase of the half-peak width of the quantum dot emission spectrum.
  • the size difference of quantum dot particles becomes larger, and the surface roughness of the solid-state film of the light-emitting layer of the quantum dot light-emitting diode device prepared by using such quantum dot materials increases, which will lead to an increase in the leakage current of the device and the problem of short-circuit device failure in the functional layer. .
  • the present disclosure provides a method for sieving quantum dots, as shown in FIG. 1 , which includes the steps:
  • the initial quantum dots synthesized were mainly composed of inorganic nanoparticles and an organic coating layer (organic ligand) connected to the surface of the inorganic nanoparticles through coordination bonds.
  • the initial quantum dots can be stably dispersed in the first solvent without agglomeration and sedimentation due to the mutual repulsive force provided by the surface-coated organic ligands and the van der Waals force between the organic ligands.
  • the first solvent is equivalent to setting a potential barrier between the initial quantum dots to prevent the quantum dots from agglomerating and settling.
  • the organic coating layer on the surface of the initial quantum dots is the key factor for the quantum dots to be dispersed in the first solvent.
  • the initial quantum dot solution is gradually added to the initial quantum dot solution.
  • the insoluble solvent that is immiscible with the organic ligand in the state of constant stirring, when the insoluble solvent is added dropwise to a certain amount, the initial quantum dot solution begins to flocculate, and the stirring is continued to completely precipitate the large particles, Then it is separated by centrifugation, and the supernatant is continuously added dropwise to the insoluble solvent. This is repeated several times, and the precipitates with similar particle sizes are collected in sections.
  • the size deviation of the isolated quantum dots can be controlled at a minimum.
  • quantum dot materials with uniform size can effectively reduce the roughness of the quantum dot light-emitting layer and increase its film formation flatness, thereby effectively improving the quantum dots.
  • the precipitation is collected in sections in chronological order, and the step of obtaining the sieved quantum dots includes:
  • the precipitation is collected in sections according to time sequence, so that the sieved quantum dots collected in the previous stage account for 25-35% of the weight of the initial quantum dots, and are recorded as large-particle quantum dots in the previous stage;
  • the precipitations are collected in chronological order, so that the sieved quantum dots collected in the middle section account for 35-45% of the weight of the initial quantum dots, and are recorded as particle quantum dots in the middle section;
  • the precipitates are collected in sections in chronological order, so that the sieved quantum dots collected in the latter stage account for 25-35% of the weight of the initial quantum dots, and are recorded as small particle quantum dots in the latter stage.
  • the samples obtained by particle size sieving are divided into large-particle quantum dots in the front section (accounting for 25-35% of the weight of the initial quantum dots) and medium-particle quantum dots in the middle section (accounting for the weight of the initial quantum dots) according to the order of flocculation and sedimentation. 35-45% of the initial quantum dots) and small particle quantum dots (25-35% of the initial quantum dot weight).
  • quantum dot particles with different particle size ranges can be sieved.
  • the emission wavelength and half-peak width of quantum dots have a certain relationship with the particle size distribution of quantum dots, that is, the larger the quantum dot particle size, the longer the emission peak position, the smaller the size distribution, and the narrower the half-peak width.
  • the collected flocculation precipitate is divided into a front part, a middle part and a rear part.
  • the front part is the large particle quantum dots in the front part, the main emission peak of which has a red shift of 1-3 nm relative to the initial quantum dots, the emission peak position of the particle quantum dots in the middle part is almost unchanged, and the main emission peak of the small particle quantum dots in the latter part is about 2 nm.
  • the blue shift is consistent with the size effect of quantum dots. As the size becomes larger or smaller, the emission wavelength shows a trend of red shift or blue shift; due to the quantum dot size sieving method, the size distribution deviation of quantum dots is reduced, Therefore, the half-peak widths of the collected three-stage quantum dot particles show a narrowing rule, and all have a narrowing trend of 2-3 nm.
