CN105070849A - Light-emitting device with compactly arranged quantum dot light-emitting layer and preparation method thereof - Google Patents
Light-emitting device with compactly arranged quantum dot light-emitting layer and preparation method thereof Download PDFInfo
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- CN105070849A CN105070849A CN201510410824.0A CN201510410824A CN105070849A CN 105070849 A CN105070849 A CN 105070849A CN 201510410824 A CN201510410824 A CN 201510410824A CN 105070849 A CN105070849 A CN 105070849A
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- H—ELECTRICITY
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
Abstract
The invention discloses a light-emitting device with a compactly arranged quantum dot light-emitting layer and a preparation method thereof. Another compound solution playing a role in crosslinking is added to the quantum dot light-emitting layer, so quantum dot surface ligand exchange is achieved, and then the crosslinking is performed. Through crosslinking processing of the quantum dots, the prepared quantum dots are arranged uniformly and compactly and do not have defects of a pinhole, a crack and the like, and a leakage current does not exist, so the problem of an impure spectrum and the like which are caused by efficiency reduction of a quantum dot light-emitting diode or light emitting of other adjacent charge transmission layers are effectively solved. Radiation composite light-emitting efficiency can be improved, and then efficiency of the quantum dot light-emitting diode is improved.
Description
Technical field
The present invention relates to QLED light emitting device technologies field, particularly relate to fine and close luminescent device of a kind of quantum dot light emitting layer arrangement and preparation method thereof.
Background technology
Quantum dot can be described as semiconductor nano again, is that radius is less than or close to the nano-crystalline granule of bohr exciton radii.Quantum dot size is very little, and its particle diameter is generally between 1-20nm.Quantum dot has quantum confined effect, and continuous print band structure becomes the discrete energy levels structure with molecular characterization, can emitting fluorescence after being excited, and quantum dot has unique characteristics of luminescence, and it is had broad application prospects at opto-electronics.QLED luminescent device is exactly that Colloidal Quantum Dots is adopted the device prepared of sandwich structure as luminescent layer, namely between different electric conducting materials, introduces luminescent layer thus obtains the light of required wavelength.QLED compares organic luminescent device, and the glow color of QLED can adjust with quantum dot size on the one hand; On the other hand because quantum dot half-peak breadth is narrower, improve color saturation, therefore can be used for flat panel display.
Quantum dot dispersibles in the solution simultaneously, has the characteristic of solution-processible, therefore can prepare QLED device by various ways such as spin coating, injection, blade coating, inkjet printings.And ink-jet printing technology can accurately by quantum dot light emitting deposition of material in position in the desired amount, allow semi-conducting material uniform deposition form thin layer, effectively control thickness, reduce material unaccounted-for (MUF), reduce costs.Three primary colors display can also be realized simultaneously, manufacture large scale QLED screen.But it is fine and close not to there is quantum dot arrangement, there is the phenomenons such as leakage current.Cause degradation under device efficiency.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, luminescent device that the object of the present invention is to provide the arrangement of a kind of quantum dot light emitting layer fine and close and preparation method thereof, is intended to solve existing quantum dot arrangement densification not, there is the phenomenons such as leakage current, the problem that device efficiency is low.
