CN111234802A - Preparation method of quantum dots - Google Patents
Preparation method of quantum dots Download PDFInfo
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- CN111234802A CN111234802A CN201811432312.4A CN201811432312A CN111234802A CN 111234802 A CN111234802 A CN 111234802A CN 201811432312 A CN201811432312 A CN 201811432312A CN 111234802 A CN111234802 A CN 111234802A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 160
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920000962 poly(amidoamine) Polymers 0.000 claims abstract description 110
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- 238000000034 method Methods 0.000 claims abstract description 22
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- 125000003277 amino group Chemical group 0.000 claims abstract description 9
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- KFPMLWUKHQMEBU-UHFFFAOYSA-N 3-methylbenzenesulfonyl chloride Chemical compound CC1=CC=CC(S(Cl)(=O)=O)=C1 KFPMLWUKHQMEBU-UHFFFAOYSA-N 0.000 claims description 2
- RTQAIFXZCMVBDT-UHFFFAOYSA-N 4-(dimethylamino)benzenesulfonyl chloride Chemical compound CN(C)C1=CC=C(S(Cl)(=O)=O)C=C1 RTQAIFXZCMVBDT-UHFFFAOYSA-N 0.000 claims description 2
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
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- RKVIAZWOECXCCM-UHFFFAOYSA-N 2-carbazol-9-yl-n,n-diphenylaniline Chemical compound C1=CC=CC=C1N(C=1C(=CC=CC=1)N1C2=CC=CC=C2C2=CC=CC=C21)C1=CC=CC=C1 RKVIAZWOECXCCM-UHFFFAOYSA-N 0.000 description 1
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- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
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- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 description 1
- 239000012359 Methanesulfonyl chloride Substances 0.000 description 1
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- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
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- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
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- 125000000040 m-tolyl group Chemical group [H]C1=C([H])C(*)=C([H])C(=C1[H])C([H])([H])[H] 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- ZTLUNQYQSIQSFK-UHFFFAOYSA-N n-[4-(4-aminophenyl)phenyl]naphthalen-1-amine Chemical compound C1=CC(N)=CC=C1C(C=C1)=CC=C1NC1=CC=CC2=CC=CC=C12 ZTLUNQYQSIQSFK-UHFFFAOYSA-N 0.000 description 1
- 239000002110 nanocone Substances 0.000 description 1
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- ATGUVEKSASEFFO-UHFFFAOYSA-N p-aminodiphenylamine Chemical compound C1=CC(N)=CC=C1NC1=CC=CC=C1 ATGUVEKSASEFFO-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of quantum dots, which comprises the following steps: providing a composite material comprising a PAMAM dendrimer and metal ions bound within the PAMAM dendrimer cavity; modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amino group in the PAMAM dendrimer into an oil-soluble group to obtain an oil-soluble composite material; and mixing the oil-soluble composite material and the initial quantum dot in a non-polar solvent, so that metal ions in the oil-soluble composite material are ionized and then are coordinately combined with cation vacancies on the surface of the initial quantum dot to obtain the quantum dot. The quantum dots with few surface cationic defects can be prepared by the method, and the fluorescence intensity of the quantum dot light-emitting diode can be effectively improved by taking the quantum dots as the quantum dot light-emitting layer material of the quantum dot light-emitting diode.
Description
Technical Field
The invention relates to the field of quantum dots, in particular to a preparation method of quantum dots.
Background
There are many preparation techniques for quantum dots, and quantum dots prepared by any method have corresponding anion and cation defects on the surface layer, that is, the surface is not well grown; the exiton trap caused quenching can be caused to a certain extent by the anion and cation defects existing on the surface layer of the quantum dots.
The anion defects on the surfaces of the quantum dots can be compensated and improved by the surface ligand modifier, while the cation defects on the surfaces of the quantum dots are mainly passivated by adopting an organic metal cation precursor in the prior art, and the anion defects are further generated on the surfaces of the quantum dots by adopting the technical scheme for treatment, so that the prior art needs to be improved.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a quantum dot, a preparation method thereof and a quantum dot light-emitting diode, and aims to solve the problem that the prior art cannot effectively remove cation defects on the surface of the quantum dot.