  • the thickness of a fixed amount of initial quantum dots that did not dissolve in the solvent was pre-measured, and then in the process of adding an insoluble solvent to precipitate the initial quantum dots, by observing the precipitation
  • the thickness estimates the proportion of the sieved quantum dots to the weight of the initial quantum dots, so that a predetermined weight of sieved quantum dots can be collected in different time periods.
  • the precipitates are collected in sections in chronological order, so that the large particle quantum dots in the first section account for 30% of the weight of the initial quantum dots; the particle quantum dots in the middle section account for 30% of the weight of the initial quantum dots 40%; the small particle quantum dots in the latter stage account for 30% of the weight of the initial quantum dots.
  • the size of the quantum dots obtained by the sieving method in this embodiment is uniform, and the size deviation of the quantum dots obtained at each stage is less than 5%.
  • an initial quantum dot is provided, the position of the main emission peak of the initial quantum dot is 621 nm, the half-peak width is 27 nm, the particle size distribution of the quantum dot is 10 ⁇ 2 nm, and when the size deviation reaches 20%, That is, the difference between the quantum dots with the largest particle size and the smallest particle size can reach 4 nm; by using the quantum dot screening method of the present disclosure to sieve the initial quantum dots, the three-stage quantum dot particles can be obtained.
  • the emission spectra of quantum dot particles were tested, and the emission wavelengths were 622nm, 621nm and 619nm, respectively, and the half-peak widths were 24nm, 25nm and 24nm, respectively.
  • the particle size of the quantum dot particles is 10 ⁇ 0.7 nm, and the particle size of the latter quantum dot particles is 8.8 ⁇ 0.5 nm.
  • the original quantum dot sample and the three groups of samples after sieving were used as light-emitting layer materials to prepare quantum dot light-emitting diode devices.
  • the leakage current of the original sample device was relatively large at 1V voltage, and the photoelectric performance of the device was poor, and the current efficiency was 12cd. /A, mainly due to the large difference in particle size of quantum dots, and the existence of quantum dot particles with relatively large size differences, which aggravates the roughness of the film, and the film formation of the light-emitting layer is poor, resulting in poor interface contact and large leakage current of the device. .
  • the roughness of the luminescent layer film prepared by the spin coating method using the front, middle and rear quantum dots after particle size sieving is obviously better than that of the original sample, mainly because the particle size of the quantum dots is closer and the film formation is better. And the leakage current of the device is significantly improved.
  • the current efficiency of the device is 18cd/A, 17.5cd/A and 20cd/A, which is nearly 1.5 times higher than the original sample.
  • the process of flocculation and precipitation will lead to organic ligands coated on the surface of quantum dots.
  • the body part falls off, thereby affecting the luminescence properties of the quantum dots.
  • the large-particle quantum dots in the front section, the quantum dots in the middle section, and the small-particle quantum dots in the rear section are dispersed in the first solvent, respectively, to obtain a solution of large-particle quantum dots in the front section, a solution with particles in the middle section, and a rear section, respectively.
  • a small particle quantum dot solution then, respectively adding organic ligands to the front large particle quantum dot solution, the middle particle quantum dot solution and the back small particle quantum dot solution, so that the organic ligands are respectively connected to the The surface of the large particle quantum dots in the front section, the middle particle quantum dots in the middle section, and the small particle quantum dots in the rear section; finally, add the large particle quantum dot solution in the front section, the medium particle quantum dot solution in the middle section, and the small particle quantum dot solution in the rear section respectively.
  • the insoluble solvent is added for cleaning to obtain a pure and uniformly sized solution of large particle quantum dots in the front part of the target, a solution of particle quantum dots in the middle part of the target, and a solution of small particle quantum dots in the rear part of the target.
  • the initial quantum dots are II-VI compounds, III-V compounds, II-V compounds, III-VI compounds, IV-VI compounds, I-III-VI compounds, II -One or more of group IV-VI compounds and group IV elements, but not limited thereto.