Technical scheme of the present invention is as follows:
A preparation method for the luminescent device that quantum dot light emitting layer arrangement is fine and close, wherein, comprises step:
A, spin coating hole injection layer are on anode layer, and then spin coating hole transmission layer is on hole injection layer;
The quantum dot light emitting layer of B, subsequently spin coating densification arrangement is on hole transmission layer, wherein, concrete steps are: quantum dot is configured to quantum dot solution, then quantum dot solution is spin-coated on hole transmission layer, obtained quantum dot light emitting layer, then on quantum dot light emitting layer, add a compound solution playing crosslinked action with the surface ligand of quantum dot be cross-linked, obtain the quantum dot light emitting layer of fine and close arrangement;
On the quantum dot light emitting layer that C, last spin coating electron transfer layer are arranged in densification, then spin coating electron injecting layer is on electron transfer layer, and evaporation cathode layer is on electron injecting layer, obtains light emitting diode with quantum dots.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, in described step B, the surface ligand of described quantum dot is that end is with-NH
2,-COOH ,-SO
3the part of the group of H ,-OH or-SH.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, in described step B, described compound is with difunctional or multi-functional compound, and described difunctional or multi-functional compound are the compound with two or more-NCO, epoxide group, acrylate or double bond group.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, in described step B, the surface ligand of described quantum dot is the part that the group of crosslinked action can occur of end with double bond.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, the surface ligand of described quantum dot is propylene bisphosphate, allylamine, allyl alcohol, allyl mercaptan, acrylic acid, the acrylate hydroxy ester containing hydroxy functional group or double bond containing disulphide.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, in described step B, the surface ligand of described quantum dot is the quantum dot stability shell through surface prepared by stability modification with double bond group.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close; wherein; described surface is that quantum dot warp contains the process of (methyl) acryl silane with the quantum dot stability shell of double bond group, and the end prepared is with the SiO of (methyl) acryl group
2quantum dot/the SiO of the nucleocapsid structure of shell
2compound.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, described compound is with difunctional or multi-functional compound, and described difunctional or multi-functional compound are two mercaptan, carbon-carbon double bond or esters of acrylic acid unsaturated comonomer.
The preparation method of the luminescent device that described quantum dot light emitting layer arrangement is fine and close, wherein, in described step B, described crosslinked crosslinking curing mode is ultraviolet light cross-linking solidification, heat cross-linking solidification or catalytic reagent crosslinking curing.
The luminescent device that quantum dot light emitting layer arrangement is fine and close, it adopts the preparation method of the as above luminescent device that arbitrary described quantum dot light emitting layer arrangement is fine and close to be prepared from.
Beneficial effect: the present invention is cross-linked by the compound solution adding a kind of crosslinked action on quantum dot light emitting layer, make quantum dot arrangement even compact in the quantum dot light emitting layer obtained, and there is no pin hole, the defects such as crack, leakage current can not be there is, thus it is luminous to efficiently solve light emitting diode with quantum dots decrease in efficiency or other adjacent charge transport layers, the problem such as cause spectrum impure; And radiation recombination luminous efficiency can be improved, and then improve light emitting diode with quantum dots efficiency.
Embodiment
The invention provides fine and close luminescent device of a kind of quantum dot light emitting layer arrangement and preparation method thereof, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides the preparation method of the fine and close luminescent device of a kind of quantum dot light emitting layer arrangement, it comprises step:
A, spin coating hole injection layer are on anode layer, and then spin coating hole transmission layer is on hole injection layer;
The quantum dot light emitting layer of B, subsequently spin coating densification arrangement is on hole transmission layer, wherein, concrete steps are: quantum dot is configured to quantum dot solution, then quantum dot solution is spin-coated on hole transmission layer, obtained quantum dot light emitting layer, then on quantum dot light emitting layer, add a compound solution playing crosslinked action with the surface ligand of quantum dot be cross-linked, obtain the quantum dot light emitting layer of fine and close arrangement;
On the quantum dot light emitting layer that C, last spin coating electron transfer layer are arranged in densification, then spin coating electron injecting layer is on electron transfer layer, and evaporation cathode layer is on electron injecting layer, obtains light emitting diode with quantum dots.
The present invention by adding the compound solution of a kind of crosslinked action on quantum dot light emitting layer, realize the chemical combination of the surface ligand of compound and quantum dot, thus be cross-linked, make quantum dot arrangement even compact in the quantum dot light emitting layer obtained, and there is no pin hole, the defects such as crack, can not leakage current be there is, and then it is luminous to efficiently solve light emitting diode with quantum dots decrease in efficiency or other adjacent charge transport layers, the problem such as cause spectrum impure; And radiation recombination luminous efficiency can be improved, thus improve light emitting diode with quantum dots efficiency.