The technical scheme of the invention is as follows:
a preparation method of quantum dots comprises the following steps:
providing a composite material comprising a PAMAM dendrimer and metal ions bound within the PAMAM dendrimer cavity;
modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amino group in the PAMAM dendrimer into an oil-soluble group to obtain an oil-soluble composite material;
and mixing the oil-soluble composite material and the initial quantum dot in a non-polar solvent, so that metal ions in the oil-soluble composite material are ionized and then combined with cation vacancies on the surface of the initial quantum dot to obtain the quantum dot.
Has the advantages that: the invention provides a preparation method of quantum dots, which is characterized in that PAMAM dendrimer combined with metal ions in a cavity is used as a passivation precursor, and surface passivation treatment is carried out on initial quantum dots to prepare the quantum dots with less surface cation defects.
Drawings
Fig. 1 is a flowchart of a method for preparing quantum dots according to a preferred embodiment of the present invention.
Detailed Description
The invention provides a preparation method of quantum dots, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, the present invention provides a flow chart of a preferred embodiment of a method for preparing quantum dots, wherein the flow chart includes the following steps:
s100, providing a composite material, wherein the composite material comprises PAMAM dendrimer and metal ions combined in a cavity of the PAMAM dendrimer;
s200, modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amino group in the PAMAM dendrimer into an oil-soluble group to obtain an oil-soluble composite material;
s300, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent, ionizing metal ions in the oil-soluble composite material, and combining the ionized metal ions with cation vacancies on the surfaces of the initial quantum dots to obtain the quantum dots.
In this embodiment, the PAMAM dendrimer having metal ions bonded in the cavity is used as a precursor of the passivation element, and the initial quantum dots are subjected to surface passivation to obtain quantum dots with fewer surface cationic defects. The mechanism for achieving the above effects is specifically as follows:
the quantum dot surface prepared by adopting the conventional oil phase technical scheme usually has more cation vacancies, and the cation vacancies on the surface of the quantum dot easily generate a coordination effect when meeting metal ions again in a certain solution environment. In this embodiment, an oil-soluble composite material obtained through modification treatment and an initial quantum dot are mixed in a non-polar solvent, metal ions in the oil-soluble composite material can be ionized, and the initial quantum dot with cation vacancies on the surface is relatively easy to generate chemical coordination when encountering free metal ions, so that the free metal ions are combined into the cation vacancies on the surface of the initial quantum dot. Therefore, in this embodiment, after the oil-soluble composite material is mixed with the quantum dot, the metal ions in the PAMAM dendrimer can fill the cation vacancies on the surface of the initial quantum dot after ionization, so as to reduce the defect state on the surface of the quantum dot.
In a preferred embodiment, the method of making the composite material comprises the steps of: providing a PAMAM dendrimer; and adding the PAMAM dendrimer into the metal ion solution, and mixing to ensure that N atoms in the PAMAM dendrimer cavity are coordinated and combined with metal ions to obtain the composite material.
In this embodiment, the PAMAM (polyamide-amine) dendrimer is obtained by reacting different molecular units a (ethylenediamine) and B (methyl acrylate), and may be synthesized by a divergent method, in the first step, ethylenediamine and methyl acrylate react to generate carboxylate, in the second step, the carboxylate obtained reacts with excess ethylenediamine, and after the above two reactions, the first generation PAMAM dendrimer may be obtained, and the above two reactions may be repeated to obtain a higher generation PAMAM dendrimer. The PAMAM dendrimer with different generations contains the molecular units A and B with the general formulas: a (2)n+2n-1+…+2n-3)+B(2n+1+2n+….+2n-1) Wherein the value of n is 3-10; in addition, the first generation PAMAM dendrimer has a general formula a +4B for molecular unit a and molecular unit B, and the second generation PAMAM dendrimer has a general formula 5A +8B for molecular unit a and molecular unit B.