  • the initial quantum dots include, but are not limited to, nanocrystals of II-VI semiconductors, such as CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgSe, HgTe, PbS, PbSe, PbTe and other binary, Ternary and quaternary II-VI compounds; nanocrystals of III-V semiconductors, such as GaP, GaAs, InP, InAs and other binary, ternary, and quaternary III-V compounds.
  • II-VI semiconductors such as CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgSe, HgTe, PbS, PbSe, PbTe and other binary, Ternary and quaternary II-VI compounds
  • III-V semiconductors such as GaP, GaAs, InP, InAs and other binary, ternary, and
  • the initial quantum dots can also be core-shell quantum dots
  • the cores constituting the core-shell quantum dots include CdSe, CdS, CdTe, CdSeTe, CdZnS, PbSe, ZnTe, CdSeS, PbS, PbTe, HgS, HgSe, At least one of HgTe, GaN, GaP, GaAs, InP, InAs, InZnP, InGaP and InGaN; the shell constituting the core-shell structure quantum dot contains at least one of ZnSe, ZnS and ZnSeS.
  • the organic ligand is a long-chain organic compound or a short-chain organic compound containing at least one of a carboxyl group, an amine group, a thiol group, and a phosphine group, but is not limited thereto.
  • the first solvent is one or more of saturated alkanes, unsaturated alkanes, saturated aromatic hydrocarbons and unsaturated aromatic hydrocarbons, but is not limited thereto.
  • the first solvent is one or more of methylene chloride, chloroform, toluene, n-hexane, cyclohexane, n-heptane, n-octane, cycloheptane and dioxane, but not limited to this.
  • the insoluble solvent is a polar solvent.
  • the insoluble solvent is one or more of methanol, ethanol, isopropanol, n-butanol, n-amyl alcohol and ethyl acetate, but not limited thereto.
  • a quantum dot light-emitting diode which includes a quantum dot light-emitting layer, and the material of the quantum dot light-emitting layer is the sieved quantum dots described in the present disclosure.
  • a quantum dot light-emitting diode is provided, as shown in FIG. 2 , which includes a substrate 10 , an anode 20 , a hole injection layer 30 , and a hole transport layer sequentially stacked from bottom to top 40.
  • the size deviation of the sieved quantum dots obtained in the present disclosure can be controlled within 5%, and their sizes are uniform, the sieved quantum dots with uniform size are used as the material of the quantum dot light-emitting layer, which can effectively reduce the The roughness of the quantum dot light-emitting layer increases the flatness of its film formation, thereby effectively improving the photoelectric performance of the quantum dot light-emitting diode.
  • the anode is selected from one or more of indium tin oxide, fluorine-doped tin oxide, indium zinc oxide, graphene, and carbon nanotubes;
  • the material of the hole injection layer is PEDOT:PSS , one or more of nickel oxide, molybdenum oxide, tungsten oxide, vanadium oxide, molybdenum sulfide, tungsten sulfide and copper oxide;
  • the hole transport layer material is one of PVK, Poly-TPD, CBP, TCTA and TFB or more;
  • the material of the electron transport layer is one or more of n-type ZnO, TiO 2 , SnO, Ta 2 O 3 , AlZnO, ZnSnO, InSnO, Alq 3 , Ca, Ba, CsF, LiF, CsCO3;
  • the cathode is selected from one or more of Al, Ca, Ba, and Ag.
  • a method for screening quantum dots comprising the following steps:
  • the surface organic coating ligand is oleic acid
  • the initial red quantum dots are concentrated, dispersed in 4ml n-octane solvent with a concentration of 100mg/ml, and in a state of constant stirring, slowly drip the insoluble solvent ethanol, when the quantum dot solution appears flocculation, Continue stirring to completely precipitate the large particles, then separate them by centrifugation, and then continue to add the insoluble solvent dropwise to the supernatant, repeat this several times, collect the 120 mg of quantum dots collected in the previous section, and add 5 ml of n-octane.