Described step B is specially, quantum dot is configured to quantum dot solution, then quantum dot solution is spin-coated on hole transmission layer, obtained quantum dot light emitting layer on hole transmission layer, then on quantum dot light emitting layer, add a compound solution that cross-linking reaction can occur with the surface ligand of quantum dot be cross-linked, thus obtain the quantum dot light emitting layer of fine and close arrangement.The invention is not restricted to described spin coating mode, by the mode of blade coating or inkjet printing, quantum dot solution can also be applied on hole transmission layer.
In described step B, the solvent of configuration quantum dot solution is organic solvent, and described organic solvent can be the mixture of non-polar solven or non-polar solven and polar solvent.Wherein, described non-polar solven can be single non-polar solven, the mixture of two kinds of non-polar solvens or the mixture of multiple non-polar solven.Preferably, boiling point is selected to be that the mixture of long chain hydrocarbon, alcohol, ester and ether between 40-250 DEG C is as organic solvent.Preferably, described hydrocarbon is straight or branched alkane, and such as, described hydrocarbon is C6-10 alkane.Described organic solvent can be chlorobenzene, o-dichlorohenzene, oxolane, methyl phenyl ethers anisole, morpholine, toluene, ortho-xylene, meta-xylene, paraxylene, alkyl benzene, nitrobenzene, n-hexane, cyclohexane, normal heptane, cycloheptane, dioxane, carrene, chloroform, dichloroethanes, chloroform, chlorobenzene, 1,4 dioxanes, 1,2 dichloroethanes, 1,1,1-trichloroethanes, 1,1,2,2-tetrachloroethanes, naphthane, naphthalane, N, a kind of or several mixture in dinethylformamide, DMA, dimethyl sulfoxide solvent.
Preferably, described polar solvent is the polar solvent that alcohol or other polar liquids of alcohol and at least one combine.More preferably, described polar solvent comprises the monoalky lether of methyl alcohol, ethanol, isopropyl alcohol, butanols, amylalcohol, 2-methyl cellosolve, acetone, methyl ethyl ketone, ethyl acetate, butyl acetate, dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO) or ethylene glycol, propylene glycol and polyethylene glycol, one or more in ethylene glycol monobutyl ether, dipropylene glycol monomethyl ether.
In described step B, quantum dot light emitting layer adds a compound solution playing crosslinked action with the surface ligand of quantum dot be cross-linked, its concrete preparation process is: at the complete quantum dot solution of spin coating, after making quantum dot light emitting layer, quantum dot light emitting layer being dipped in the temperature that can play crosslinked action with the surface ligand of quantum dot is that in the compound solution of 30 ~ 100 DEG C, 1 ~ 10min is cross-linked, then quantum dot light emitting layer taken out and repeatedly clean 5min with pure small molecule solvent, then rinse with isopropyl alcohol and drying under nitrogen flowing, then by quantum dot light emitting layer in nitrogen glove box after 100 ~ 200 DEG C, annealing 5 ~ 60min, obtain the quantum dot light emitting layer of fine and close arrangement on hole transmission layer.
In described step B, the chemical combination of the surface ligand of compound and quantum dot, can be that compound carries out chemical combination from parts different on a quantum dot, also can be that the part between compound from different quantum dot carries out chemical combination.In other words, be namely the surface ligand that can act on same quantum dot for crosslinked compound, also can be act on the surface ligand of a different quantum dot, the surface ligand realizing compound and quantum dot be cross-linked.