The number of metal ions capable of being combined by PAMAM dendrimer of different generations is different, the main reason is that the PAMAM dendrimer of different generations has different ability of coordinating metal ions, and when the PAMAM dendrimer is from the first generation to the fourth generation, the PAMAM dendrimer is not easy to be used as a carrier for adsorbing metal ions because the concentration of peripheral functional groups (amine groups) is low.
Preferably, in this embodiment, the PAMAM dendrimer is selected from one or more of the fifth generation PAMAM dendrimer (G5), the sixth generation PAMAM dendrimer (G6), the seventh generation PAMAM dendrimer (G7), the eighth generation PAMAM dendrimer (G8), the ninth generation PAMAM dendrimer (G9), the tenth generation PAMAM dendrimer (G10), and the like. When the generation number of the PAMAM dendrimer is G5-G10, the PAMAM dendrimer of G5-G10 can be used as a candidate material for preparing a metal ion coordination bond, because the PAMAM dendrimer has more functional groups (amine groups) on the periphery and has electronegativity, and a complete and closed cavity can be formed between the functional groups by generating electrostatic interaction.
Preferably, the element species of the metal ion is selected from one or more of Mn, Zn, Cd, Hg, Pb, In, Ag, Mg, Au, Cu, Li, Al, Cd, In, Cs, Ga and Gd, but not limited thereto.
In a preferred embodiment, the step of modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amine group in the PAMAM dendrimer into an oil-soluble group to obtain the oil-soluble composite material comprises: dissolving the composite material in a polar solvent, and then adding an end group modifier to react an amino functional group on the PAMAM dendrimer in the composite material with the end group modifier to convert the amino functional group into an oil-soluble group, thereby obtaining the oil-soluble composite material.
In this embodiment, since the PAMAM dendrimer is a hydrophilic organic molecule, and the metal ion is bonded to the N atom of the terminal functional group in the PAMAM dendrimer through a coordination bond, the composite material can be stably stored and dissolved in a polar solvent to prepare a composite solution. And adding an excessive amount of end group modifier into the composite material solution under an inert atmosphere, and quickly stirring to ensure that the amino functional group on the PAMAM dendrimer reacts with the end group modifier to be converted into an oil-soluble group, thereby preparing the oil-soluble composite material. Preferably, the terminal group modifier is selected from p-toluene sulfonic acidOne or more of acid chloride, o-toluenesulfonyl chloride, m-toluenesulfonyl chloride, p-dimethylaminobenzenesulfonyl chloride, o-dimethylbenzenesulfonyl chloride, and m-dimethylaminobenzenesulfonyl chloride, but is not limited thereto. By way of example, when p-toluenesulfonyl chloride is added to the composite solution, the reaction is represented by the formula: Dendrimer-NH2+(CH3)2-N-C10H6-SOCl
Dendrimer-NHOS- C10H6-N-(CH3)2
+ HCl; when p-methanesulfonyl chloride is added to the composite solution, the reaction formula is Dendrimer-NH2+CH3-C6H4-SOOC
Dendrimer-NHSOO- C6H4- CH3(ii) a The Dendrimer-NH2PAMAM dendrimers of generations G5-G10. The composite material can be effectively dispersed in a non-polar solvent after being modified by the end group.
More preferably, the composite material is dissolved in a polar solvent at the temperature of 20-50 ℃, and then an end group modifier is added, so that an amino functional group on the PAMAM dendrimer in the composite material reacts with the end group modifier to be converted into an oil-soluble group, and the oil-soluble composite material is obtained.
In a preferred embodiment, the oil-soluble composite material and the initial quantum dots are added into a non-polar solvent according to a predetermined ratio, and the mixture is mixed to ionize metal ions in the oil-soluble composite material and then coordinate and combine with cation vacancies on the surfaces of the initial quantum dots to obtain the quantum dots.
The metal ions in the oil-soluble composite material can be efficiently coordinated and combined with the cation vacancies on the surface of the quantum dot, and other unnecessary anions are not introduced to influence the passivation effect of the quantum dot.