  • step 3 according to the same operation as step 2), respectively collect 150 mg of the quantum dot solution in the middle section and 110 mg of the quantum dot solution in the rear section, and the weight loss is caused by the loss during the operation.
  • the initial red quantum dots and the sieved quantum dots prepared in this example were characterized by scanning electron microscopy, and the results are shown in Figure 3- Figure 6.
  • the device structure and the selected functional layer materials are: ITO/PEDOT:PSS/TFB/QDs/ZnO/ Al; and the photoelectric properties of quantum dot light-emitting diode devices were tested, and the test results are shown in Table 1.
  • the measured current efficiency of the quantum dot light-emitting diode is 12cd/A, and its photoelectric performance is poor
  • the current efficiencies of the quantum dot light-emitting diode devices were 18cd/A, 17.5cd/A and 20cd/A, respectively.
  • the photoelectric efficiency is nearly 1.5 times higher than that of the original sample, which is mainly because the particle size of the sieved quantum dots is closer, and the film formation is better, so that the leakage current of the device is significantly improved.
  • a method for sieving quantum dots comprising the following steps:
  • step 3 according to the same operation as step 2), respectively collect 140 mg of quantum dot solution in the middle and 130 mg of the latter part, and the weight loss is caused by the loss during the operation.
  • the sieved quantum dots prepared in this example were characterized by emission spectrum and scanning electron microscope.
  • the device structure and the selected functional layer materials are: ITO/PEDOT:PSS/TFB/QDs/ZnO/ Al; and the photoelectric properties of quantum dot light-emitting diode devices were tested, and the test results are shown in Table 2.
  • the measured current efficiency of the quantum dot light-emitting diode is 45cd/A, and its photoelectric performance is poor, and when this
  • the current efficiencies of the quantum dot light-emitting diode devices were 73cd/A, 68cd/A, and 62cd/A, respectively.
  • the efficiency is greatly improved, mainly because the particle size of the sieved quantum dots is closer, and the film formation is better, so that the leakage current of the device is significantly improved.
  • the present disclosure gradually adds an insoluble solvent that is mutually soluble with the first solvent but immiscible with the organic ligand into the initial quantum dot solution.
  • the initial quantum dot solution begins to flocculate, continue to stir to make the large particles completely precipitate, and then separate them by centrifugation, and then continue to drop the supernatant with insoluble solvent, repeat this several times, segment Collect precipitates with similar particle sizes, and the size deviation of the isolated quantum dots can be controlled within 5%, so as to obtain quantum dot materials with uniform size; the quantum dots with uniform size are used as quantum dot light-emitting layer materials, The photoelectric performance of the quantum dot light-emitting diode can be effectively improved.

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Abstract

La présente invention concerne un procédé de criblage de points quantiques et une diode électroluminescente à points quantiques. Le procédé de criblage comprend les étapes suivantes consistant à : disperser des points quantiques initiaux avec les surfaces reliées à un ligand organique dans un premier solvant pour obtenir une solution de points quantiques initiale ; et ajouter progressivement un solvant non soluble dans la solution de points quantiques initiale et mélanger, précipiter progressivement des points quantiques initiaux selon l'ordre décroissant de la taille des particules, et collecter séquentiellement les précipités selon un ordre chronologique dans les étapes de façon à obtenir des points quantiques criblés, le solvant non soluble étant miscible avec le premier solvant, et n'étant pas miscible avec le ligand organique. La déviation de taille minimale des points quantiques obtenus par séparation dans la présente invention peut être régulée dans 5 %, ce qui permet d'obtenir un matériau à points quantiques de taille uniforme ; et l'utilisation des points quantiques ayant une taille uniforme en tant que matériau de couche électroluminescente à points quantiques peut améliorer efficacement les propriétés photoélectriques d'une diode électroluminescente à points quantiques.
PCT/CN2021/141020 2020-12-30 2021-12-24 Procédé de criblage de points quantiques et diode électroluminescente à points quantiques WO2022143435A1 (fr)

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