Preferably, the surface ligand that can carry out the described quantum dot be cross-linked comprises end with-NH
2,-COOH ,-SO
3h ,-OH ,-SH and-CH=CH
2etc. the part of group that crosslinked action can occur.Wherein, end is with-NH
2,-COOH ,-SO
3h, the surface ligand that the quantum dot of the group of crosslinked action can occur-OH or-SH etc. comprises TGA, mercaptopropionic acid, mercaptobutyric acid, 11-sulfydryl-1-undecyl alcohol, sulfydryl oleic acid, mercaptoethylmaine, sulfydryl oleyl amine, 1,2-propane diamine, 1,6-hexamethylene diamine, 1,7-heptamethylene diamine, 1,8-octamethylenediamine, 1,9-nonamethylene diamine, 1,10-decamethylene diamine, 1,6-adipic acid, 1,7-pimelic acid, 1,8-suberic acid, 1,9-azelaic acid, 1,10-decanedioic acid, 1,1,2-second three acid, 1,2,7-acid in heptan three, the own disulfonic acid of 1,6-, 1,7-disulfonic acid in heptan, the pungent disulfonic acid of 1,8-, 1,9-disulfonic acid in the ninth of the ten Heavenly Stems, 1,5 naphthalenedisulfonic acids, 1,6-hexylene glycol, 1,7-heptandiol, 1,8-ethohexadiol, 1,9-nonanediol, 1,10-decanediol, 1,3-dimercaptopropane, Isosorbide-5-Nitrae-succinimide mercaptans, 1,5-pentane disulfide thioalcohol, 1,6-ethanthiol, 1,7-mercaptan in heptan two, pungent two mercaptan of 1,8-, 1,9-mercaptan in the ninth of the ten Heavenly Stems two, 1,10-mercaptan in the last of the ten Heavenly stems two, 6-aminocaprolc acid, 7-aminoheptylic acid, 8-aminocaprylic acid, 9 aminononanoic acid, 10-aminocapric acid, diaminopimelic acid, three (3-hydroxypropyl) phosphine, 2-mercaptobenzoic acid, 3-mercaptobenzoic acid, 4-mercaptobenzoic acid, triethanolamine, isopropanolamine, two (3-the aminopropyl)-Putriscine of N, N'-, 4-amino-5-hydroxyl-2,7-naphthalenedisulfonic acid.
In described step B, the surface ligand of described quantum dot is that end is with-NH
2,-COOH ,-SO
3during the part of the group of H ,-OH or-SH, the corresponding described compound carrying out being cross-linked with the surface ligand of quantum dot described in it is for difunctional or multi-functional compound, and described difunctional or multi-functional compound can be the compound with two or more-NCO, epoxide group, acrylate or double bond group.Above-mentioned difunctional or multi-functional compound can with the surface ligand generation cross-linking reaction of above-mentioned quantum dot.The compound of two or more-NCO described, epoxide group, acrylate or double bond group can be but be not limited to 1,6-hexyl diisocyanate, 1,7-heptyl vulcabond, 1,8-octyl diisocyanate, 1,9-nonyl vulcabond, ethylene glycol diglycidylether, propylene glycol diglycidylether, butanediol diglycidyl ether, neopentylglycol diglycidyl ether, hexanediol diglycidyl ether, glycol diacrylate, propylene glycol diacrylate or Glycerin triacrylate etc.
In described step B, the surface ligand of described quantum dot can have double bond (such as ,-CH=CH for end strips
2) etc. the part that the group of crosslinked action can occur.Wherein, end is with double bond (such as ,-CH=CH
2) etc. the part that the group of crosslinked action can occur comprise propylene bisphosphate, allylamine, allyl alcohol, allyl mercaptan, acrylic acid, (methyl) acrylate hydroxy ester containing hydroxy functional group (such as, (methyl) acrylic acid-α-hydroxyl ethyl ester, (methyl) senecioate-hydroxyl ethyl ester, (methyl) hydroxyethyl methacrylate and (methyl) hy-droxybutyl), and double bond containing disulphide (such as, mercaptopropionic acid allyl acid amides, mercaptopropionic acid (Beta-methyl acrylate) ethyl ester, lipoic acid allyl acid amides, lipoic acid (Beta-methyl acrylate) ethyl ester) etc.