Preferably, the molar mass ratio of the oil-soluble composite material to the initial quantum dots is related to the generation number of the PAMAM dendrimer, because the PAMAM dendrimer of different generation numbers has different abilities to coordinate metal ions, so that the amount of the PAMAM dendrimer combined with the metal ions is different. Taking the example that the number of the PAMAM dendrimer coordination-bound metal ions reaches the maximum, when the PAMAM dendrimer in the composite material is a fifth generation PAMAM dendrimer, the weight ratio of the molar weight of the fifth generation PAMAM dendrimer to the initial quantum dots is 1 mmol: (1-100) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent. Preferably, when the PAMAM dendrimer in the composite material is a sixth generation PAMAM dendrimer, the molar weight of the sixth generation PAMAM dendrimer to the mass ratio of the initial quantum dots is 1 mmol: (10-150) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent. Preferably, when the PAMAM dendrimer in the composite material is a seventh generation PAMAM dendrimer, the ratio of the molar weight of the seventh generation PAMAM dendrimer to the mass of the initial quantum dots is 1 mmol: (50-200) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent. Preferably, when the PAMAM dendrimer in the composite material is an eighth generation PAMAM dendrimer, the molar weight of the eighth generation PAMAM dendrimer to the mass ratio of the initial quantum dots is 1 mmol: (100-250) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent. Preferably, when the PAMAM dendrimer in the composite material is a ninth generation PAMAM dendrimer, the ratio of the molar weight of the ninth generation PAMAM dendrimer to the mass of the initial quantum dots is 1 mmol: (150-300) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent. Preferably, when the PAMAM dendrimer in the composite material is a tenth generation PAMAM dendrimer, the molar weight of the tenth generation PAMAM dendrimer is 1mmol relative to the mass of the initial quantum dots: (200-500) mg, mixing the oil-soluble composite material and the initial quantum dots in a non-polar solvent.
In a more preferred embodiment, the PAMAM dendrimer is selected from one or both of a fifth generation PAMAM dendrimer and a sixth generation PAMAM dendrimer. Because metal ions in the composite material can generate chemical bonds with a plurality of N atoms in gaps of the PAMAM dendrimer terminal functional groups, the pyrolysis rate of the metal ions in the composite material is much slower than that of the organic metal precursor; and the PAMAM dendrimer containing the metal ions has higher corresponding viscosity along with the increase of the generation number, and the higher the viscosity, the lower the coordination and combination efficiency of the metal ions and the cation vacancies on the surface of the initial quantum dot is. Therefore, in order to ensure that the metal ions in the composite material can be more efficiently coordinated and combined with the cation vacancies on the surface of the quantum dot, the PAMAM dendrimer is preferably selected from one or two of the fifth generation PAMAM dendrimer and the sixth generation PAMAM dendrimer.
In a preferred embodiment, the oil-soluble composite material and the quantum dots are added into a non-polar solvent, and mixed under the condition of 80-300 ℃ to enable metal ions in the oil-soluble composite material to be combined with cation vacancies on the surfaces of the quantum dots to obtain the quantum dots. When the temperature of the PAMAM dendrimer (oil-soluble composite material) which is modified by the end group and contains the metal ions in the nonpolar solvent is higher than a certain value, the metal ions can be separated from the dendrimer and enter the nonpolar solvent to participate in other chemical reactions, and the temperature range of the metal ions in different generations of PAMAM dendrimer being capable of being separated from the PAMAM dendrimer is 800-300 ℃. Therefore, in order to ensure that the metal ions in the oil-soluble composite material can be coordinately bound with the cation vacancies on the surface of the quantum dot, the oil-soluble composite material and the quantum dot are preferably mixed at a temperature of 80 to 300 ℃.
In a preferred embodiment, the oil-soluble composite and the quantum dots are added to a non-polar solvent, wherein the metal ions in the oil-soluble composite are the same elements as the cations on the surface of the quantum dots. By way of example, when the surface cation of the quantum dot to be passivated is Zn2+When the metal ion is Zn, the metal ion in the oil-soluble composite material which is coordinated and combined with the N atom in the gap of the PAMAM dendrimer terminal functional group is Zn2+. When the metal ions in the oil-soluble composite material are on the surface of the quantum dotsWhen the cations are the same elements, the passivated effect can effectively reduce the defects on the surface of the quantum dot and improve the fluorescence intensity of the luminescent quantum dot.