In described step B, when the surface ligand of quantum dot be not double bond containing surface ligand time, the present invention takes to carry out stability modification to the surface ligand of described quantum dot, makes the surface ligand of described quantum dot be quantum dot stability shell through surface prepared by stability modification with double bond group.Particularly, described surface is that quantum dot warp contains the process of (methyl) acryl silane with the quantum dot stability shell of double bond group, and the end prepared is with the SiO of (methyl) acryl group
2quantum dot/the SiO of the nucleocapsid structure of shell
2compound.Preferably, described (methyl) acryl silane comprises 3-(methacryloxy) propyl trimethoxy silicane, 3-acryloxypropyl trimethoxy silane, 3-(methacryloxy) hydroxypropyl methyl dimethoxysilane, 3-(acryloxypropyl) methyl dimethoxysilane, 3-(methacryloxy) dimethylamine methoxylsilane, 3-(acryloxypropyl) dimethyl methoxy silane, 3-(methacryloxy) propyl trimethoxy silicane, 3-methacryloxypropyl dimethylethoxysilane, 3-methacryloxypropyl methyldiethoxysilane, 3-methacryloxypropyl, 3-methacryloxypropyl triethoxysilane, 3-methacryloyloxypropyl methyl diethoxy silane, methacryloxymethyl three (trimethylsiloxy group) silane, two (trimethylsiloxy group) silane of (3-acryloxy) methyl, N-(3-acryloxy-2-hydroxypropyl)-3-aminopropyl triethoxysilane, (3-acryloxypropyl) three (trimethylsiloxy group) silane, two (trimethylsiloxy group) methyl of (3-methacryloxy-2-hydroxy propyloxy group) propyl group.In above-mentioned silane, (methyl) acryl silane has pliability more better than acryl silane usually.
In the present invention, when the surface ligand of described quantum dot is that end is with-CH=CH
2can there is the part of the group of crosslinked action time, corresponding is with difunctional or multi-functional compound with the described compound of the surface ligand generation cross-linking reaction of described quantum dot.Preferably, described difunctional or multi-functional compound can be two mercaptan (such as, 1, 3-dimercaptopropane, 1, 4-succinimide mercaptans, 1, 5-pentane disulfide thioalcohol, 1, 6-ethanthiol, 1, 7-mercaptan in heptan two, 1, pungent two mercaptan of 8-, 1, 9-mercaptan in the ninth of the ten Heavenly Stems two, 1, 10-mercaptan in the last of the ten Heavenly stems two), carbon-carbon double bond (such as, divinylbenzene, trivinylbenzene, diallyl ether), and other suitable esters of acrylic acid unsaturated comonomers (such as, (methyl) acrylic acid triethylene glycol monoesters, (methyl) methoxyethyl multicondensed ethylene glycol ester, (methyl) acrylate, butoxy propylene glycol ester, 1, 6-hexanediyl ester, double trimethylolpropane tetraacrylate) etc.
Preferably, described compound solution forms by being dissolved in configuration in Small molecule organic solvents containing difunctional or the multi-functional part that can be used for being cross-linked.Particular by by containing difunctional or the multi-functional part that can be used for being cross-linked, be dissolved in the Small molecule organic solvents such as alcohols, ketone, amide-type, ester class, ethers and configure crosslinker solution, wherein, in compound solution, the concentration of difunctional or multi-functional part is 5-50mM.The present invention by adopting same or multiple difunctionality or the different quantum dot of multi-functional ligand substituting surface ligand, thus realizes the crosslinked of quantum dot.Preferably, described Small molecule organic solvents is the lipids such as the ketones such as methyl alcohol, ethanol, isopropyl alcohol, butanols, amylalcohol, 2-methyl cellosolve, acetone, methylethylketone, methyl ethyl ketone, methyl iso-butyl ketone (MIBK), cyclohexanone, 1-METHYLPYRROLIDONE, dimethyl formamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), ethyl acetate, n-butyl acetate or acetic acid 1-methoxyl group-2-propyl diester, one or more in the monoalky lether (such as, ethylene glycol monobutyl ether, dipropylene glycol monomethyl ether) of ethylene glycol, propylene glycol and polyethylene glycol.
In described step B, be that end is with-CH=CH at the surface ligand of described quantum dot
2deng the part that the group of crosslinked action can occur, or the surface ligand of quantum dot is when being the quantum dot stability shell through surface prepared by stability modification with double bond group, the crosslinking curing mode that quantum dot light emitting layer of the present invention carries out being cross-linked with the compound solution playing crosslinked action can be solidified for ultraviolet light cross-linking, heat cross-linking solidifies or other catalytic reagent crosslinking curings.In addition, the present invention also takes to be added into a small amount of radical initiator in quantum dot solution, then by the quantum dot solution spin coating containing radical initiator, spraying or inkjet printing hole transmission layer, then on obtained quantum dot light emitting layer, added the compound solution of crosslinked action, finally by quantum dot light emitting layer under ultraviolet light or heating condition, also or under the catalytic reagent be applicable to carry out cross-linking and curing reaction, thus form crosslinked quantum dot light emitting layer.
Preferably, when above-mentioned crosslinked crosslinking curing mode is heat cross-linking solidification, described radical initiator is free radical thermal initiator, and described free radical thermal initiator can be one or more in azo, peroxide, persulfate, redox initiator.
Preferably, when above-mentioned crosslinked crosslinking curing mode is ultraviolet light cross-linking solidification, described radical initiator is free radical photo-initiation, described free radical photo-initiation comprises the light trigger that can be used for UV curing acrylic ester polymer, such as, can be 2-hydroxy-2-methyl-1-phenyl-1 acetone, 2, 2-dimethoxy-2-phenyl acetophenone, 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholinyl-1-acetone, 1-hydroxycyclohexyl phenyl ketone, 2, 2-dimethoxy-phenylf ketone, phenyl two (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone, 2, 4-dimethyl thioxanthone or 2, one or more in 4-diethyl thioxanthone.
Based on above-mentioned preparation method, the luminescent device that the present invention also provides a kind of quantum dot light emitting layer to arrange densification, wherein, described luminescent device adopts the preparation method of the as above luminescent device that arbitrary described quantum dot light emitting layer arrangement is fine and close to be prepared from.Luminescent device of the present invention comprises from bottom to top successively: anode layer, hole injection layer, hole transmission layer, quantum dot light emitting layer, electron transfer layer, electron injecting layer and cathode layer; Wherein, described quantum dot light emitting layer is the quantum dot blooming of fine and close arrangement.
Preferably, described quantum dot is that inorganic semiconductor nano luminous body is selected from the Colloidal Quantum Dots or nanometer rods with single distribution.Wherein, described quantum dot or nanometer rods can be II-IV compound semiconductor and nucleocapsid structure (as CdS, CdSe, CdS/ZnS, CdSe/ZnS or CdSe/CdS/ZnS) thereof, or are the one in III-V or the semiconductor nano such as group IV-VI compound semiconductor and nucleocapsid structure (as GaAs, InP, PbS/ZnS or PbSe/ZnS), I-III-VI race or nucleocapsid structure semiconductor nano.
Preferably, described quantum dot is of a size of average feature size 2 ~ 10nm.And described quantum dot is homogeneous mixed type, gradient mixed type, core-shell type or union type.Quantum dot of the present invention can be oil-soluble quantum dot.Described quantum dot can be selected from the quantum dot of doping or the quantum dot of undoped.
Preferably, the material of anode layer of the present invention can be high work function transparent conductive glass, and such as, the material of described anode layer is ITO, FTO or GZO, also can be the combination of ITO, FTO, GZO and PEDOT:PSS.The material of cathode layer of the present invention can be Au, Ag, Al, In, Mg/Ag or Li/Al.Hole injection layer/hole transmission layer of the present invention includes a p-type inorganic semiconductor material or p-type organic material.Wherein, described p-type inorganic semiconductor material can be selected from NiO
x, WO
x, MoO
x, RuO
x, VO
xin one or more.Described p-type organic material can be selected from amine, biphenyl class triaryl amine, thiophene, bithiophene as one or more in two thienothiophenes and bithiophene, pyrroles, aniline, carbazole, indolocarbazole, phthalocyanine, porphyrin and their derivative.Such as, p-type organic material is TPD, NPB, PTT or PPV.
Preferably, electron injecting layer/electron transfer layer of the present invention can include a n-type inorganic semiconductor material or n-type organic material.Wherein, described n-type inorganic semiconductor material can be selected from ZnO, ZnS, ZnSe, TiO
2, one or more in ZnTe, GaN, GaP, AlN, CdSe, CdS, CdTe, CdZnSe and their any alloy.Described n-type organic material can be selected from three (oxine) aluminium (AlQ
3), azophenlyene, phenanthroline, anthracene, phenanthrene, fluorenes, two fluorenes, spiral shell two fluorenes, to phenylacetylene, triazine, triazole, imidazoles, Bi, perylene, azophenlyene, phenanthroline, anti-indenofluorene, along one or more in indeno, dibenzo-indenofluorene, indeno naphthalene, benzanthracene and their derivative.