In a preferred embodiment, the metal ions in the oil-soluble composite material are different elements from the cations on the surface of the quantum dots. By way of example, when the cation on the surface of the quantum dot to be passivated is Cd2+When the metal ion in the oil-soluble composite material is Zn2+. When the metal ions in the oil-soluble composite material are different from the cationic elements on the surface of the quantum dot, if the band gap of the passivated quantum dot surface compound is larger than that of the inner shell layer, the fluorescence intensity of the quantum dot can be enhanced, and the stability of the quantum dot can also be improved.
In a preferred embodiment, the quantum dot is selected from one of a single type quantum dot, a core-shell quantum dot or an alloy structure quantum dot. By way of example, the group III-V single quantum dots are selected from one or more of GaN, GaP, GaAs, InP, InAs, InAsP, GaAsP, InGaP, InGaAs, and InGaAsP. The II-VI single quantum dots are selected from one or more of CdSe, CdS, CdTe, ZnSe, ZnS, ZnTe, HgSe, HgS and HgTe. The III-V group and II-VI group alloy structure quantum dots are selected from one or more of InPZnS, InPZnSe, InPZnSeS, InGaP ZnSe, InGaP ZnS and InGaP ZnSeS. The II-VI family core-shell quantum dots are selected from one or more of CdHgTe/CdS, CdTe/CdS, CdSe/ZnS, CdSeS/CdS and ZnSe/ZnS.
The invention also provides a quantum dot, wherein the quantum dot is prepared by the method.
The invention also provides a quantum dot light-emitting diode which comprises a quantum dot light-emitting layer, wherein the quantum dot light-emitting layer is made of the quantum dot material prepared by the preparation method.
Because the quantum dots provided by the invention have fewer surface cationic defects, the quantum dots with fewer surface defects prepared by the invention are used as the quantum dot light-emitting layer material of the quantum dot light-emitting diode, and the fluorescence intensity of the quantum dot light-emitting diode can be effectively improved.
In a preferred embodiment, the quantum dot light emitting diode comprises an anode, a hole transport layer, a quantum dot light emitting layer, an electron transport layer and a cathode which are arranged in a stacked manner, wherein the material of the quantum dot light emitting layer is the quantum dot prepared by the preparation method provided by the invention.
It should be noted that the invention is not limited to the quantum dot light emitting diode with the above structure, and may further include an interface functional layer or an interface modification layer, including but not limited to one or more of an electron blocking layer, a hole blocking layer, an electrode modification layer, and an isolation protection layer. The quantum dot light emitting diode can be partially packaged, fully packaged or not packaged.
The following describes the structure of a quantum dot light emitting diode (QLED) including a hole transport layer and a method for manufacturing the same in detail:
the QLED may be classified into a forward-mounted structure QLED and a flip-chip structure QLED according to the emission type of the QLED.
In a preferred embodiment, the QLED with the forward mounting structure comprises an anode (the anode is stacked on a substrate), a hole transport layer, a quantum dot light-emitting layer, an electron transport layer and a cathode, wherein the anode is stacked from bottom to top, and the quantum dot light-emitting layer is made of the quantum dot material prepared by the preparation method of the invention.
In another preferred embodiment, the QLED with the flip-chip structure comprises a cathode (the cathode stack is disposed on a substrate), an electron transport layer, a quantum dot light-emitting layer, a hole transport layer and an anode, wherein the cathode stack is stacked from bottom to top, and the quantum dot light-emitting layer is made of the quantum dot material prepared by the preparation method of the present invention.
Preferably, the material of the anode is selected from doped metal oxides; wherein the doped metal oxide includes, but is not limited to, one or more of indium-doped tin oxide (ITO), fluorine-doped tin oxide (FTO), antimony-doped tin oxide (ATO), aluminum-doped zinc oxide (AZO), gallium-doped zinc oxide (GZO), indium-doped zinc oxide (IZO), magnesium-doped zinc oxide (MZO), and aluminum-doped magnesium oxide (AMO).