In addition, also it should be noted that, in the preparation process of luminescent device of the present invention, quantum dot light emitting layer can pass through spin coating proceeding film forming, but is not limited to spin coating proceeding, and quantum dot light emitting layer is also by the technique such as ink-jet or blade coating film forming.Except anode, negative electrode, other functional layers can pass through the technique film forming such as evaporation or spin coating, ink-jet, blade coating.
Below by specific embodiment, the present invention is described in detail.
Embodiment 1
1), ITO electro-conductive glass substrate uses chloroform, acetone and isopropyl alcohol to clean successively, then carries out UV ozone plasma treatment to the ITO electro-conductive glass substrate after cleaning.
2), hole injection layer: MoO
3(10nm) in high vacuum (1 × 10
-6mPa) by thermal evaporation (MoO
3powder) form.
3), the quantum dot light emitting layer of fine and close arrangement: 3-(methacryloxy) propyl trimethoxy silicane is hydrolyzed at CdTe/CdS quantum dot surface, prepares the SiO of end with methacryl
2the CuInS that shell is stable
2/ SiO
2core-shell quanta dots, is configured in cyclohexane solvent (15mg/mL), and adds 0.5wt% light trigger 2-hydroxy-2-methyl-1-phenyl-1 acetone, then by its inkjet printing at MoO
3on, 2000rpm, 30s.Next, the methanol solution of 1, the 3-dimercaptopropane of 20mM is heated to 40 DEG C, then quantum dot film is immersed in 5min in the methanol solution of 1,3-dimercaptopropane, remove under being placed on UV-irradiation and carry out cross-linking reaction 5min.And clean 5min with pure methanol solution.Then rinse with isopropyl alcohol and drying under nitrogen flowing, then by film 180 DEG C of after annealing 30min in nitrogen glove box.
4), electron injecting layer: TiO
2(40nm), titania sol gel presoma is diluted to 5wt% in butanols, and rotary coating carries out 30 seconds under the rotating speed of about 2000rpm, then anneals 30 minutes at 100 DEG C.
5) negative electrode: Al (150nm) is in high vacuum (1 × 10
-6mPa) in, thermal evaporation forms.
6) encapsulate: device encapsulates with a kind of ultraviolet hardening resin in nitrogen glove box.
Embodiment 2
1), ITO electro-conductive glass substrate uses chloroform, acetone and isopropyl alcohol to clean successively, then carries out UV ozone plasma treatment to the ITO electro-conductive glass substrate after cleaning.
2), hole injection layer/hole transmission layer: the aqueous solution for the PEDOT:PSS of hole injection layer is spun on ITO, and rotary coating carries out 60 seconds under the rotating speed of about 4000rpm, then toasts 10 minutes at 140 DEG C.
For the Poly-TPD of hole transmission layer rotary coating, in chlorobenzene, dissolved dilution is to 8mg/mL, and rotary coating carries out 45 seconds under the rotating speed of about 2000rpm, then baking fire 20 minutes at 110 DEG C.
3), quantum dot light emitting layer: be that cyclohexane solvent (10mg/ml) inkjet printing of the CdSe/ZnS quantum dot of 8-aminocaprylic acid is on Poly-TPD hole transmission layer by part.Next, the toluene solution of 1, the 6-hexyl diisocyanate of configuration 20mM, is then immersed in quantum dot film in the toluene solution of 1,6-hexyl diisocyanate, and cleans 5min with pure methanol solution.Then rinse with isopropyl alcohol and drying under nitrogen flowing, then by film 200 DEG C of after annealing 30min in nitrogen glove box.
4), electron transfer layer: ZnO (40nm), zinc oxide sol-gel precursor is diluted to 50mg/mL in ethanol.Rotary coating carries out 50 seconds under the rotating speed of about 2000rpm, then anneals 5 minutes at 60 DEG C.
5), negative electrode: Al (150nm) is in high vacuum (1 × 10
-6mPa) in, thermal evaporation forms.
6) encapsulate: device encapsulates with a kind of ultraviolet hardening resin in nitrogen glove box.
To sum up above-mentioned, the present invention, by adding the compound solution that another plays crosslinked action on quantum dot light emitting layer, realizes quantum dot surface ligand exchange, thus is cross-linked.By the crosslinking Treatment of quantum dot, make the quantum dot arrangement even compact obtained, and there is no pin hole, the defects such as crack, leakage current can not be there is, thus it is luminous to efficiently solve light emitting diode with quantum dots decrease in efficiency or other adjacent charge transport layers, the problem such as cause spectrum impure.And radiation recombination luminous efficiency can be improved, and then improve light emitting diode with quantum dots efficiency.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection range that all should belong to claims of the present invention.
Claims (10)
1. a preparation method for the luminescent device that quantum dot light emitting layer arrangement is fine and close, is characterized in that, comprise step:
A, spin coating hole injection layer are on anode layer, and then spin coating hole transmission layer is on hole injection layer;
The quantum dot light emitting layer of B, subsequently spin coating densification arrangement is on hole transmission layer, wherein, concrete steps are: quantum dot is configured to quantum dot solution, then quantum dot solution is spin-coated on hole transmission layer, obtained quantum dot light emitting layer, then on quantum dot light emitting layer, add a compound solution playing crosslinked action with the surface ligand of quantum dot be cross-linked, obtain the quantum dot light emitting layer of fine and close arrangement;
On the quantum dot light emitting layer that C, last spin coating electron transfer layer are arranged in densification, then spin coating electron injecting layer is on electron transfer layer, and evaporation cathode layer is on electron injecting layer, obtains light emitting diode with quantum dots.
2. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 1 is fine and close, it is characterized in that, in described step B, the surface ligand of described quantum dot is that end is with-NH
2,-COOH ,-SO
3the part of the group of H ,-OH or-SH.
3. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 2 is fine and close, it is characterized in that, in described step B, described compound is with difunctional or multi-functional compound, and described difunctional or multi-functional compound are the compound with two or more-NCO, epoxide group, acrylate or double bond group.
4. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 1 is fine and close, it is characterized in that, in described step B, the surface ligand of described quantum dot is the part that the group of crosslinked action can occur of end with double bond.
5. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 4 is fine and close, it is characterized in that, the surface ligand of described quantum dot is propylene bisphosphate, allylamine, allyl alcohol, allyl mercaptan, acrylic acid, the acrylate hydroxy ester containing hydroxy functional group or double bond containing disulphide.
6. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 1 is fine and close, it is characterized in that, in described step B, the surface ligand of described quantum dot is the quantum dot stability shell through surface prepared by stability modification with double bond group.
7. the preparation method of the luminescent device that quantum dot light emitting layer arrangement according to claim 6 is fine and close; it is characterized in that; described surface is that quantum dot warp contains the process of (methyl) acryl silane with the quantum dot stability shell of double bond group, and the end prepared is with the SiO of (methyl) acryl group
2quantum dot/the SiO of the nucleocapsid structure of shell
2compound.
8. the preparation method of the luminescent device that the quantum dot light emitting layer arrangement according to claim 4 or 6 is fine and close, it is characterized in that, described compound is with difunctional or multi-functional compound, and described difunctional or multi-functional compound are two mercaptan, carbon-carbon double bond or esters of acrylic acid unsaturated comonomer.
9. the preparation method of the luminescent device that the quantum dot light emitting layer arrangement according to claim 4 or 6 is fine and close, is characterized in that, described crosslinked crosslinking curing mode is ultraviolet light cross-linking solidification, heat cross-linking solidification or catalytic reagent crosslinking curing.
10. the luminescent device that quantum dot light emitting layer arrangement is fine and close, is characterized in that, adopts as arbitrary in claim 1 ~ 9 as described in the arrange preparation method of luminescent device of densification of quantum dot light emitting layer be prepared from.
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