Preferably, the material of the hole transport layer is selected from organic materials having good hole transport ability, such as but not limited to Poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), Polyvinylcarbazole (PVK), Poly (N, N 'bis (4-butylphenyl) -N, N' -bis (phenyl) benzidine) (Poly-TPD), Poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-Phenylenediamine) (PFB), 4', 4 "-tris (carbazol-9-yl) triphenylamine (TCTA), 4' -bis (9-Carbazole) Biphenyl (CBP), N '-diphenyl-N, N' -bis (3-methylphenyl) -1, one or more of 1 '-biphenyl-4, 4' -diamine (TPD), N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine (NPB), doped graphene, undoped graphene, and C60.
Preferably, the material of the cathode is selected from one or more of a conductive carbon material, a conductive metal oxide material and a metal material; wherein the conductive carbon material includes, but is not limited to, one or more of doped or undoped carbon nanotubes, doped or undoped graphene oxide, C60, graphite, carbon fibers, and porous carbon; the conductive metal oxide material includes, but is not limited to, one or more of ITO, FTO, ATO, and AZO; metallic materials include, but are not limited to, Al, Ag, Cu, Mo, Au, or alloys thereof; wherein, the metal material has a form including but not limited to one or more of a compact film, a nanowire, a nanosphere, a nanorod, a nanocone and a hollow nanosphere.
The invention also provides a preparation method of the QLED with the positive-mounted structure and the hole transport layer, which comprises the following steps:
providing a substrate containing an anode, and preparing a hole transport layer on the anode;
preparing a quantum dot light-emitting layer on the hole transport layer, wherein the quantum dot light-emitting layer is made of the quantum dot prepared by the preparation method;
preparing an electron transport layer on the quantum dot light emitting layer;
and preparing a cathode on the electron transport layer to obtain the QLED.
The invention also provides a preparation method of the QLED with the inverted structure and the hole transport layer, which comprises the following steps:
providing a substrate containing a cathode, and preparing an electron transport layer on the cathode;
preparing a quantum dot light-emitting layer on the electron transmission layer, wherein the quantum dot light-emitting layer is made of the quantum dot prepared by the preparation method;
preparing a hole transport layer on the quantum dot light emitting layer;
and preparing an anode on the hole transport layer to obtain the QLED.
The preparation method of each layer can be a chemical method or a physical method, wherein the chemical method comprises one or more of but not limited to a chemical vapor deposition method, a continuous ion layer adsorption and reaction method, an anodic oxidation method, an electrolytic deposition method and a coprecipitation method; physical methods include, but are not limited to, physical coating methods or solution methods, wherein solution methods include, but are not limited to, spin coating, printing, knife coating, dip-coating, dipping, spraying, roll coating, casting, slot coating, bar coating; physical coating methods include, but are not limited to, one or more of thermal evaporation coating, electron beam evaporation coating, magnetron sputtering, multi-arc ion coating, physical vapor deposition, atomic layer deposition, pulsed laser deposition.
In summary, the present invention provides a method for preparing quantum dots, in which PAMAM dendrimer having metal ions bonded in a cavity is used as a passivation precursor, and a surface passivation treatment is performed on the initial quantum dots to obtain quantum dots with fewer surface cationic defects. Furthermore, the quantum dots are used as the quantum dot light-emitting layer material of the quantum dot light-emitting diode, so that the fluorescence intensity of the quantum dot light-emitting diode can be effectively improved.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of quantum dots is characterized by comprising the following steps:
providing a composite material comprising a PAMAM dendrimer and metal ions bound within the PAMAM dendrimer cavity;
modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amino group in the PAMAM dendrimer into an oil-soluble group to obtain an oil-soluble composite material;
and mixing the oil-soluble composite material and the initial quantum dot in a non-polar solvent, so that metal ions in the oil-soluble composite material are ionized and then combined with cation vacancies on the surface of the initial quantum dot to obtain the quantum dot.
2. The method for preparing the quantum dot according to claim 1, wherein the PAMAM dendrimer is selected from one or more of the PAMAM dendrimers of the fifth generation to the tenth generation.
3. The method for preparing the quantum dot according to claim 1, wherein the PAMAM dendrimer is selected from one or two of the generation five and generation six PAMAM dendrimers.
4. The method for preparing the quantum dot according to claim 1, wherein the element species of the metal ions are selected from one or more of Mn, Zn, Cd, Hg, Pb, In, Ag, Mg, Au, Cu, Li, Al, Cd, In, Cs, Ga and Gd.
5. The method for preparing the quantum dot according to claim 1, wherein the step of modifying the PAMAM dendrimer terminal functional group in the composite material to convert the amine group in the PAMAM dendrimer into an oil-soluble group comprises:
dissolving the composite material in a polar solvent, and then adding an end group modifier to react an amino functional group on the PAMAM dendrimer in the composite material with the end group modifier to convert the amino functional group into an oil-soluble group, thereby obtaining the oil-soluble composite material.
6. The method for preparing the quantum dot according to claim 5, wherein the end group modifier is selected from one or more of p-toluenesulfonyl chloride, o-toluenesulfonyl chloride, m-toluenesulfonyl chloride, p-dimethylaminobenzenesulfonyl chloride, o-dimethylbenzenesulfonyl chloride and m-dimethylaminobenzenesulfonyl chloride.
7. The preparation method of the quantum dot according to claim 5, wherein the composite material is dissolved in a polar solvent at 20-50 ℃, and then an end group modifier is added, so that an amine functional group on the PAMAM dendrimer in the composite material reacts with the end group modifier to be converted into an oil-soluble group, thereby obtaining the oil-soluble composite material.
8. The method for preparing the quantum dot according to claim 2, wherein when the PAMAM dendrimer in the composite material is a fifth generation PAMAM dendrimer, the ratio of the molar weight of the fifth generation PAMAM dendrimer to the mass of the initial quantum dot is 1 mmol: (1-100) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing;
and/or when the PAMAM dendrimer in the composite material is a sixth generation PAMAM dendrimer, the molar weight of the sixth generation PAMAM dendrimer is 1mmol to the mass ratio of the initial quantum dots: (10-150) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing;
and/or when the PAMAM dendrimer in the composite material is a seventh generation PAMAM dendrimer, the ratio of the molar weight of the seventh generation PAMAM dendrimer to the mass of the initial quantum dots is 1 mmol: (50-200) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing;
and/or when the PAMAM dendrimer in the composite material is an eighth generation PAMAM dendrimer, the molar weight of the eighth generation PAMAM dendrimer is 1mmol to the mass ratio of the initial quantum dots: (100-250) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing;
and/or when the PAMAM dendrimer in the composite material is a ninth generation PAMAM dendrimer, the molar weight of the ninth generation PAMAM dendrimer is 1mmol to the mass ratio of the initial quantum dots: (150-300) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing;
and/or when the PAMAM dendrimer in the composite material is a tenth generation PAMAM dendrimer, the molar weight of the tenth generation PAMAM dendrimer is 1mmol to the mass ratio of the initial quantum dots: (200- & ltSUB & gt 500- & gt) mg, adding the oil-soluble composite material and the initial quantum dots into a non-polar solvent for mixing.
9. The preparation method of the quantum dot according to claim 7, wherein the oil-soluble composite material and the initial quantum dot are mixed in a nonpolar solvent at the temperature of 80-300 ℃, so that metal ions in the oil-soluble composite material are ionized and then are coordinately combined with cation vacancies on the surface of the initial quantum dot to obtain the quantum dot.
10. The preparation method of the quantum dot according to claim 7, wherein the quantum dot is a single-type quantum dot, a core-shell quantum dot or an alloy-structured quantum dot.
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| CN107936943A (en) * | 2017-12-05 | 2018-04-20 | 华南师范大学 | A kind of quantum dot fluorescence intensity enhancing method based on dendrimer |
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| CN107936943A (en) * | 2017-12-05 | 2018-04-20 | 华南师范大学 | A kind of quantum dot fluorescence intensity enhancing method based on dendrimer |
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